commiss regul ec januari lai detail rule applic council regul ec method analysi qualiti evalu milk milk product amend regul ec ec commiss european commun regard treati establish european commun regard council regul ec common organis market milk milk product articl articl thereof commiss regul eec eec ec ec ec ec ec ec ec ec full refer annex xxvi regul lai refer routin method analysi qualiti evalu milk milk product establish scope rule appli method interest clariti provid oper sector singl set method rule appli abovement regul recast brought singl text reason commiss regul ec decemb lai detail rule applic council regul ec intervent market butter cream ec decemb lai detail rule appli regul ec grant aid skim milk skim milk powder intend anim feed sale skim milk powder amend annex regul analysi method includ regul composit qualiti requir milk milk product laid arrang provid regul ec verifi ensur strictli compli refer method verif method publish intern organis cen idf iso aoac intern regularli updat organis case commun refer method laid case refer method commun rule order ensur refer method uniformli appli list refer method drawn year method includ list appli routin method rule condit common method establish ensur uniform practic evalu result analys sensori evalu product concern examin result disput analys internation accept refer method valid inform laboratori variat analyt result commun method laid valid internation establish rule appli refer method commiss regul ec decemb sale butter reduc price grant aid cream butter concentr butter manufactur pastri product ic cream foodstuff amend regul ec trace cream butter concentr butter circumst order ensur correct end product trace import scheme function properli order ensur oper particip receiv equal treatment common method establish determin tracer commiss regul eec novemb sale reduc price intervent butter intend direct consumpt form concentr butter amend regul ec commiss regul eec februari grant invit tender aid concentr butter intend direct consumpt commun amend regul ec regul ec concentr butter tracer ad supervis complianc requir trace concentr butter strictli enforc ensur product divert common method detect tracer laid articl regul ec privat storag aid grant chees made ew milk special refund product grant articl regul chees made ew milk goat milk buffalo milk mixtur ew goat buffalo milk import commun preferenti arrang countri view provis check need ensur cow milk incorpor product concern commun refer method establish detect cow milk prejudic routin method provid compli criteria commiss regul eec octob grant aid skim milk product casein casein amend regul ec absenc coliform detect internation accept refer method detect coliform milk milk product intern standard idf standard applic modifi form detect coliform quantiti product commun refer method detect coliform establish base abovement standard council regul eec juli tariff statist nomenclatur common custom tariff amend regul ec rate custom duti compound feedingstuff fall tariff head depend milk product content ensur rule question uniformli appli gener recognis method analys lactos content laid compulsori member state regul ec butter skim milk powder intend intervent case skim milk powder anim feed meet qualiti requir refer method laid verifi requir met implement method introduc time regul requir period adapt applic method defer manag committe milk milk product deliv opinion time limit set chairman adopt regul chapter gener provis articl scope field applic regul lai rule appli method chemic physic microbiolog analysi sensori evalu milk milk product arrang provid common organis market milk milk product establish regul ec lai method articl list method annex regul list refer method applic analys refer articl commiss updat list year accord procedur laid articl regul ec articl routin method routin method analys requir commun rule provid properli calibr regularli check refer method procedur annex ii appli check result obtain routin method close limit regul concern case disput result obtain refer method decis articl valid refer method refer method valid meet pre determin precis criteria repeat reproduc limit refer method laid regul concern valid member state set provision reproduc limit limit obtain procedur annex iii month entri forc regul member state equival procedur complianc limit check year result appli valid refer method method provision precis figur show limit exceed analyt result evalu method annex iv determin critic differ limit concern articl admiss analysi result analys perform laboratori oper intern qualiti control procedur accord annex procedur equival standard detail descript procedur appli consult laboratori laboratori establish hous precis run method procedur annex publish valid procedur establish repeat complianc reproduc limit check year procedur annex iii subparagraph appli laboratori particip profici test scheme year laboratori report result analysi suffici inform evalu result made accord annex iv annex viii analysi result consid admiss obtain accord accept criteria intern qualiti control procedur refer paragraph hous precis refer paragraph articl sensori evalu butter procedur annex vi appli check perform assessor reliabl result procedur annex vii appli refer method sensori evalu milk milk product butter refer method member state sensori evalu idf standard compar method notifi commiss procedur annex vi check perform assessor reliabl result articl sampl disput result analys duplic sampl analys requir commun rule procedur annex viii case result analysi accept oper chapter ii method analysi articl water solid fat fat content butter analysi method annex ix refer method determin water content butter analysi method annex refer method determin solid fat content butter analysi method annex xi refer method determin fat content butter articl tracer analysi method annex xii refer method determin vanillin concentr butter butter cream analysi method annex xiii refer method determin ethyl ester beta apo caroten acid content concentr butter butter analysi method annex xiv refer method determin sitosterol stigmasterol content butter concentr butter concentr butter butter cream trace conform relev commun rule result obtain accord specif paragraph annex refer paragraph articl detect cow milk casein refer method analysi annex xv ensur chees made exclus ew milk goat milk buffalo milk mixtur ew goat buffalo milk fact cow milk casein cow milk casein held present appar cow milk casein content sampl analys equal higher content refer sampl cow milk annex xv routin method detect cow milk casein chees refer paragraph provid detect limit lower fals posit result cow milk casein detect requir sensit long ripen period occur usual commerci condit requir provid met sampl give posit result analys refer method requir provid met type chees refer paragraph chees analys refer method articl detect coliform refer method analysi annex xvi detect presenc coliform butter skim milk powder casein casein routin method detect coliform provid result obtain compar result obtain refer method annex routin method adequ detect limit fals neg result occur occurr fals posit result exclud posit result confirm refer method articl lactos content method determin lactos content product fall cn code annex xvii articl detect rennet whei method detect rennet whei skim milk powder intend public storag annex xviii method detect rennet whei skim milk powder mixtur intend anim feed annex xix articl detect buttermilk method detect buttermilk skim milk powder annex xx articl antimicrobiot residu method detect antibiot sulphonamid dapson residu skim milk powder annex xxi articl skim milk powder content method determin skim milk powder content compound feedingstuff annex xxii articl detect starch method detect starch skim milk powder denatur milk powder compound feedingstuff annex xxiii articl moistur content acid buttermilk powder method determin moistur content acid buttermilk powder intend feedingstuff annex xxiv articl detect foreign fat method detect foreign fat milk fat annex xxv chapter iii final provis articl amend regul ec regul ec amend sentenc articl replac quot compet author check qualiti butter method annex basi sampl accord rule set annex iv quot annex footnot replac quot annex regul ec quot annex ii iii delet penultim sentenc annex iv word quot annex iii quot replac quot annex vii regul ec quot articl amend regul ec regul ec amend articl replac quot skim milk powder content mixtur compound feedingstuff determin test sampl duplic analysi method annex xxii regul ec supplement check provid articl regul discrep result check result spot inspect conclus absenc rennet whei proven method annex xix regul ec starch content compound feedingstuff determin check provid articl regul supplement analysi method annex xxiii regul ec moistur content acid buttermilk powder determin analysi method annex xxiv regul ec quot annex iii iv vi delet articl repeal regul eec eec ec ec ec ec ec ec ec ec repeal refer repeal regul constru refer regul articl entri forc regul enter forc seventh dai public offici journal european commun method annex iii iv vi viii appli month entri forc regul regul bind entireti directli applic member state brussel januari commiss franz fischler member commiss oj oj oj oj oj oj oj oj oj oj oj oj oj annex articl list refer methodsnot list european union refer method note milk fat isol idf standard protect light note refer method establish note sampl prepar idf standard idf standard note incub hour temperatur care prevent cultur medium dry note snf solid fat note butter correspond nation qualiti class member state product refer annex commiss regul ec note commiss direct eec note commiss regul ec oj note commiss direct eec gt tabl gt gt tabl gt annex ii articl check result obtain routin method close limit regul composit qualiti requir mo limit composit qualiti requir regul decis limit gt refer graphic gt rrout rref amp lt rrout reproduc limit routin method rref reproduc limit refer method mo upper limit rrout rref amp gt decis limit obtain formula gt refer graphic gt condit mo lower limit decis limit obtain formula gt refer graphic gt crd critic differ refer method annex iv mo upper limit final result decis limit obtain routin method substitut final result obtain refer method final result base number analys sampl final result obtain routin method mo lower limit procedur final result decis limit obtain routin method remark procedur detect matrix effect matrix effect detect sampl calibr differ wi result obtain refer routin method determin standard deviat calcul formula gt refer graphic gt number sampl calibr compar arithmet repeat standard deviat refer routin method gt refer graphic gt matrix effect exclud gt pic file quot en ep quot gt number degre freedom error probabl case investig decis limit fix annex iii articl procedur determin complianc establish reproduc limit chemic analysi complianc reproduc limit check compar laboratori result result experienc laboratori obtain ident sampl doubl determin carri laboratori result evalu formula gt refer graphic gt crd critic differ gt refer graphic gt arithmet result obtain laboratori gt refer graphic gt arithmet result obtain laboratori reproduc limit determin interpol repeat limit precis vari level critic differ exceed experi perform month result experi compli reproduc limit compet author step procedur obtain provision reproduc limit chemic analysi provision reproduc limit rprov obtain equat gt refer graphic gt gt refer graphic gt result obtain laboratori gt refer graphic gt result obtain laboratori annex iiia repeat limit provision repeat limit remark rprov calcul critic differ annex vi rprov fix calcul rprov smaller calcul larger greater predict horwitz equat rprov unaccept high calcul critic differ rprov determin year basi result obtain laboratori annex iv rprov calcul critic differ rule appli rprov reproduc limit obtain calcul rsdr gt refer graphic gt gt refer graphic gt arithmet result obtain calcul rsdr valu exampl gt tabl gt concentr analyt obtain gt refer graphic gt experienc laboratori gener particip successfulli valid test method profici test horwitz equat gt refer graphic gt rsdr rel standard deviat reproduc concentr express decim fraction refer peeler horwitz albert ass anal chem annex iv articl evalu analyt result obtain valid method analyt result show limit exceed arithmet result calcul procedur case analyt result repres singl result analysi carri repeat condit analys carri repeat condit carri duplic analysi repeat condit result assess critic differ complianc absolut differ arithmet result obtain repeat condit limit determin absolut differ greater critic differ mean sampl analys fulfil requir critic differ determin formula gt refer graphic gt gt refer graphic gt arithmet result obtain mo limit number analys sampl precis vari level determin interpol final result report sampl show limit comli final result rang gt refer graphic gt gt refer graphic gt limit maximum rang gt refer graphic gt gt refer graphic gt limit minimum occur exceptionnali final result rang mention accept occur sampl analys