commiss decis august implement council direct ec perform analyt method interpret result notifi document number text eea relev ec commiss european commun regard treati establish european commun regard council direct ec april measur monitor substanc residu thereof live anim anim product repeal direct eec eec decis eec eec subparagraph articl thereof presenc residu product anim origin matter concern public health commiss decis ec februari lai detail rule offici sampl monitor substanc residu thereof live anim anim product analysi sampl carri exclus laboratori approv offici residu control compet nation author ensur qualiti compar analyt result gener laboratori approv offici residu control achiev qualiti assur system specif appli method valid common procedur perform criteria ensur traceabl common standard standard commonli agre council direct eec octob subject addit measur offici control foodstuff decis ec requir offici control laboratori accredit iso januari onward pursuant decis ec particip internation recognis extern qualiti control assess accredit scheme requir approv laboratori approv laboratori prove compet regular success particip adequ profici test scheme recognis organis nation commun refer laboratori network commun refer laboratori nation refer laboratori nation control laboratori oper direct ec enhanc coordin result advanc analyt chemistri adopt direct ec concept routin method refer method supersed criteria approach perform criteria procedur valid screen confirmatori method establish determin common criteria interpret test result offici control laboratori order ensur harmonis implement direct ec provid progress establish minimum requir perform limit mrpl analyt method substanc permit limit establish substanc authoris specif prohibit commun order ensur harmonis implement direct ec commiss decis eec septemb lai refer method detect residu heavi metal arsen commiss decis eec lai method detect residu substanc hormon thyrostat action commiss decis eec april lai refer method list nation refer laboratori detect residu amend decis ec examin order account develop scientif technic knowledg found outdat scope provis repeal decis order method analysi offici sampl adapt provis decis transit period laid measur provid decis accord opinion stand committe food chain anim health adopt decis articl subject matter scope decis rule analyt method test offici sampl pursuant articl sentenc direct ec specifi common criteria interpret analyt result offici control laboratori sampl decis appli substanc specif rule laid commun legisl articl definit purpos decis definit direct ec annex decis appli articl analyt method member state ensur offici sampl pursuant direct ec analys method document test instruct prefer iso compli part annex decis valid procedur part annex compli relev minimum requir perform limit mrpl establish accord articl articl minimum requir perform limit present decis review progress establish minimum requir perform limit mrpl analyt method substanc permit limit establish articl qualiti control member state ensur qualiti result analysi sampl pursuant direct ec monitor test calibr result chapter iso articl interpret result result analysi consid compliant decis limit confirmatori method analyt exceed permit limit establish substanc decis limit concentr decid statist certainti permit limit exceed permit limit establish substanc decis limit lowest concentr level method discrimin statist certainti analyt present substanc list group annex direct ec error lower substanc error lower articl repeal decis eec eec eec repeal articl transit provis method analysi offici sampl substanc list group annex direct ec satisfi criteria set decis eec eec eec year decis enter forc method appli substanc list group annex direct ec compli decis latest year date applic decis articl date applic decis appli septemb articl addresse decis address member state brussel august commiss david byrn member commiss oj oj oj oj oj oj oj annex perform criteria requir procedur analyt method definit accuraci mean close agreement test result accept refer determin determin trueness precis alpha error mean probabl test sampl compliant compliant measur obtain fals compliant decis analyt mean substanc detect identifi quantifi deriv emerg analysi beta error mean probabl test sampl compliant compliant measur obtain fals compliant decis bia mean differ expect test result accept refer calibr standard mean devic measur repres quantiti substanc interest ti refer base certifi refer materi crm mean materi analyt content assign chromatographi mean procedur extract prior chromatograph step divid part part chromatograph part mix standard analyt measur mixtur chromatograph amount ad standard analyt similar estim amount analyt extract method design improv identif analyt chromatograph method suitabl intern standard collabor studi mean analys sampl method determin perform characterist method studi cover random measur error laboratori bia confirmatori method mean method provid full complementari inform enabl substanc unequivoc identifi quantifi level interest decis limit ccα mean limit conclud error probabl sampl compliant detect