consign sampl analys consign result rang mention accept rule result rang mention obtain sampl analys adher consign repeatedli offer produc final result calcul formula form water solid food fat content butter calcul fat content final result singl type analysi repeat reproduc limit rx rx final result calcul gt refer graphic gt gt refer graphic gt repeat limit reproduc limit compar limit rule critic differ determin formula gt refer graphic gt arithmeth result obtain final result calcul formula form gt refer graphic gt fat dry matter content chees final result singl type analysi repeat reproduc limit rx rx calcul gt refer graphic gt gt refer graphic gt gt refer graphic gt limit target fat limit target dry matter gt refer graphic gt gt refer graphic gt repeat limit repeat limit gt refer graphic gt gt refer graphic gt reproduc limit reproduc limit procedur calcul rx rx applic rel repeat reproduc limit smaller equal compar limit μx rule critic differ determin formula gt refer graphic gt gt refer graphic gt arithmet result obtain chronolog order note result obtain arithmet calcul annex intern control articl intern qualiti control iqc procedur chemic analysi definit control materi materi purpos iqc subject part procedur test materi control materi certifi refer materi hous refer materi materi valid interlaboratori test fortifi materi procedur establish iqc laboratori introduc iqc procedur iupac document quot harmon guidelin intern qualiti control analyt laboratori quot iqc involv includ control materi analyt sequenc replic analysi test sampl control materi similar chemic composit test sampl adequ stabl period interest demonstr suitabl divid ident portion analysi concentr analyt rang interest control materi insert analyt run obtain plot control chart order measur long term error addit laboratori period demonstr complianc repeat condit run achiev duplic analysi control test materi result analys compar publish repeat limit exist data hous precis control materi valu obtain run analysi control materi plot shewhart chart iso control limit action limit set gt refer graphic gt st total standard deviat warn limit gt refer graphic gt total standard deviat gt refer graphic gt sb run standard deviat sw run standard deviat number determin case control materi lack stabil test materi analys duplic run absolut differ obtain duplic analys run annex iii plot centr line sw lower limit upper limit action limit sw sw run standard deviat control procedur includ materi low high level concentr rang larg test materi cover wide rang analyt concentr laboratori establish relationship precis level precis proport level subsequ control base rel precis absolut differ percentag control condit analyt system signal occur current plot fall action limit current previou fall warn limit action limit control materi success valu fall side line laboratori respond control condit stop analysi pend diagnost test remedi action reject run result analys test materi procedur select hous control materi determin quot hous quot precis limit chemic analysi data laboratori precis obtain replic analysi control materi replic analysi test sampl laboratori procedur establish precis paramet run run variat subsequ construct control chart laboratori adopt altern procedur provid adequ demonstr reliabl precis data deriv select control materi laboratori control materi data gather order set limit certifi refer materi crm candid control materi analys repeat condit run includ suitabl crm replic randomis approach laboratori seek particip profici test establish consensu mean assign valu regard convent true meaning uncertainti attach procedur includ assign true formul spike control materi addit laboratori regularli carri type analysi establish statist control control materi requir stock run obtain refer analys control exist materi assign limit select control materi laboratori establish run run precis figur minimum requir establish run precis control materi analys duplic occas duplic analysi perform repeat condit oper reagent duplic analysi control materi randomis analyt run duplic analysi undertaken separ dai period time reflect reason run run variat take account normal variat reagent instrument calibr analyst note data fulli repres run variat result unnecessari replic analysi excess tight limit set convers laboratori present precis data imprecis unabl meet prescrib limit refer method expect show poor perform compar peer laboratori produc data fit intend purpos determin run precis run precis control materi duplic data minimum duplic subject cochran maximum varianc test involv compar squar maximum duplic rang sum squar rang gt refer graphic gt di differ duplic cochran criterion compar tabul valu iso classifi straggler outlier result investig explan technic error comput error slip perform test analysi wrong sampl explan technic error prove imposs replac suspect result discard real outlier straggler outlier remain explain straggler retain correct statist outlier discard laboratori seek obtain replac valu laboratori satisfi data free outlier run standard deviat sw obtain pair xi xi duplic data sum duplic gt refer graphic gt differ duplic gt refer graphic gt comput sum gt refer graphic gt gt refer graphic gt gt refer graphic gt estim run standard deviat gt refer graphic gt hous precis limit sw refer method hous precis limit compar publish repeat limit laboratori compli requir refer method failur meet requir investig limit set regard provision subject review run precis control materi laboratori choos establish run precis duplic analysi repres test sampl minimum duplic analys case control materi instabl duplic data accumul method note assum analys cover narrow rang valu singl appli sampl case rang result wider order magnitud precis depend level laboratori investig rel standard deviat data subject cochran test laboratori satisfi data free outlier run standard deviat hous precis limit obtain section run standard deviat sw construct control chart annex ii limit set regard provision subject review determin run precis comput averag pair subject grubb test iso reject accept criteria outlier straggler laboratori seek obtain replac discard result laboratori satisfi data free outlier run standard deviat sb calcul gt refer graphic gt express squar root sign neg total standard deviat st construct control chart averag determin annex ii limit set regard provision subject review review initi limit control limit set regard initi estim order updat limit set basi accept run precis section duplic data test sampl collect interv review depend frequenc analysi guidelin data review duplic obtain data subject cochran test limit reset basi standard deviat figur subsequ decis valid control limit made light data review initi data obtain run precis depend frequenc analysi guidelin ten data point obtain analysi control materi frequenc analysi batch initi assumpt made standard deviat review data subject grubb test outlier standard deviat recalcul basi data addit stage laboratori appli cusum chart bs amend investig problem ag reagent singl result fall cusum quot mask quot limit investig limit standard deviat subject regular inspect cusum techniqu indic valid control materi brought question investig report precis data laboratori send inform compet nation author method emploi run standard deviat sw hous precis limit run standard deviat sb total standard deviat number analys involv obtain precis data thompson wood quot pure appli chemistri quot annex vi articl evalu assessor reliabl result sensori analys procedur applic score method idf standard determin quot repeat index quot ten sampl analys blind duplic assessor period month happen session result individu product characterist evalu formula gt refer graphic gt wi repeat index xi score evalu sampl xi xi score evalu sampl xi number sampl sampl evalu reflect broad qualiti rang wi exce point scale determin quot deviat index quot index check assessor scale qualiti evalu experienc group assessor score obtain assessor compar averag score obtain assessor group formula evalu result gt refer graphic gt xi xi section gt refer graphic gt gt refer graphic gt averag score assessor group evalu sampl xi number sampl ten month sampl evalu reflect broad qualiti rang di exce point scale member state notifi difficulti encount appli procedur comparison result obtain region member state member state applic test organis year compar result obtain assessor region signific differ observ step identifi reason arriv compar result member state organis test compar result obtain assessor assessor neighbour member state signific differ lead depth investig aim arriv compar result member state notifi commiss result comparison annex vii articl sensori evalu butter scope purpos procedur sensori evalu butter provid uniform method applic member state definit sensori evalu assess mean examin attribut product sens organ panel mean group select assessor work assess intercommun influenc score mean sensori evalu panel numer scale nomenclatur defect grade mean qualiti classif perform basi score control document document record individu score attribut final grade product document record chemic composit test room precaut order assessor test room influenc extern factor test room free foreign odour easi clean wall light colour test room light properti product score affect room equip temperatur control select assessor assessor familiar butter product compet carri sensori grade compet assess regular basi year compet author requir panel number assessor panel uneven minimum number major employe compet author authoris person emploi dairi industri number factor account evalu order obtain optim perform subject subject suffer ill affect perform case assessor concern replac panel subject time part evalu make time make evalu subject strong smell substanc perfum shave lotion deodor avoid eat strong favour highli spice food subject smoke eat drink water half hour evalu assess attribut sensori evalu carri relat attribut appear consist flavour appear involv featur colour visibl puriti mould growth water dispers water dispers test idf standard consist involv featur firm spreadabl physcial method appli evalu butter consist commiss envisag futur harmonis method flavour involv featur tast odour signific deviat recommend temperatur prevent reliabl evalu consist flavour temperatur paramount import attribut sensori evalu separ score tabl desir assessor score start assess refer sampl appear consist flavour order achiev uniform score accept gt tabl gt requir score obtain descript defect score assessor attribut record control document product accept reject basi major decis case differ individu score attribut wider adjac point occur frequent sampl compet panel check panel leader supervis panel leader offici employe compet author member panel gener respons entir procedur record individu score attribut control document certifi product accept reject sampl prepar sampl desir ident sampl conceal assess bia avoid organ panel leader prior evalu presenc panel member sensori evalu carri cold store sampl butter trier sensori evalu carri locat cold store sampl evalu butter temperatur larg deviat avoid cost nomenclatur refer append tabl tabl butter score gt tabl gt gt tabl gt gt tabl gt tabl tabl butter defect appear loos free moistur uniform colour streaki mottl marbl speckl oil separ overcolour weak open textur granular foreign matter mouldi undissolv salt ii consist short brittl crumbl pasti doughi greasi sticki hard soft iii flavour amp aroma flavour unclean foreign flavour stale cheesi lactic chees flavour acid yeasti cook flavour scorch flavour mouldi flavour rancid oili fishi tallowi oxid flavour metal flavour feed flavour coars bitter oversalt musti flat putrid malti chemic flavour design seldom defect accur annex viii articl procedur applic result analysi disput chemic analysi analysi carri request oper work dai notif result analysi provid seal duplic sampl product store appropri compet author compet author send sampl laboratori request expens oper laboratori authoris carri offici analys proven compet analys question compet document success particip collabor studi profici test interlaboratori comparison laboratori refer method result obtain laboratori evalu laboratori meet repeat requir reproduc requir arithmet test result obtain laboratori report final result final result evalu take critic differ consider formula gt refer graphic gt gt refer graphic gt arithmet result obtain laboratori mo limit reproduc repeat number result obtain laboratori number result obtain laboratori note final result calcul formula gt refer graphic gt gt refer graphic gt annex iv insert formula laboratori meet repeat requir reproduc requir analysi confirm quantiti analysi reject compliant quantiti accept laboratori meet repeat requir final result laboratori meet repeat requir decid accept quantiti analysi laboratori meet repeat requir reproduc requir met appli laboratori meet repeat requir reproduc requir quantiti analysi accept result obtain laboratori lead conclus result obtain valid method quantiti analysi accept result obtain laboratori lead conclus result analysi notifi compet author oper cost analysi born oper quantiti analysi reject oper prove work dai sampl sampl procedur carri correctli sampl repeat sampl repeat quantiti analysi accept annex ix articl determin water content butter scope field applic refer method specifi method determin water content butter refer idf standard milk milk product method sampl definit water content butter loss mass complet heat process standard express gram gram principl evapor water test portion presenc pumic temperatur dry oven apparatu materi usual laboratori apparatu analyt balanc sensit mg desicc provid effici dry agent freshli dri silica gel hygroscop indic dry oven ventil thermostat control oper total work space glass porcelain corros metal dish height mm diamet mm pumic stone granul wash diamet mm sampl idf procedur prepar test sampl warm laboratori sampl close glass suitabl plastic contain half third full temperatur sampl soft facilit mix homogen state mechan shaker hand temperatur mix exce cool sampl ambient temperatur cool open sampl contain stir briefli longer second suitabl devic spoon spatula weigh determin water content place approxim pumic dish dry dish pumic oven hour note dry period mention start temperatur oven reach dish cool desicc temperatur balanc room weigh nearest mg weigh dish nearest mg test portion approxim test sampl place dish oven leav hour dish cool desicc temperatur balanc room weigh nearest mg repeat dry process addit period hour cool weigh time constant mass mass chang exceed mg reach event increas mass calcul lowest mass record express result method calcul formula calcul water content percentag mass formula gt refer graphic gt gt tabl gt report result decim place repeat absolut differ result singl determin carri simultan rapid success oper condit ident test materi exce reproduc absolut differ singl independ result obtain oper work laboratori ident test materi exce test report test report method result obtain mention oper detail intern standard regard option detail incid influenc result test report includ inform complet identif sampl annex articl butter determin solid fat content scope field applic standard speci method determin solid fat content butter refer idf standard milk milk product method sampl definit solid fat content butter percentag mass substanc determin procedur express gram gram principl evapor water mass butter extract fat light petroleum weigh residu reagent light petroleum boil rang reagent leav mg residu evapor ml apparatu materi analyt balanc sensit mg desicc provid effici dry agent freshli dri silica gel hygroscop indic dry oven ventil thermostat control oper total work space glass porcelain corros metal dish spout height mm diamet mm provid glass stir rod filter crucibl sinter glass pore diamet μm suction flask sampl idf standard procedur prepar test sampl warm laboratori sampl close glass suitabl plastic contain half third full temperatur sampl soft facilit mix homogen state mechan shaker hand temperatur mix exce cool sampl ambient temperatur cool open sampl contain stir briefli longer second suitabl devic spoon spatula weigh determin dry dish rod crucibl oven hour object cool desicc weigh dish rod crucibl nearest mg note rule cool time minut suffici import combin dish rod crucibl test portion test portion analys batch remov crucibl record weight dish rod nearest mg weigh dish nearest mg test portion test sampl place dish rod butter oven leav night dish cool room temperatur add ml warm approxim light petroleum dish detach sediment adher dish glass rod transfer solvent crucibl filter suction flask carri oper addit time trace fat surfac dish quantit transfer fourth wash sediment crucibl repeat oper till complet elimin trace fat wash sediment crucibl ml warm light petroleum dry dish glass rod crucibl oven minut cool desicc room temperatur weigh nearest mg repeat oper constant mass mass chang exceed mg reach dish rod crucibl express result calcul solid fat content calcul solid fat content snf percentag mass formula gt refer graphic gt mass gram empti dish glass rod crucibl mass gram empti dish glass rod mass gram test portion dish glass rod final mass gram dish rod crucibl sediment report result decim place repeat absolut differ result singl determin carri simultan rapid success oper condit ident test materi exce reproduc absolut differ singl independ result obtain oper work laboratori ident test materi exce test report test report method result obtain mention oper detail intern standard regard option detail incid influenc result test report includ inform complet identif sampl note gt tabl gt conclud precis figur obtain solid fat determin valid determin milk solid fat content annex xi articl determin fat content butter fat content obtain indirecli determin water content solid fat content annex ix annex percentag mass fat equal gt refer graphic gt gt tabl gt gt tabl gt annex xii articl determin vanillin content concentr butter butter cream high perform liquid chromatographi scope field applic method describ procedur quantit determin vanillin concentr butter butter cream principl extract quantiti sampl mixtur isopropanol ethanol acetonitril precipit major fat cool centrifug dilut water determin vanillin content high perform liquid chromatographi hplc apparatu usual laboratori apparatu freezer oper temperatur rang syring dispos ml capac membran microfilt μm pore size resist solut extract solut liquid chromatographi system consist pump flow ml min injector μl inject automat manual uv detector oper nm au full scale record integr column thermostat oper analyt column mm mm id pack lichrosph rp merck μm equival guard column ca mm mm id dry pack perisorb rp μm equival reagent reagent recognis analyt qualiti isopropanol ethanol acetonitril extract solut mix isopropanol ethanol acetonitril ratio vanillin hydroxi methoxybenzaldehyd vanillin stock solut μg ml weigh accur mg mg cm mg vanillin ml volumetr flask add ml extract solut make water vanillin standard solut μg ml pipett ml vanillin stock solut volumetr flask ml make water methanol hplc qualiti acet acid glacial water hplc qualiti hplc mobil phase mix ml methanol ml water ml acet acid volumetr flask ml make water filter μm filter procedur prepar test sampl butter heat sampl melt start avoid local overh sampl suffici plastic homogenis shake stir butter take sampl weigh nearest mg sm butter ml volumetr flask concentr butter immedi sampl place contain concentr butter oven melt complet mix sampl swirl stir avoid format air bubbl vigor stir weigh nearest mg sm concentr butter ml volumetr flask cream heat sampl waterbath incub temperatur distribut fat homogen swirl stir cool sampl quickli sampl homogen procedur repeat weigh nearest mg sm cream ml volumetr flask prepar test solut add ml extract solut test portion stir shake vigor minut make extract solut transfer ml extract test tube fit stopper place test tube freezer stand minut centrifug cold extract minut approxim rpm decant immedi decant solut cool room temperatur pipett ml decant solut ml volumetr flask make water filter aliquot membran microfilt filtrat readi determin hplc calibr pipett ml vanillin standard solut ml volumetr flask add ml extract solut make mark water solut μg ml vanillin determin hplc chromatograph system stabilis minut inject standard solut repeat differ peak area peak height success inject condit retent time vanillin minut analys standard solut duplic inject μl inject μl test solut determin area height vanillin peak obtain repeat duplic inject standard solut alter inject test sampl calcul result calcul averag peak area height ac vanillin peak bracket duplic inject batch test solut area height total calcul respons factor gt refer graphic gt cm mass vanillin mg content mg kg vanillin test sampl gt refer graphic gt peak area vanillin peak test sampl sm mass test sampl cream analys vanillin tracer concentr express mg tracer kg milk fat multipli fat content cream percent factor take account dilut standard test sampl correct factor fat content dilut test sampl note peak area peak height accuraci method repeat differ result determin carn shortest feasibl time interv oper apparatu ident test materi exce mg kg reproduc differ result determin carri oper laboratori apparatu ident test materi exce mg kg toler limit sampl trace product order check homogen tracer obtain vanilla synthet vanillin incorpor rate hydroxi methoxybenzaldehyd tonn concentr butter butter cream trace tbe incorpor rate tonn milk fat result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate mg kg minimum incorpor rate tracer concentr sampl give lowest result conjunct interpol mg kg mg kg tracer obtain exclus vanilla bean integr extract thereof incorpor rate hydroxi methoxybenzaldehyd tonn concentr butter butter cream trace incorpor rate tonn milk fat result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate mg kg minimum incorpor rate tracer concentr sampl give lowest result conjunct interpol mg kg mg kg note repeat absolut differ singl test result obtain method ident test materi condit apparatu laboratori short interv time expect lie probabl absenc indic probabl reproduc absolut differ singl test result obtain method ident test materi condit oper apparatu laboratori time expect lie probabl absenc indic probabl recoveri ad vanillin level mg kg butteroil vari averag content found standard deviat standard solut extract solut compens peak broaden caus presenc extract solut test sampl enabl quantif peak height analysi base linear calibr line intercept dilut standard solut linear check time analysi carri regular interv repair hplc equip annex xiii articl determin ethyl ester beta apo caroten acid concentr butter butter spectrometri scope field applic method describ procedur quantit determin ethyl ester beta apo caroten acid apo caroten ester concentr butter butter apo caroten ester sum substanc present extract sampl obtain condit method absorb light nm principl butterfat dissolv light petroleum absorb measur nm apo caroten ester content determin refer extern standard apparatu pipett graduat capac ml spectrophotomet suitabl nm nm equip cell optic path length cm volumetr flask ml ml analyt balanc sensit mg reagent reagent recognis analyt grade apo caroten ester suspens approxim establish content suspens weigh mg volumetr flask ml dissolv ml chloroform make volum cyclohexan dilut ml solut ml cyclohexan solut dilut ml solut ml cyclohexan measur absorb nm measur maximum cyclohexan blank cell cm optic path length gt refer graphic gt amax absorb measur solut maximum weight sampl refer cm puriti suspens note apo caroten ester suspens sensit air heat light unopen origin contain seal nitrogen cool place store month open content short period apo caroten ester standard solut approx mg ml weigh nearest mg apo caroten ester suspens wg dissolv petroleum spirit transfer quantit volumetr flask capac ml make mark petroleum spirit solut mg ml apo caroten ester note solut store cool place dark discard unus solut month petroleum spirit sodium sulphat anhydr granular previous dri hour chloroform cyclohexan procedur prepar test sampl concentr butter melt sampl oven approxim butter melt sampl oven approxim filter repres portion filter anhydr sodium sulphat environ shield strong natur artifici light maintain collect suitabl amount butterfat determin weigh nearest mg approxim concentr butter extract butterfat mg transfer quantit ml vml volumetr flask petroleum spirit make mark mix transfer aliquot cm cell measur absorb nm petroleum spirit blank obtain concentr apo caroten ester solut refer calibr graph ml calibr graph pipett ml apo caroten ester standard solut ml volumetr flask dilut volum petroleum spirit mix approxim concentr solut rang μg ml calcul accur refer concentr standard solut mg ml measur absorb nm petroleum spirit blank plot valu absorb axi apo caroten ester concentr axi calcul result apo caroten ester content express mg kg product concentr butter butter apo caroten ester content μg ml read calibr graph volum ml test solut mass test portion correct factor butterfat content butter accuraci method repeat butter analysi differ result determin carri shortest feasibl time interv oper apparatu ident test materi exce mg kg concentr butter analysi differ result determin carri shortest feasibl time interv oper apparatu ident test materi exce mg kg reproduc butter analysi differ result determin carri oper laboratori apparatu ident test materi exce mg kg concentr butter analysi differ result determin carri oper laboratori apparatu ident test materi exce mg kg sourc precis data precis data determin experi conduct involv laboratori trace sampl blind duplic butter trace blind duplic concentr butter toler limit sampl trace product order check correct trace product butter incorpor rate butter take account background absorb mg kg result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate mg kg minimum incorpor rate tracer concentr sampl give lowest result conjunct interpol mg kg mg kg concentr butter incorpor rate concentr butter take account background absorb mg kg result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate mg kg minimum incorpor rate tracer concentr sampl give lowest result conjunct interpol mg kg mg kg annex xiv articl determin sitosterol stigmasterol butter concentr butter capillari column ga chromatographi scope field applic method describ procedur quantit determin sitosterol stigmasterol butter concentr butter sitosterol sum sitosterol dihydro sitosterol sitosterol assum insignific principl butter concentr butter saponifi potassium hydroxid ethanol solut unsaponifi extract diethyl ether sterol transform trimethyl silyl ether analys capillari column ga chromatographi refer intern standard betulin apparatu ml saponif flask fit reflux condens ground glass joint ml separ funnel ml flask pressur equalis funnel ml similar collect wast diethyl ether glass column mm mm fit sinter glass plug waterbath isomantl reaction vial ml ga chromatograph suitabl capillari column provid split system consist thermostat chamber column capabl maintain desir temperatur accuraci temperatur adjust vaporis unit flame ionis detector convert amplifi integr record suitabl convert amplifi fuse silica capillari column coat bp equival uniform thick μm column capabl resolv trimethyl silyl deriv lanosterol sitosterol bp length intern diamet mm suitabl μl ga chromatographi microsyring harden needl reagent reagent recognis analyt grade water distil water water equival puriti ethanol pure potassium hydroxid solut dissolv potassium hydroxid minimum water make litr water betulin puriti solut betulin diethyl ether concentr betulin solut sitosterol determin mg ml concentr betulin solut stigmasterol determin mg ml diethyl ether analyt puriti free peroxid residu sodium sulphat anhydr granular previous dri hour silyl reagent tri sil pierc chemic cat equival import tri sil inflamm toxic corros possibl carcinogen laboratori personnel familiar tri sil safeti data precaut lanosterol sitosterol puriti pure note puriti standard materi calibr determin method normalis assum sterol present sampl repres chromatogram total area peak repres sterol constitu sterol give detector respons linear system valid concentr rang interest sitosterol standard solut prepar solut nearest mg ml approxim mg ml sitosterol diethyl ether stigmasterol puriti pure stigmasterol standard solut prepar solut nearest mg approxim mg ml stigmasterol diethyl ether resolut test mixtur prepar solut mg ml lanosterol mg ml sitosterol diethyl ether method prepar standard solut chromatographi intern standard solut ad sterol standard solut time ad saponifi sampl sitosterol standard chromatograph solut transfer ml sitosterol standard solut reaction vial remov diethyl ether stream nitrogen add ml intern solut remov diethyl ether stream nitrogen stigmasterol standard chromatograph solut transfer ml stigmasterol standard solut reaction vial remov diethyl ether stream nitrogen add ml intern standard solut remov diethyl ether stream nitrogen prepar unsaponifi melt butter sampl temperatur exceed mix sampl stir weigh nearest mg approxim butter concentr butter ml flask add ml ethanol ml potassium hydroxid solut fit reflux condens heat approxim minut detach condens cool flask approxim ambient temperatur add ml intern standard solut flask sitosterol determin stigmasterol determin mix transfer content flask quantit ml separ funnel wash flask turn ml water ml diethyl ether shake separ funnel vigor minut phase separ run lower aqueou layer wash ether layer shake success ml aliquot water note avoid format emuls essenti water wash carri gentli invers wash shaken vigor second emuls form destroi addit ml ethanol ethanol ad essenti carri vigor water wash pass clear soap free ether layer glass column anhydr sodium sulphat collect ether ml flask add anti bump granul evapor dryness waterbath isomantl take care collect wast solvent note sampl extract complet dryness high temperatur sterol loss occur prepar trimethyl silyl ether transfer ether solut remain flask ml reaction vial ml diethyl ether remov ether stream nitrogen wash flask ml aliquot diethyl ether transfer vial remov ether nitrogen time silyl sampl addit ml tri sil close vial shake vigor dissolv dissolut incomplet warm stand minut inject ga chromatograph silyl standard sampl silyl resolut test mixtur sampl note silyl effect water free environ incomplet silyl betulin peak close betulin presenc ethanol silyl stage interfer silyl result inadequ wash extract stage problem persist wash introduc extract stage shake vigor second ga chromatograph analysi choic oper condit set ga chromatograph manufactur instruct guidelin oper condit column temperatur injector temperatur detector temperatur carrier ga flow rate ml min hydrogen pressur kpa air pressur kpa sampl split split ratio optimis accord manufactur instruct linear detector respons valid concentr rang interest note import inject liner regularli clear amount substanc inject μl tmse solut system equilibr obtain satisfactori stabl respons commenc analysi condit vari light column ga chromatograph characterist obtain chromatogram meet requir sitosterol peak adequ resolv lanosterol figur show typic chromatogram obtain silyl resolut test mixtur rel retent time sterol approxim cholesterol stigmasterol sitosterol betulin retent time betulin approxim minut analyt procedur inject μl silyl standard solut stigmasterol sitosterol adjust integr calibr paramet inject μl silyl standard solut determin respons factor refer betulin inject μl silyl sampl solut measur peak area chromatograph run bracket inject standard guid inject sampl includ bracket run note integr stigmasterol peak includ tail defin point figur integr sitosterol peak includ area dihydro sitosterol stigmastanol peak elut immedi sitosterol figur evalu total sitosterol calcul result determin area sterol peak betulin peak standard bracket batch calcul gt refer graphic gt determin area sterol peak stigmasterol sitosterol betulin peak sampl calcul gt refer graphic gt sterol content standard mg contain ml standard solut weight sampl puriti standard sterol gt refer graphic gt accuraci method butter repeat stigmasterol differ result determin carri shortest feasibl time interv oper apparatu ident test materi exce mg kg sitosterol differ result determin carri shortest feasibl time interv oper apparatu ident test materi exce mg kg reproduc stigmasterol differ result determin carri oper laboratori apparatu ident test materi exce mg kg sitosterol differ result determin carri oper laboratori apparatu ident test materi exce rel determin sourc precis data precis data determin experi conduct involv laboratori sampl blind duplic stigmasterol sampl blind duplic sitosterol concentr butter repeat stigmasterol differ result determin carri shortest feasibl time interv oper apparatu ident test materi exce mg kg sitosterol differ result determin carri shortest feasibl time interv oper apparatu ident test materi exce rel determin reproduc stigmasterol differ result determin carri oper laboratori apparatu ident test materi exce mg kg sitosterol differ result determin carri oper laboratori apparatu ident test materi exce rel determin sourc precis data precis data determin experi conduct involv laboratori sampl blind duplic stigmasterol sampl blind duplic sitosterol toler limit sampl trace product order check correct trace product butter stigmasterol incorpor rate stigmasterol pure stigmasterol tonn butter mg kg pure stigmasterol tonn butter mg kg result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate pure stigmasterol mg kg minimum incorpor rate pure stigmasterol mg kg minimum incorpor rate pure stigmasterol mg kg minimum incorpor rate pure stigmasterol tracer concentr sampl give lowest result conjunct interpol mg kg mg kg mg kg mg kg sitosterol incorpor rate sitosterol pure sitosterol tonn butter mg kg result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate pure sitosterol mg kg minimum incorpor rate pure sitosterol tracer concentr sampl give lowest result conjunct interpol mg kg mg kg concentr butter stigmasterol incorpor rate stigmasterol pure stigmasterol tonn concentr butter mg kg pure stigmasterol tonn concentr butter mg kg result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate pure stigmasterol mg kg minimum incorpor rate pure stigmasterol mg kg minimum incorpor rate pure stigmasterol mg kg minimum incorpor rate pure stigmasterol tracer concentr sampl give lowest result conjunct interpol mg kg mg kg mg kg mg kg sitosterol incorpor rate sitosterol pure sitosterol tonn concentr butter mg kg result sampl obtain analysi product check rate homogen tracer incorpor lowest result compar limit critic differ probabl level dcr consider mg kg minimum incorpor rate pure sitosterol mg kg minimum incorpor rate pure sitosterol tracer concentr sampl give lowest result conjunct interpol mg kg mg kg gt pic file quot en ep quot gt gt pic file quot en ep quot gt gt pic file quot en ep quot gt annex xv articl refer method detect cow milk casein chees ew milk goat milk buffalo milk mixtur ew goat buffalo milk scope detect cow milk casein chees made ew milk goat milk buffalo milk mixtur ew goat buffalo milk isoelectr focus casein plasminolysi field applic method suitabl sensit specif detect nativ heat treat cow milk casein fresh ripen chees made ew milk goat milk buffalo milk mixtur ew goat buffalo milk suitabl detect milk chees adulter heat treat bovin whei protein concentr principl method isol casein chees refer standard dissolv isol casein submit plasmin ec cleavag isoelectr focus plasmin treat casein presenc urea stain protein evalu stain casein pattern evid cow milk comparison pattern obtain sampl obtain gel refer standard cow milk reagent analyt grade chemic water doubl distil equival puriti note detail appli laboratori prepar polyacrylamid gel urea dimens mm size type gel separ condit adjust isoelectr focus reagent product urea polyacrylamid gel stock gel solut dissolv acrylamid methylen bi acrylamid bi urea glycerol water make ml store brown glass bottl refriger note commerci preblend acrylamid bi solut prefer quot fix weight neurotox acrylamid solut acrylamid bi volum ml formul fix weight shelf life stock solut maximum dai conduct μs de ioniz stir amberlit mb minut filter μm membran gel solut prepar gel solut mix addit ampholyt stock gel solut ml stock solut mg alanin μl ampholyt ph μl ampholyt ph μl ampholyt ph mix gel solut de ga minut ultrason bath vacuo note prepar gel solut immedi prior pour catalyst solut tetramethylethylenediamin teme ammonium persulph dissolv mg water make ml note freshli prepar solut contact fluid kerosen liquid paraffin anod solut dissolv phosphor acid water dilut ml cathod solut dissolv sodium hydroxid water dilut ml water sampl prepar reagent protein isol dilut acet acid ml glacial acet acid made ml water dichloromethan aceton protein dissolv buffer dissolv glycerol urea mg dithiothreitol water make ml note store refriger maximum shelf life week reagent plasmin cleavag casein ammonium carbon buffer titrat mol ammonium hydrogencarbon solut ml water mol ethylenediaminetetraacet acid edta ml mol ammonium carbon solut ml water mol edta ph bovin plasmin ec activ ml aminocapro acid solut enzym inhibit dissolv aminocapro acid amino hexano acid ml ethanol standard certifi refer standard mixtur rennet ew goat skim milk cow milk commiss institut refer materi measur geel belgium prepar laboratori interim standard buffalo rennet milk cow milk skim milk prepar centrifug buffalo bovin raw bulk milk minut cool tube content rapidli upper fat layer remov complet prepar standard add ml bovin skim milk ml buffalo skim milk beaker adjust ph addit dilut lactic acid adjust temperatur add μl calf rennet rennet activ ml stir minut leav beaker cover aluminium foil hour format curd curd form rennet milk freez dri prior homogen drain whei freez dry fine ground produc homogen powder prepar standard carri procedur genuin buffalo skim milk standard store note advis check puriti buffalo milk isoelectr focus plasmin treat casein prepar standard reagent protein stain fix dissolv trichloroacet acid water make ml destain solut dilut ml methanol ml glacial acet acid ml distil water note prepar destain solut fresh dai prepar mix equal volum stock solut methanol glacial acet acid stain solut stain solut stock solut dissolv coomassi brilliant blue ml methanol magnet stirrer approxim minut filter medium speed fold filter stain solut stock solut dissolv copper sulphat pentahydr ml acet acid stain solut work solut mix ml stock solut immedi prior stain note stain solut prepar dai equip glass plate mm rubber roller width cm level tabl gel carrier sheet mm cover sheet mm stick strip adhes tape mm long edg figur electrofocus chamber cool plate mm suitabl power suppli amp gt kv automat electrophoresi devic circul cryostat thermostat control centrifug adjust electrod strip amp gt mm long plastic drop bottl fot anod cathod solut sampl applic mm viscos low protein adsorpt filter paper stainless steel scissor scalpel tweezer stainless steel glass stain destain dish mm instrument trai adjust rod homogen mm shaft diamet rpm rang magnet stirrer ultrason bath film welder μl