capabl ccβ mean smallest content substanc detect identifi quantifi sampl error probabl case substanc permit limit establish detect capabl lowest concentr method detect contamin sampl statist certainti case substanc establish permit limit mean detect capabl concentr method detect permit limit concentr statist certainti fortifi sampl materi mean sampl enrich amount analyt detect interlaboratori studi comparison mean organis perform evalu test sampl laboratori accord predetermin condit determin test perform purpos studi classifi collabor studi profici studi intern standard mean substanc contain sampl physic chemic properti similar analyt identifi ad sampl calibr standard laboratori sampl mean sampl prepar send laboratori intend inspect test level interest mean concentr substanc analyt sampl signific determin complianc legisl minimum requir perform limit mrpl mean minimum content analyt sampl detect confirm intend harmonis analyt perform method substanc permit limit establish perform characterist mean function qualiti attribut analyt method instanc specif accuraci trueness precis repeat reproduc recoveri detect capabl rugged perform criteria mean requir perform characterist judg analyt method fit purpos gener reliabl result permit limit mean maximum residu limit maximum level maximum toler substanc establish commun legisl precis mean close agreement independ test result obtain stipul predetermin condit measur precis express term imprecis comput standard deviat test result precis determin larger standard deviat profici studi mean analys sampl allow laboratori choos method provid method routin condit studi perform iso guid assess reproduc method qualit method mean analyt method identifi substanc basi chemic biolog physic properti quantit method mean analyt method determin amount mass fraction substanc express numer unit reagent blank determin mean complet analyt procedur appli test portion equival amount suitabl solvent place test portion recoveri mean percentag true concentr substanc recov analyt procedur determin valid certifi refer materi refer materi mean materi properti confirm valid method calibr apparatu verifi method measur repeat mean precis repeat condit repeat condit mean condit independ test result obtain method ident test item laboratori oper equip reproduc mean precis reproduc condit reproduc condit mean condit test result obtain method ident test item laboratori oper equip rugged mean suscept analyt method experiment condit express list sampl materi analyt storag condit environment sampl prepar condit method appli present minor modif experiment condit practic subject fluctuat stabil reagent composit sampl ph temperatur variat affect analyt result sampl blank determin mean complet analyt procedur appli test portion sampl analyt absent screen method mean method detect presenc substanc class substanc level interest method capabl high sampl throughput sift larg number sampl potenti compliant result specif design avoid fals compliant result singl laboratori studi hous valid mean analyt studi involv singl laboratori method analys test materi condit justifi long time interv specif mean abil method distinguish analyt measur substanc characterist predominantli function measur techniqu vari class compound matrix standard addit mean procedur test sampl divid test portion portion analys amount standard analyt ad test portion analysi amount standard analyt ad time estim amount analyt sampl procedur design determin content analyt sampl take account recoveri analyt procedur standard analyt mean analyt certifi content puriti refer analysi substanc mean matter definit chemic constitut metabolit test portion mean quantiti materi drawn test sampl test observ carri test sampl mean sampl prepar laboratori sampl test portion trueness mean close agreement averag obtain larg seri test result accept refer trueness express bia unit mean unit iso direct ec valid mean confirm examin provis effect evid requir specif intend fulfil laboratori reproduc mean precis obtain laboratori stipul predetermin condit method test materi oper environ justifi long time interv perform criteria requir analyt method analyt method combin method screen confirmatori purpos proven fulfil relev requir establish decis gener requir handl sampl sampl obtain handl process maximum chanc detect substanc sampl handl procedur prevent possibl accident contamin loss analyt perform test recoveri analysi sampl recoveri determin batch sampl fix recoveri correct factor recoveri limit fix correct factor recoveri factor obtain specif batch specif recoveri factor analyt sampl appli case standard addit procedur intern standard quantit determin analyt sampl specif method distinguish analyt substanc experiment condit estim extent provid strategi overcom forese interfer substanc measur techniqu homologu analogu metabol product residu interest emploi prime import interfer aris matrix compon investig screen method analyt techniqu demonstr document traceabl manner valid fals compliant rate amp lt error level interest screen purpos conform direct ec case suspect compliant result result confirm confirmatori method confirmatori