micropipett vacuum concentr freez dryer thermostat control water bath adjust shaker densitomet equip read nm procedur sampl prepar isol casein weigh amount equival dry mass chees refer standard ml centrifug tube add distil water homogen rod homogen rpm adjust ph dil acet acid centrifug minut decant fat whei homogen residu rpm ml distil water adjust ph dil acet acid add ml dichloromethan homogen centrifug minut remov casein layer li aqueou organ phase figur spatula decant phase rehomogen casein ml distil water ml dichloromethan centrifug repeat procedur extract phase colourless time homogen protein residu ml aceton filter medium speed fold filter paper wash residu filter separ ml portion aceton time dry air stream nitrogen pulver fine mortar note dry casein isol plasmin cleavag casein intensifi casein dispers mg isol casein ml ammonium carbon buffer homogen minut ultrason treatment heat add μl plasmin mix incub hour continu shake inhibit enzym add μl aminopro acid solut add mg solid urea mg dithiothreitol note obtain symmetri focus casein band advis freez dry solut ad aminocapro acid dissolv residu ml protein dissolv buffer prepar urea polyacrylamid gel aid drop water roll gel carrier sheet glass plate remov extran water paper towel tissu roll cover sheet spacer mm glass plate lai plate horizont level tabl add μl teme prepar de aerat gel solut stir add μl solut mix immedi pour evenli centr cover sheet place edg gel carrier plate sheet side cover sheet plate lower slowli gel film form sheet spread regularli free bubbl figur carefulli lower gel carrier plate complet thin spatula place glass plate top act weight polymer complet minut remov gel polymer gel carrier sheet cover sheet tip glass plate clean revers carrier sheet carefulli remov gel residu urea weld gel sandwich film tube store refriger maximum week note cover sheet spacer polyacrylamid gel cut smaller size recommend sampl automat electrophoresi devic gel size cm lsoelectr focus set cool thermostat wipe revers gel carrier sheet kerosen drip drop kerosen centr cool block roll gel sandwich carrier side take care avoid bubbl wipe excess kerosen remov cover sheet soak electrod strip electrod solut cut gel length place posit provid distanc electrod cm condit isoelectr focus gel size mm gt tabl gt note thick width gel chang valu current power suitabl adjust doubl valu electr current power mm gel voltag programm automat electrophoresi devic gel cm electrod strip appli directli gel gt tabl gt place sampl applic step vh remov sampl applic step vh protein stain protein fixat remov electrod strip immedi turn power put gel immedi stain destain dish fill ml fix leav minut shake continu wash stain gel plate drain fix wash gel plate second time ml destain solut pour destain solut fill dish ml stain solut stain minut gentl shake destain gel plate pour stain solut wash gel plate ml destain solut time shake ml destain solut minut repeat destain step time background clear uncolour rins gel plate distil water minut dry air hour hairdryer minut note carri fix wash stain destain elev temperatur note sensit silver stain silver stain kit protein pharmacia biotech code prefer plasmin treat casein sampl dilut mg ml evalu evalu perform compar protein pattern unknown sampl refer standard gel detect cow milk chees ew milk goat milk buffalo milk mixtur ew goat buffalo milk casein isolelectr point rang ph ph figur figur detect limit visual estim visual evalu amount bovin milk advis adjust concentr sampl standard obtain level intens ovin caprin buffalo casein quot quot quot quot figur figur amount bovin milk equal greater unknown sampl judg directli compar intens bovin casein quot quot quot quot figur figur refer standard ew goat laboratori interim standard buffalo densitometr estim appli densitometri determin peak area ratio bovin ovin caprin buffalo casein figur compar casein peak area ratio refer standard ew goat laboratori interim standard buffalo analys gel note method oper satisfactorili clear posit signal bovin casein refer standard refer standard optim procedur detail method precis sampl judg posit bovin casein peak area ratio equal greater level refer standard refer addeo moio chianes stingo resmini berner kraus di luccia bocca plasmin increas sensit detect bovin milk ovin caprin chees gel isoelectr focus casein milchwissenschaft addeo nicolai chianes moio spagna musso bocca del giovin control method detect bovin milk ew water buffalo chees immunoblot milchwissenschaft kraus berner klostermey sensit detect cow milk ew goat milk chees carrier ampholyt carrier ampholyt immobil ph gradient isoelectr focus casein plasmin signal amplifi electrophoresi forum radola ed pp bode verlag münchen kraus belitz kaiser nachwei von kuhmilch schaf ziegenmilch bzw käse durch isoelektrisch fokussierung harnstoffhaltigen polyacrylamidgelen lebensm unter forsch radola ultrathin layer isoelectr focus μm polyacrylamid gel silanis glass plate polyest film electrophoresi figur schemat draw cover sheet gt pic file quot en ep quot gt figur casein layer float aqueou organ phase centrifug gt pic file quot en ep quot gt figur flap techniqu cast ultrathin polyacrylamid gel gt pic file quot en ep quot gt spacer tape mm cover sheet glass plate gel solut gel carrier sheet figur isoelectr focus plasmin treat casein ew goat milk chees amount cow milk gt pic file quot en ep quot gt cm percentag cow milk cow ew goat upper half ief gel shown figur isoelectr focus plasmin treat casein chees made mixtur ew goat buffalo milk amount cow milk gt pic file quot en ep quot gt cm percentag cow milk sampl cow milk spike pure bovin casein middl track cow ew goat buffalo total separ distanc ief gel shown figur surperposit densitogram standard std chees sampl made mixtur ew goat milk isoelectr focus gt pic file quot en ep quot gt standard cow milk chees sampl cow milk cow ew goat upper half ief gel scan nm produc ampholin ph pharmacia resolyt ph ph bdh merck prove suitabl obtain requir separ casein produc ampholin ph pharmacia resolyt ph ph bdh merck prove suitabl obtain requir separ casein produc ampholin ph pharmacia resolyt ph ph bdh merck prove suitabl obtain requir separ casein annex xvi articl refer method detect coliform butter skim milk powder casein casein sampl butter inocul cultur medium butter test presenc coliform skim milk powder casein casein test presenc coliform sampl inocul cultur medium idf standard method appli modif sampl prepar idf standard acid casein sampl prepar procedur idf standard altern tube inocul sampl butter sampl skim milk powder casein casein incub evalu decim dilut made evalu result gt tabl gt remark coliform content butter skim milk powder casein casein averag result indic requir fulfil obtain probabl coliform content butter skim milk powder casein casein averag result indic requir fulfil obtain probabl assumpt poisson distribut annex xvii articl method determin lactos content product fall cn code part field applic method appli case lactos content exce principl dissolv sugar water yeast saccharomyc cerevisia act leav lactos intact determin lactos content solut luff schoorl method clarif filter reagent sodium thiosulph indic starch solut add mixtur solubl starch mg mercur iodid ad preserv agent ml water litr boil water mixtur boil minut leav cool potassium iodid solut ar sulphur acid solut luff schoorl reagent dissolv iron free copper ii sulphat pentahydr cuso ml water dissolv citric acid monohydr ml water dissolv anhydr sodium carbon na ml hot water cool add shake gentli add make litr stand overnight filter check normal reagent obtain cu na ph approxim carrez solut dissolv zn glacial acet acid water make ml carrez ii dissolv de cn water make ml grain pumic stone treat boil hydrochlor acid wash water dri suspens saccharomyc cerevisa fresh yeast ml water week refriger procedur weigh nearest mg sampl analysi place calibr ml flask add ml water place flask boil waterbath thirti minut cool approxim add ml yeast suspens shake leav calibr flask content waterbath temperatur hour ferment cool temperatur approxim add ml carrez solut shake thirti second add ml carrez ii solut shake thirti second make ml water mix filter pipett quantiti filtrat ml prefer mg lactos make ml water determin anhydr lactos content luff schoorl method carri complet blank test yeast part ii determin lactos content luff schoorl method pipett ml luff schoorl reagent place erlenmey flask ml add ml clarifi solut measur ad grain pumic stone heat shake hand nake flame averag height bring liquid boil approxim minut immedi place erlenmey flask wire gauz asbesto screen flame previous lit regul erlenmey flask heat sole bottom fit reflux condens moment boil ten minut cool immedi cold water approxim minut test add liquid ml potassium iodid immedi caution consider foam occur ml sulphur acid test sodium thiosulph dull yellow colour appear end test add starch indic carri test mixtur precis ml luff schoorl reagent ml water ad ml potassium iodid ml sulphur acid time bring boil tabl establish amount mg lactos differ result test express ml sodium thiosulph tabl tabl ml de luff schoorl reagent condit text sodium thiosulph lactos gt tabl gt regul eec product ferment sugar increas quantiti suspens annex xviii articl detect rennet whei skim milk powder public storag determin glycomacropeptid high perform liquid chromatographi hplc scope field applic method detect rennet whei skim milk powder intend public storag determin glycomacropeptid refer intern standard iso milk milk product method sampl conform guidelin contain annex paragraph definit glycomacropeptid content skim milk powder content substanc determin method set express percentag mass principl reconstitut skim milk powder remov fat protein trichloroacet acid centrifug determin quantiti glycomacropeptid gmp supernat high perform liquid chromatographi hplc evalu result obtain sampl refer standard sampl consist skim milk powder addit percentag whei powder reagent reagent recognis analyt grade water distil water water equival puriti tricloroacet acid solut dissolv trichloroacet acid cl ccooh water make ml eluent solut ph dissolv dipotassium hydrogen phosphat hpo potassium dihydrogen phosphat kh po sodium sulphat na ml water adjust ph solut phosphor acid potassium hydroxid make ml water homogenis filter eluent solut prior membran filter μm pore diamet flush solvent mix volum acetonitril ch cn volum water filter mixtur prior membran filter μm pore diamet note flush solvent bactericid effect impair column resolut effici standard sampl skim milk powder meet requir resolut skim milk powder adulter rennet type whei powder standard composit apparatu analyt balanc centrifug capabl attain centrifug forc fit stopper centrifug tube ml capac mechan shaker magnet stirrer glass funnel diamet cm filter paper medium filtrat diamet cm glass filtrat equip μm pore diamet membran filter graduat pipett allow deliveri ml iso class iso thermostat waterbath set hplc equip consist pump injector hand automat μl capac tsk sw column seri length cm intern diamet cm equival column precolumn cm cm pack materi equival effect thermostat column oven set variabl wavelength uv detector permit measur nm sensit integr capabl vallei vallei integr note work column room temperatur power resolut slightli lower case temperatur vari rang analys sampl intern standard iso quot milk milk product method sampl quot conform guidelin contain annex paragraph store sampl condit preclud deterior chang composit procedur prepar test sampl transfer milk powder contain capac volum powder fit airtight lid close contain immedi mix milk powder mean repeat invers contain test portion weight test sampl centrifug tube remov fat protein add warm water test portion dissolv powder shake minut mechan shaker cool tube add ml trichloroacet acid solut minut stir aid magnet stirrer place tube waterbath leav minut centrifug minut filter paper discard ml filtrat chromatograph determin inject μl accur measur supernat filtrat hplc apparatu oper flow rate ml eluent solut minut note eluent solut chromatograph analysi order eluent degass prevent bacteri growth precaut similar effect rins column water interrupt leav eluent solut prior interrupt hour rins column water wash solut hour flow rate ml minut result chromatograph analysi test sampl obtain form chromatogram peak identifi retent time rt gt tabl gt qualiti column effect retent time individu peak integr automat calcul area peak gt tabl gt essenti examin appear chromatogram prior quantit interpret order detect abnorm due malfunct apparatu column origin natur sampl analys doubt repeat analysi calibr appli procedur point point standard sampl freshli prepar solut gmp degrad trichloroacet environ loss estim hour prior chromatograph determin sampl condit column repeatedli inject standard sampl solut area retent time peak gmp constant determin respons factor inject volum filtrat sampl express result method calcul formula calcul respons factor gt tabl gt rii riv respons factor peak ii iv aii aiv area peak ii iv standard sampl obtain gt tabl gt riii respons factor peak iii aiii aiii area peak iii standard sampl obtain quantiti whei standard sampl calcul rel area peak sampl gt refer graphic gt gt refer graphic gt gt refer graphic gt sii siii siv rel area peak ii iii iv sampl aii aiii aiv area peak ii iii iv sampl obtain rii riii riv respons factor calcul calcul rel retent time peak iii sampl gt refer graphic gt rrtiii rel retent time peak iii sampl rtiii retent time peak iii sampl obtain rtiii retent time peak iii control sampl obtain experi shown linear relat rel retent time peak iii rrtiii percentag whei powder ad rrtiii amp lt whei content amp gt rrtiii amp gt whei content amp lt uncertainti allow valu rrtiii rrtiii deviat depend condit column approach greater calcul percentag rennet whei powder sampl gt refer graphic gt gt tabl gt accuraci procedur repeat differ result determin carri simultan rapid success analyst apparatu ident test materi exce reproduc differ singl independ result obtain laboratori ident test materi exce interpret assum absenc whei rel area peak iii siii express gram rennet whei product amp lt gt refer graphic gt gt tabl gt rel area peak iii siii amp gt gt refer graphic gt rel area peak ii sii amp lt determin rennet whei content point rel area peak iii siii amp gt gt refer graphic gt rel area peak ii sii amp lt determin total protein content examin graph data obtain analysi sampl unadulter skim milk powder high total protein content assembl graph continu line repres linear regress coeffici calcul squar method dash straight line fix upper limit rel area peak iii probabl exceed case equat dash straight line graph gt tabl gt gt tabl gt equat equival figur mention point discrep rel area siii found rel area siii mean gt refer graphic gt gt refer graphic gt gt tabl gt rennet whei content calcul formula gt refer graphic gt distanc vertic axi continu dot straight line gt pic file quot en ep quot gt annex xix articl determin rennet whei solid skim milk powder mixtur refer regul ec purpos detect addit rennet whei solid skim milk powder defin articl regul ec mixtur defin articl regul ec refer intern standard iso definit content rennet whei solid defin percentag mass determin procedur principl glycomacropeptid content determin accord annex xviii sampl give posit result analys glycomacropeptid revers phase high perform liquid chromatographi procedur hplc procedur evalu result obtain refer standard sampl consist skim milk powder percentag whei powder result higher show rennet whei solid present reagent reagent recognis analyt grade water distil water water equival puriti acetonitril spectroscop hplc qualiti reagent need procedur annex xviii regul reagent revers phase hplc trichloroacet acid solut dissolv trichloroacet acid cci ccooh water make ml eluent eluent ml acetonitril ch cn ml isopropanol ch chohch ml trifluoroacet acid tfa cf cooh ml volumetr flask make ml water eluent ml acetonitril ml isopropanol ml tfa ml volumetr flask make ml water filter eluent solut prior membran filter μm pore diamet conserv column analys column flush eluent gradient subsequ flush acetonitril gradient minut column store acetonitril standard sampl skim milk powder meet requir public storag skim milk powder adulter rennet type whei powder standard composit skim milk powder adulter rennet type whei powder standard composit apparatu apparatu need procedur annex xviii regul analyt balanc centrifug capabl attain centrifug forc fit stopper centrifug tube ml capac mechan shaker provis shake magnet stirrer glass funnel diamet cm filter paper medium filtrat diamet cm glass filtrat equip μm pore diamet membran filter graduat pipett allow deliveri ml iso class iso system capabl deliv ml minut thermostat waterbath set hplc equip consist binari gradient pump system injector hand automat μl capac dupont protein column length cm cm intern diamet equival wide pore silica base revers phase column thermostat column oven set variabl wavelength uv detector permit measur nm higher wavelength nm sensit integr capabl vallei vallei integr note oper column room temperatur provid room temperatur fluctuat variat retent time gmpå take place sampl sampl accord procedur laid intern standard iso member state method sampl provid compli principl abovement standard store sampl condit preclud deterior chang composit procedur prepar test sampl transfer milk powder contain capac volum powder fit airtight lid close contain immedi mix milk powder mean repeat invers contain test portion weigh test sampl centrifug tube suitabl stopper flask ml remov fat protein add warm water test portion dissolv powder shake minut minut case acid buttermilk mechan shaker place tube waterbath equilibr add ml trichloroacet acid solut constantli minut stir vigor aid magnet stirrer place tube waterbath leav minut centrifug minut filter paper discard ml filtrat chromatograph determin perform hplc analysi annex xviii neg result obtain sampl analys rennet whei solid detect amount result posit revers phase hplc procedur appli presenc acid buttermilk powder give rise fals posit result revers phase hplc method exclud possibl revers phase hplc analysi carri gradient condit optimis retent time minut gmpa optim gradient system dead volum ml volum point solvent volum injector loop inclus gradient system lower dead volum ml minut optim retent time solut standard sampl rennet whei inject μl supernat filtrat hplc apparatu oper scout gradient condit tabl tabl scout gradient condit optimis chromatographi gt tabl gt comparison chromatogram reveal locat peak gmpα formula initi solvent composit normal gradient calcul gt refer graphic gt gt refer graphic gt rtgmpa retent time gmpα scout gradient initi scout gradient midpoint minu initi normal gradient midpoint time scout gradient requir retent time gmpα ratio slope scout normal gradient initi minu minut scout gradient run time scout gradient solut test sampl inject μl accur measur supernat filtrat hplc apparatu oper flow rate ml eluent solut minut composit eluent start analysi obtain close immedi inject linear gradient start result higher percentag minut subsequ linear gradient start bring eluent composit minut composit maintain minut composit chang linear gradient minut initi composit depend intern volum pump system inject made minut reach initi condit remark retent time glycomacropeptid minut achiev vari initi end condit gradient differ initi end condit gradient remain eluent degass suffici remain degass essenti proper function gradient pump system standard deviat retent time gmp peak smaller minut sampl refer sampl inject calcul respons factor result chromatograph analysi test sampl obtain form chromatogram gmp peak identifi retent time minut integr automat calcul peak height gmp peak baselin locat check chromatogram analysi integr repeat baselin incorrectli locat essenti examin appear chromatogram prior quantit interpret order detect abnorm due malfunct apparatu column origin natur sampl analys doubt repeat analysi calibr appli procedur point point standard sampl freshli prepar solut gmp degrad trichloroacet acid environ room temperatur solut remain stabl hour case long seri analys cool sampl trai automat injector desir note omit initi condit previou analys chromatogram refer sampl analog figur figur gmpa peak preced small peak essenti obtain similar separ prior chromatograph determin sampl inject μl standard sampl rennet whei chromatogram show peak retent time gmpa peak determin respons factor inject volum filtrat sampl express result method calcul formula calcul respons factor gmp peak hwhere respons factor gmp peak height gmp peak quantiti whei standard sampl calcul percentag rennet whei powder sampl percentag rennet whei sampl respons factor gmp peak height gmp peak sampl greater differ retent time standard sampl smaller minut rennet whei solid present accuraci procedur repeat differ result determin carri simultan rapid success analyst apparatu ident test materi exce reproduc determin linear rennet whei linear relationship obtain coeffici correl amp gt interpret whei consid present result obtain higher retent time gmp peak differ minut standard sampl limit fix agreement provis point annex regul eec gt pic file quot en ep quot gt rennet type whei powder standard composit adulter skim milk powder nizo kernhemseweg po box nl ba ed powder give equival result nizo powder annex xx articl skim milk powder quantit determin phosphatidylserin phosphatidylethanolamin method revers phase hplc purpos field applic method describ procedur quantit determin phosphatidylserin ps phosphatidylethanolamin pe skim milk powder smp suitabl detect buttermilk solid smp definit ps pe content mass fraction substanc determin procedur result express milligram phosphatidylethanolamin dipalmitoyl pedp perr powder principl extract aminophospholipid methanol reconstitut milk powder determin ps pe phthaldialdehyd opa deriv revers phase rp hplc fluoresc detect quantitif ps pe content test sampl refer standard sampl amount pedp reagent reagent recognis analyt grade water distil equival puriti standard materi pedp pure note standard materi store reagent standard sampl test sampl prepar hplc grade methanol hplc grade chloroform tryptamin monohydrochlorid reagent phthaldialdehyd derivatis sodium hydroxid water solut boric acid water solut adjust ph sodium hydroxid mercaptoethanol phthaldialdehyd opa hplc elut solvent elut solvent prepar hplc grade reagent hplc grade water methanol fluorimetr test puriti tetrahydrofuran sodium dihydrogen phosphat sodium acet acet acid apparatu analyt balanc beaker ml capac pipett deliv ml magnet stirrer graduat pipett deliv ml volumetr flask ml capac syring μl capac ultrason bath centrifug oper glass vial ml capac graduat cylind ml capac ph meter hplc equip gradient pump system capabl oper ml min bar autosampl derivatis capabl column heater set fluoresc detector set nm excit wavelength nm emiss wavelength integr data process softwar capabl peak area measur lichrospher column mm equival column pack octadecylsilan μm particl size sampl sampl carri accord idf standard procedur prepar intern standard solut weigh mg tryptamin monohydrochlorid ml volumetr flask make mark methanol pipett ml solut ml volumetr flask make mark methanol order obtain mm tryptamin concentr prepar test sampl solut weigh smp sampl ml beaker add ml distil water pipett stir magnet stirrer minut order dissolv lump pipett ml reconstitut milk ml volumetr flask add μl mm tryptamin solut syring make volum methanol mix carefulli invers sonic min centrifug minut collect supernat glass vial note test sampl solut store hplc analysi perform prepar extern standard solut weigh mg pedp ml volumetr flask add ml chloroform graduat cylind heat stopper flask mix carefulli till pedp dissolv cool flask make volum methanol mix invers pipett ml solut ml volumetr flask make volum methanol pipett ml solut ml volumetr flask add μl mm tryptamin solut make volum methanol mix invers note refer sampl solut store hplc analysi perform prepar derivatis reagent weigh mg opa ml volumetr flask add ml methanol mix carefulli dissolv opa make mark boric acid solut add μl mercaptoethanol syring note derivatis reagent store dark vial stabl week determin hplc elut solvent solvent solut mm sodium dihydrogen phosphat mm sodium acet solut adjust ph acet acid methanol tetrahydrofuran solvent methanol suggest elut gradient gt tabl gt note elut gradient requir slight modif order achiev resolut shown figur column temperatur inject volum μl derivatis reagent μl sampl solut column equilibr start system daili basi flush column solvent minut set equilibr ml min minut perform blank run inject methanol note long term storag flush column methanol chloroform minut determin ps pe content test sampl perform sequenc chromatograph analys keep constant run run time order obtain constant retent time inject extern standard solut test sampl solut order evalu respons factor note column clean flush solvent minut run integr mode pedp peak pedp elut singl peak determin peak area vallei vallei integr tryptamin peak tryptamin elut singl peak figur determin peak area vallei vallei integr ps pe peak group condit figur ps elut main partial unresolv peak preced minor peak pe elut main partial unresolv peak determin area peak cluster set baselin report figur calcul express result ps pe content test sampl calcul gt refer graphic gt ps pe content mg powder test sampl pedp peak area standard sampl solut ps pe peak area test sampl solut tryptamin peak area standard sampl solut tryptamin peak area test sampl solut precis note valu repeat calcul idf intern standard provision reproduc limit calcul procedur defin annex iii hereto repeat rel standard deriv repeat express variabl independ analyt result obtain oper apparatu condit test sampl short interv time exce rel determin obtain condit rel differ result greater arithmet result reproduc determin obtain oper laboratori apparatu condit analysi test sampl rel differ result greater arithmet result refer resmini pellegrino hogenboom sadini rampilli quot detect buttermilk solid skimmilk powder hplc quantif aminophospholipid quot sci tecn latt ca figur hplc pattern opa deriv phosphatidylserin ps phosphatidylethanolamin