method organ residu contamin confirmatori method organ residu contamin provid inform chemic structur analyt method base chromatograph analysi spectrometr detect suitabl confirmatori method singl techniqu lack suffici specif desir specif achiev analyt procedur consist suitabl combin clean chromatograph separ spectrometr detect method method combin consid suitabl identif organ residu contamin substanc group tabl suitabl confirmatori method organ residu contamin gt tabl gt common perform criteria requir confirmatori method provid inform chemic structur analyt compound respons method discrimin compound method base chromatograph analysi spectrometr detect suitabl confirmatori method method suitabl intern standard ad test portion begin extract procedur depend avail stabl isotop label form analyt suit mass spectrometr detect compound structur relat analyt suitabl intern standard identif analyt confirm chromatographi case peak obtain enhanc peak height area equival amount ad analyt ga chromatographi gc liquid chromatographi lc peak width half maximum height rang origin width retent time ident margin thin layer chromatographi tlc method spot presum due analyt intensifi spot visual appear chang refer fortifi materi amount analyt permit limit decis limit compliant control sampl compliant control materi reagent blank prefer carri entir procedur simultan batch test sampl analys order inject extract analyt instrument reagent blank compliant control sampl sampl confirm compliant control sampl final compliant control sampl variat sequenc justifi addit perform criteria requir quantit method analysi trueness quantit method case repeat analys certifi refer materi guidelin rang deviat experiment determin recoveri correct mass fraction certifi tabl minimum trueness quantit method gt tabl gt crm accept trueness measur assess recoveri addit amount analyt blank matrix data correct recoveri accept fall rang shown tabl precis quantit method inter laboratori coeffici variat cv repeat analysi refer fortifi materi reproduc condit exce level calcul horwitz equat equat gt refer graphic gt mass fraction express power expon mg exampl shown tabl tabl exampl reproduc cv quantit method rang analyt mass fraction gt tabl gt analys carri repeat condit intra laboratori cv typic half third valu analys carri laboratori reproduc condit laboratori cv greater reproduc cv case substanc establish permit limit method achiev laboratori reproduc greater reproduc cv concentr permit limit perform criteria requir mass spectrometr detect mass spectrometr method suitabl consider confirmatori method line line chromatograph separ chromatograph separ gc ms procedur ga chromatograph separ carri capillari column lc ms procedur chromatograph separ carri suitabl lc column case minimum accept retent time analyt examin retent time void volum column retent time rel retent time analyt test portion match calibr standard retent time window retent time window commensur resolv power chromatograph system ratio chromatograph retent time analyt intern standard rel retent time analyt correspond calibr solut toler gc lc mass spectrometr detect mass spectrometr detect carri emploi ms techniqu record full mass spectra full scan select ion monitor sim ms msn techniqu select reaction monitor srm suitabl ms ms msn techniqu combin ionis mode high resolut mass spectrometri hrm resolut typic greater entir mass rang vallei full scan mass spectrometr determin perform record full scan spectra presenc measur diagnost ion molecular ion characterist adduct molecular ion characterist fragment ion isotop ion rel intens refer spectrum calibr standard obligatori sim mass spectrometr determin perform fragmentographi molecular ion prefer select diagnost ion molecular ion characterist adduct molecular ion characterist fragment ion isotop ion select diagnost ion exclus origin part molecul signal nois ratio diagnost ion amp gt full scan sim rel intens detect ion express percentag intens intens ion transit correspond calibr standard calibr standard solut spike sampl compar concentr measur condit toler tabl maximum permit toler rel ion intens rang mass spectrometr techniqu gt tabl gt interpret mass spectral data rel intens diagnost ion precursor product ion pair identifi compar spectra integr signal singl mass trace background correct appli appli uniformli batch paragraph full scan full scan spectra record singl mass spectrometri minimum ion present rel intens amp gt base peak molecular ion includ present refer spectrum rel intens amp gt ion lie maximum permit toler rel ion intens tabl comput aid librari search case comparison mass spectral data test sampl calibr solut exce critic match factor factor determin valid process analyt basi spectra criteria fulfil variabl spectra caus sampl matrix detector perform check sim mass fragment measur full scan techniqu system identif point interpret data confirm substanc list group annex direct ec minimum identif point requir confirm substanc list group annex direct ec minimum identif point requir tabl show number identif point basic mass spectrometr techniqu earn order qualifi identif point requir confirm