pe methanol extract reconstitut skim milk powder integr mode peak ps pe tryptamin intern standard report gt pic file quot en ep quot gt intern idf standard milk milk product precis characterist analyt method outlin collabor studi procedur annex xxi articl detect antibiot sulfonamid dapson residu skim milk powder microbi inhibitor screen test bacillu stearothermophilu var calidolacti test micro organ suffici sensit detect μg benzylpenicillin milk μg sulfadimidin milk commerci test kit requir sensit benzylpencillin sulfadimidin test reconstitut skim milk powder powder ml aqua dest test carri idf bulletin section chapter instruct test kit manufactur posit result interpret repeat test ad penicillinas test system posit result inhibit substanc identifi procedur neg result inhibit substanc lactam antibiot repeat test ad amino benzoic acid test system posit result inhibit substanc identifi procedur neg result inhibit substanc sulfonamid dapson repeat test ad pencillinas amino benzoic acid test system posit result inhibit substanc identifi procedur neg result inhibit substanc lactam antibiot sulfonamid dapson import notic fals posit result obtain skim milk powder analys import verifi test system yield fals posit result annex xxii articl quantit determin skim milk powder compound feedingstuff enzymat coagul para casein purpos quantit determin skim milk powder compound feedingstuff enzymat coagul para casein scope method appli compound feedingstuff skim milk powder larg quantiti buttermilk milk protein lead interfer principl method dissolv casein contain compound feedingstuff extract sodium citrat solut adjust calcium ion concentr requir level precipit para casein addit rennet para casein obtain casein nitrogen content para casein precipit determin kjeldahl method idf standard quantiti skim milk powder calcul basi minimum casein content reagent reagent analyt grade water distil water water equival puriti except rennet reagent solut free nitrogen substanc trisodium citrat dihydr solut calcium chlorid solut weigh caco analyt grade porcelain vessel suitabl size ml beaker cover distil water transfer boil water bath add slowli ml hcl solut conc hcl water solubilis carbon complet boil water bath cacl dri elimin hcl react transfer distil water ml measur flask dilut mark measur ph lower store solut refriger sodium hydroxid hydrochlor acid liquid calf rennet standard strength store refriger reagent quantit determin nitrogen kjeldahl method idf standard apparatu common laboratori apparatu includ mortar homogenis analyt balanc bench top centrifug rpm ml tube magnet stirrer mm follow ml beaker ml flask glass funnel mm diamet fast filter ashless filter diamet mm pipett nomin volum thermostat control water bath ph meter kjeldahl digest distil assembl fit ml graduat burett plastic wash bottl distil water stainless steel spatula thermomet temperatur control dry oven procedur prepar sampl grind mortar homogenis mill sampl obtain homogen mixtur dissolv milk powder separ insolubl residu weigh homogenis compound feedingstuff directli ml centrifug tube add ml trisodium citrat solut previous heat mix aid magnet stirrer minut centrifug rpm minut decant clear aqueou supernat ml beaker take care loos materi bottom carri extract residu procedur ad extract layer oil form surfac cool refriger fat solidifi remov solid layer spatula coagul casein enzym rennet stir continu add dropwis ml satur solut calcium chlorid total aqueou extract ml adjust ph solut naoh hcl place thermostat control water bath minut obtain salin balanc evid format light turbid transfer liquid centrifug tube centrifug minut order remov precipit materi transfer supernat wash sediment centrifug tube bring temperatur supernat back stir extract add dropwis ml liquid rennet coagul occur minut return sampl water bath leav temperatur minut remov sampl bath break coagulum stir centrifug minut filter supernat suitabl filter paper whatman equival retain filter paper wash precipit centrifug tube ml water approxim stir precipit centrifug minut filter supernat filter paper retain previous determin casein nitrogen wash transfer quantit precipit filter paper retain distil water transfer filter paper kjeldahl flask determin nitrogen kjeldahl method idf standard blank test blank test made regularli ashless filter paper moisten mixtur ml sodium citrat solut ml satur solut calcium chlorid ml liquid rennet wash ml distil water mineralis kjeldahl method idf standard volum acid blank test subtract volum acid titrat sampl control test test abovement procedur reagent make determin standard compound feedingstuff skim milk powder content establish collabor studi averag result duplic determin differ collabor studi express result percentag skim milk powder compound feedingstuff calcul formula gt refer graphic gt percentag para casein nitrogen factor convert determin casein percentag skim milk powder correct factor obtain regress analysi accuraci method repeat case studi duplic analysi sampl oper laboratori give differ result equival greater skim milk powder compound feedingstuff reproduc case studi sampl analys laboratori give differ result greater skim milk powder compound feedingstuff toler limit crd critic differ confid limit calcul formula iso gt refer graphic gt reproduc repeat doubl determin crd result chemic analysi differ declar content skim milk powder doubl determin consign compound feedingstuff deem compli provis regul observ addit larg percentag milk protein soya protein heat skim milk powder lead high result due precipit para casein milk addit buttermilk lead low figur due fact fat portion determin addit acid buttermilk give consider low figur due incomplet dissolv citrat solut lecithin addit lead low result incorpor high heat skim milk powder lead high figur due precipit whei protein para casein milk fast filter ashless paper annex xxiii articl qualit determin starch skim milk powder denatur milk powder compound feedingstuff scope method detect starch issu tracer denatur milk powder limit detect method approxim starch sampl principl reaction base iodometri fixat colloid free iodin aqueou solut absorpt starch micel colour format reagent iodin solut iodin potassium iodin distil water ml apparatu analyt balanc water bath test tube mm mm procedur weight sampl transfer test tube add ml distil water shake order dispers sampl place boil water bath leav minut remov bath cool room temperatur add ml iodin solut shake observ result colour express result blue colour presenc nativ starch sampl sampl modifi starch colour blue remark colour intens colour microscop appear starch vari depend origin nativ starch maiz potato type modifi starch present sampl presenc modifi starch colour produc turn violet red brown degre modif crystallin structur nativ starch annex xxiv articl determin moistur acid buttermilk powder scope determin moistur content acid buttermilk powder intend anim feedingstuff principl sampl dri vacuum loss mass determin weigh apparatu analyt balanc dry contain corrod metal glass lid ensur airtight closur work surfac allow test sampl spread cm adjust electr heat vacuum oven fit oil pump mechan introduc hot dri air dry agent calcium oxid desicc effici dry agent dry oven ventil thermostat control procedur heat contain lid oven hour place lid contain immedi transfer desicc cool room temperatur weigh nearest mg weigh contain lid nearest mg weight weight contain nearest mg sampl spread evenli place contain lid vacuum oven preheat prevent oven temperatur fall unduli introduc contain rapidli bring pressur torr kpa leav dry hour pressur current hot dry air dry agent sampl instanc disconnect vacuum pump prescrib pressur reach reckon dry time moment oven temperatur return carefulli bring oven back atmospher pressur open oven place lid contain immedi remov contain oven leav cool minut desicc weigh nearest mg dry addit minut vacuum oven reweigh differ weigh exce moistur calcul gt refer graphic gt initi mass gramm test sampl mass gramm dry test sampl precis repeat limit differ result determin carri shortest feasibl time interv oper apparatu ident test materi exce water acid buttermilk powder reproduc limit differ result determin carri oper laboratori apparatu ident test materi exce water acid buttermilk powder sourc precis data precis data determin experi conduct involv laboratori sampl blind duplic annex xxv articl refer method detect foreign fat milk fat ga chromatograph analysi triglycerid revis scope field applic standard lai method detect foreign fat veget fat anim fat beef tallow lard milk fat milk product ga chromatograph analysi triglycerid defin triglycerid formula veget anim fat qualit quantit detect pure milk fat irrespect feed lactat condit note butyr acid occur exclus milk fat enabl quantit estim low amount milk fat veget fat made qualit quantit inform provid rang addit weight foreign fat pure milk fat larg variat rang approxim weight note quantit result practic obtain triglycerid analys sterol content veget fat function product treatment condit definit foreign fat milk fat foreign fat defin standard veget anim fat milk fat principl method extract milk fat stock solut prepar solut triglycerid total carbon number determin ga chromatograph pack column insert weight fat molecul size number triglycerid formula foreign fat qualit detect quantit determin note observ evalu capillari ga chromatographi guarante compar result achiev reagent analysi grade chemic carrier ga nitrogen puriti degre ge standard triglycerid satur cholesterol standard standard milk fat section methanol water free hexan heptan toluen dimethylchlorosilan solut ml dimethylchlorosilan dissolv ml toluen combust ga hydrogen synthet air stationari phase ov μm mesh ga chromq cocoa butter solut instrument normal laboratori apparatu high temperatur ga chromatograph suit temperatur equip flame ioniz detector fid constant mass flow control carrier ga combust ga ml min ml min synthet air high carrier ga flow flame jet larg note high temperatur occur triglycerid analys glass insert fid injector system frequent clean ga chromatograph equip septa withstand high temperatur frequent exhibit gener low degre quot bleed quot note suit chromblu tm septa chrompack septa exchang regular interv roughli inject resolut deterior figur chromatographi column shape glass column insid diamet mm mm length silan section dimethylchlorosilan order deactiv glass surfac note suit longer mm length pack column slightli reproduc result achiev hand stationari phase exhibit occasion fractur oper lead turn wors quantit result fid flame easili extinguis result requir extrem high carrier ga flow ml min arrang fill column figur figur fill column gt pic file quot en ep quot gt plastic column screw end cap provid mark requir quantiti stationari phase fill fine siev mesh size approxim μm screw cap suit seal glass column figur deactiv silan glass wool vibrat uniform distribut stationari phase fill ml extrelut column silica gel column altern extract obtain milk fat graphit seal mm quot mm bore devic silan glass surfac column section woulff bottl water suction pump water bath adjust dry cabinet adjust microlitr pipett ml graduat pipett dose ml methanol ml round bottom flask erlenmey flask nomin volum ml funnel fine pore filter rotari evapor ampoul nomin volum ml sealabl aluminium cap septum interior inject syring plunger syring reach tip needl note syring reproduc result obtain oder avoid deterior septum tip needl check regular interv stereomicroscop procedur prepar column silan connect woulff bottl shown figur water suction pump tube dip solut section close stopcock column fill subsequ tube remov figur arrang silanis gt pic file quot en ep quot gt column fix stand complet fill dimethyldichlorosilan solut mean pipett min woulff bottl replac filter flask column empti connect water suction pump figur fill column success rins ml toluen ml methanol empti column dri dry cabinet approxim minut figur arrang rins gt pic file quot en ep quot gt fill column arrang repres figur stationari phase fill plastic column mark lower end glass column fill seal approxim cm long plug glass wool silan press steel rod end column close siev section column fill pressur bar stationari phase obtain uniform continu firm pack vibrat move glass column fill fill solid plug silan glass wool press end pack column protrud end cut plug press column millimetr spatula prepar sampl sampl prepar method isol milk fat butter butter melt suitabl vessel water bath section ml erlenmey flask funnel insert filter section heat dry cabinet fat layer molten butter sampl filter preheat devic milk fat phospholipid free extract fat fraction röse gottlieb method extract idf standard milk fat phospholipid cholesterol peak obtain increas approxim triglycerid spectrum standard cholesterol influenc neglig extent extract milk silica gel column ml milk sampl temper appli ml extrelut column microlitr pipett section allow distribut uniformli silica gel approxim minut denatur protein lipid complex ml methanol ad pipett subsequ sampl extract ml hexan hexan slowli ad small amount solvent drain collect ml round bottom flask dri constant weight extract led column drain empti eluat solvent distil rotatori evapor water bath temperatur flask dri fat yield determin weigh note fat extract gerber weibul berntrop schmid bondzynski ratzlaff isol milk fat deterg bdi method suit triglycerid analysi method larg quantiti partial glycerid phospholipid pass fat phase prepar sampl solut ga chromatographi solut fat heptan obtain section prepar sampl solut amount sampl materi obtain section weigh dissolv amount heptan sampl prepar section amount heptan ad sampl materi flask calcul basi weigh remain dissolv approxim ml sampl solut fill ampul section chromatograph triglycerid determin high temperatur elut long chain triglycerid increas baselin occur easili column adequ condit begin rise baselin high temperatur avoid complet combin column baselin subtract compens mode oper singl column glass insert injector detector graphit seal section baselin correct avoid baselin rise method combin column pack column compens mode baselin correct ga chromatograph applic run ga chromatograph inject fat solut subsequ subtract store baselin rise baselin avoid baselin correct integr softwar applic run integr system inject fat solut subsequ subtract store baselin rise baselin avoid baselin correct adequ condit adequ initi condit column approxim inject milk fat solut baselin rise high temperatur frequent low baselin correct inject techniqu avoid discrimin effect quot hot inject quot techniqu appli achiev quantit result high boil triglycerid compon fat solut drawn syring cold needl syring warm prior inject approxim second injector head τhen syring content rapidli inject note inject techniqu risk fraction phenomena insid syring inject block reduc quot column quot direct inject upper extend heat part column appli fragment septum accumul contamin easili elimin techniqu regularli chang injector insert dismount column bend tip needl caus touch bottom sampl beaker visibl ey alsolut avoid order damag septum figur triglycerid chromatogram milk fat sampl gt pic file quot en ep quot gt condit pack column step top column connect detector avoid contamin column fill section condit min ml min flow heat min ml min hold inject μl cocoa butter solut section respect temperatur program inject μm milk fat solut dai section note cocoa butter consist exclus high boil triglycerid inject cocoa butter serv purpos special condit long chain rang high boil triglycerid partli respons factor approxim occur repeat inject milk fat solut reduct initi high respons factor expect triglycerid low acyl number factor approxim pair column fill section prepar condit pair check milk fat analysi routin test pair quantit result respons factor respons factor amp gt column calibr calibr respons factor triglycerid cholesterol milk fat standard fat determin standard triglycerid satur triglycerid cholesterol addition intermedi respons factor found mathemat interpol standard fat calibr perform dai ident result obtain reproduc quantit result achiev triglycerid analysi sampl standard milk fat stock life month storag temperatur maxim standard note respons factor constitu determin standardis fat certifi triglycerid composit crm anhydr milk fat obtain institut refer materi measur geel belgium temperatur programm carrier ga condit triglycerid analysi temperatur programm initi column temperatur hold minut program min hold final temperatur minut detector injector temperatur note detector injector oven temperatur initi temperatur maintain constant level overnight weekend holidai carrier ga nitrogen flow rate ml min note cm column flow ml min carrier ga flow constantli maintain overnight weekend holidai exact carrier ga flow adjust manner independ column length elut durat analysi minut inject volum μl note syring rins time pure heptan inject fid condit section note flame ioniz detector ignit begin work dai integr evalu control measur condit triglycerid odd acyl number combin preced number triglycerid reproduc low content account remain triglycerid peak area chromatogram includ cholesterol peak multipli respect respons factor standard fat calibr altogeth normal free cholesterol triglycerid evalu result weight evalu chromatogram peak integr baselin plot reintegr optim integr paramet figur demonstr exampl triglycerid chromatogram figur show chromatogram evalu whilst figur repres sporad error rang baselin run incorrectli compar figur typic error detect high degre certainti avoid integr baselin plot figur easi evalu triglycerid chromatogram milk fat baselin drawn gt pic file quot en ep quot gt figur wrongli integr chromatogram milk fat gt pic file quot en ep quot gt control measur condit rel standard deviat rsd coeffici variat tabl triglycerid calcul consecut analys milk fat tabl rel standard deviat rsd triglycerid content gt tabl gt rsd consider higher valu tabl chromatograph condit septa carrier ga flow rate verifi small particl septum form deposit glass wool entranc column column unsuit result ag temperatur influenc figur note valu tabl mandatori indic qualiti control purpos higher rsd valu accept repeat reproduc limit point compli qualit foreign fat detect detect foreign fat triglycerid formula tabl limit tabl develop valu pure milk fat fluctuat limit transgress presenc foreign fat assum sensit formula detect lard addit gt refer graphic gt note milk fat sampl confid rang establish pure milk fat sampl standard deviat valu sd start triglycerid composit unknown fat sampl formula comput verifi simpl manner sum triglycerid content state factor fall rang foreign fat addit detect foreign fat tabl show triglycerid formula detect foreign fat soybean oil sunflow oil oliv oil rape seed oil linse oil wheat germ oil maiz germ oil cotton seed oil hydrogen fish oil veget fat coconut palm kernel fat palm oil beef tallow common formula triglycerid composit foreign fat subject fluctuat experiment measur foreign fat triglycerid data type foreign fat type favour limit consid tabl quot total formula quot similarli good result obtain foreign fat gt refer graphic gt calcul detect foreign fat combin milk fat shown formula lard tabl limit foreign fat low fat coconut fat palm oil palm kernel fat detect limit formula detect extrem high amount ad milk fat appli formula tabl tabl triglycerid formula detect foreign fat milk fat indic standard deviat sd formula soybean sunflow oliv rape seed linse wheat germ maiz germ cotton seed fish oil gt refer graphic gt formula coconut palm kernel fat gt refer graphic gt formula palm oil beef tallow gt refer graphic gt formula lard gt refer graphic gt check unknown fat sampl formula tabl total formula sampl mixtur milk fat foreign fat combin foreign fat insert triglycerid fat sampl analys obtain fall rang tabl formula sampl modifi milk fat detect foreign fat milk fat mean formula tabl conclus drawn type foreign fat admixtur tabl limit milk fat gt tabl gt tabl detect limit foreign fat confid column show minim detect limit milk fat formula tabl column detect limit total formula limit higher formula detect bit higher amount foreign fat formula combin foreign fat detect rang variat triglycerid foreign fat type consider influenc detect limit tabl limit detect addit foreign fat milk fat gt tabl gt note rang calcul foreign fat assum limit individu formula exceed tabl quantit foreign fat determin order obtain quantit inform foreign fat concentr milk fat sampl formula gt refer graphic gt quantiti unknown foreign fat foreign fat mixtur unknown milk fat result addit unknown foreign fat insert triglycerid foreign fat milk fat mixtur total triglycerid formula unknown foreign fat ad milk fat foreign fat total formula chosen sf obtain insert triglycerid data pure foreign fat formula calcul sf good quantit result foreign fat addit obtain palm oil beef tallow formula tabl sf foreign fat type sf valu insert formula respect foreign fat formula tabl chosen tabl sf valu foreign fat gt tabl gt rang applic detect method method appli bulk milk base repres milk fat sampl highli specif detect repres number milk fat formula deriv countri suit possibl detect obtain countri formula set repres number milk fat case complex comput programm requir triglycerid combin tabl appli factor redetermin method squar appli rang shown tabl formula feed condit instanc underfeed feed cow feed yeast ca soap gener applic case extrem feed condit high uptak pure feed oil high administr ca soap combin feed fat formula partli modifi milk fat note fraction milk fat gener recogn unmodifi milk fat modif assum limit exceed fraction milk fat unusu milk fat composit case hard fraction obtain fraction physic method high temperatur approxim low yield percent fraction overcrit formula modif milk fat fraction detect procedur differenti scan calorimetri accuraci method determin milk fat basi formula tabl rang tabl repeat differ valu determin carri shortest feasibl time interv oper procedur ident sampl materi condit person instrument devic laboratori tabl repeat limit formula gt tabl gt reproduc differ valu determin carri oper laboratori procedur ident sampl materi condit person instrument time tabl reproduc limit formula gt tabl gt critic differ repeat reproduc limit critic differ rang tabl calcul duplic analys respect valu tabl tabl critic differ triglycerid formula gt tabl gt accept result calibr round decim calcul triglycerid content cholesterol normal result duplic analysi check repeat absolut differ result triglycerid formula transgress repeat limit tabl repeat requir met control optim ga chromatograph condit qualiti column guarante repetit run differ maximum minimum valu triglycerid formula transgress rang run literatur repeat limit formula tabl quot standard gt tabl gt refer commiss european commun detect foreign fat milk fat mean ga chromatograph triglycerid analysi doc vi en vi commiss european commun control butter fat puriti sampl feed period eec countri doc vi commiss european commun consider result fourth sixth eec collabor trial determin triglycerid milk fat doc vi vi vi vi vi vi timm detect quantif milk fat mixtur milk milk fat dairi research precht hein nachwei von modifiziertem milchfett mit der triglyceridanalys fremdfettnachwei im milchfett mit hilf von triglyceridkombinationen luf stock brandl zum nachwei von fremdfett milchfett über die trigylceridanalys österr milchwirtsch wissensch beilag precht bestimmung von pflanzlichen fetten oder tierischen depotfetten milchfett kieler milchwirtsch forschungsb precht schnell extrakt von milchfett kieler milchwirtsch forschungsb precht schnell gaschromatographisch triglyceridanalys von milchfett kieler milchwirtsch forschungsb precht control milk fat puriti ga chromatograph triglycerid analysi kieler milchwirtsch forschungsb precht detect adulter milk fat fatti acid triglycerid analysi fat sci technol precht detect foreign fat milk fat qualit detect triacylglycerol formula ii quantit evalu foreign fat mixtur lebensm unter forsch precht ga chromatographi triacylglycerol lipid pack column crc handbook chromatographi analysi lipid ed mukherje weber sherma crc press boca raton precht molkentin quantit triglycerid analysi short capillari column chrompack new molkentin precht comparison pack capillari column quantit ga chromatographi triglycerid milk fat chromatographia stang angewandt statistik erster teil eindimensional problem springer verlag berlin suit method precht molkentin quantit triglycerid analysi short capillari column chrompack new suitabl product commerci trade name extrelut ga chromq chrompack exampl suit product specialis trade inform serv purpos easi handl standard user repres request product indic grain transfer si unit μm bs quot british standard specif test siev quot footnot page annex xxvi list regul refer recit commiss regul eec august lai method determin lactos content compound feed stuff import countri amend commiss regul eec decemb amend measur applic common market organis milk milk product sector introduct combin nomenclatur commiss regul eec decemb establish refer method determin sitosterol stigmasterol butteroil amend commiss regul ec amend regul eec ec ec ec establish refer method determin tracer butter butteroil cream commiss regul ec januari establish refer method determin sitosterol stigmasterol butter amend regul ec commiss regul ec novemb establish rule applic refer routin method analysi qualiti evalu milk milk product common market organis commiss regul ec june establish refer method detect coliform butter skim milk powder casein casein commiss regul ec june establish refer method detect cow milk casein chees made ew milk goat milk buffalo milk mixtur ew goat buffalo milk repeal regul eec commiss regul ec june establish refer method determin ethyl ester beta apo caroten acid concentr butter butter amend regul ec commiss regul ec septemb establish list refer method appli analysi qualiti evalu milk milk product common market organis amend regul ec commiss regul ec april establish refer method determin water solid fat fat content butter commiss regul ec juli establish refer method determin vanillin concentr butter butter cream amend regul ec oj oj oj oj oj oj oj oj oj oj oj oj oj