sum identif point calcul minimum ion ratio measur relev measur ion ratio meet criteria maximum separ techniqu combin achiev minimum number identif point tabl relationship rang class mass fragment identif point earn gt tabl gt footnot ion count gc ms electron impact ionis regard techniqu gc ms chemic ionis analyt increas number identif point deriv emploi reaction chemistri substanc group annex direct ec techniqu analyt procedur hplc coupl full scan diod arrai spectrophotometri dad hplc coupl fluoresc detect hplc coupl immunogram dimension tlc coupl spectrometr detect maximum identif point contribut provid relev criteria techniqu fulfil transit product includ daughter granddaught product tabl exampl number identif point earn rang techniqu combin thereof integ gt tabl gt perform criteria requir chromatographi coupl infrar detect adequ peak adequ peak absorpt maxima infrar spectrum calibr standard fulfil requir infra red detect absorpt maximum wavenumb rang cm intens absorpt specif molar absorb respect peak base line rel absorb absorb intens peak region cm measur respect absorb absorb intens peak region cm measur respect peak base line note adequ peak prefer theoret point view easier determin practic number peak infrar spectrum analyt frequenc correspond adequ peak spectrum calibr standard margin cm determin interpret infra red spectral data absorpt present region analyt spectrum correspond adequ peak refer spectrum calibr standard minimum adequ peak requir infrar spectrum calibr standard adequ peak spectrum issu refer spectrum quot score quot percentag adequ peak found infrar spectrum analyt exact match adequ peak relev region analyt spectrum consist presenc match peak procedur applic absorpt peak sampl spectrum intens time peak peak nois perform criteria requir determin analyt lc detect techniqu chromatograph separ intern standard materi suitabl purpos prefer relat standard retent time close analyt analyt elut retent time typic calibr standard experiment condit minimum accept retent time analyt time retent time void volum column ratio retent time analyt intern standard rel retent time analyt calibr standard matrix margin full scan uv vi detect perform criteria lc method fulfil absorpt maxima spectrum analyt wavelength calibr standard margin determin resolut detect system diod arrai detect typic nm spectrum analyt nm part spectra rel absorb amp gt visibl spectrum calibr standard criterion met firstli maxima present differ spectra point observ greater absorb calibr standard case comput aid librari search match comparison spectral data test sampl calibr solut exce critic match factor factor determin valid process analyt basi spectra criteria fulfil variabl spectra caus sampl matrix detector perform check perform criteria fluorimetr detect perform criteria lc method fulfil appli molecul exhibit nativ fluoresc molecul exhibit fluoresc transform derivatis select excit emiss wavelength combin chromatograph condit minimis occurr interf compon blank sampl extract nearest peak maximum chromatogram separ design analyt peak full peak width maximum height analyt peak perform criteria determin analyt lc immunogram lc immunogram suitabl confirmatori method relev criteria lc method fulfil pre defin qualiti control paramet specif bind rel bind control sampl absorb blank limit obtain valid assai immunogram construct fraction fraction half peak width fraction maximum content analyt suspect sampl compliant control sampl standard determin analyt lc uv vi detect singl wavelength lc uv vi detect singl wavelength suitabl confirmatori method nearest peak maximum chromatogram separ design analyt peak full peak width maximum height analyt peak perform criteria requir determin analyt tlc coupl full scan uv vi spectrometr detect dimension hptlc chromatographi mandatori rf valu analyt agre rf valu standard visual appear analyt indistinguish standard spot colour centr nearest spot separ centr spot analyt half sum spot diamet spectrum analyt visual spectrum standard full scan uv vi detect case comput aid librari search match comparison spectral data test sampl calibr solut exce critic match factor factor determin valid process analyt basi spectra criteria fulfil variabl spectra caus sampl matrix detector perform check perform criteria requir determin analyt gc combin electron captur detect ecd intern standard materi suitabl purpos prefer relat substanc retent time close analyt analyt elut retent time typic calibr standard experiment condit minimum accept retent time analyt time retent time void volum column ratio retent time analyt intern standard rel retent time analyt calibr standard matrix margin nearest peak maximum chromatogram separ design analyt peak full peak width maximum height analyt peak addit inform chromatographi confirmatori method element confirmatori analys chemic element base concept unequivoc identif accur precis quantif mean physic chemic properti uniqu chemic element hand element characterist wavelength emit absorb radiat atom mass level interest method combin method consid suitabl identif chemic element tabl suitabl confirmatori method chemic element gt tabl gt common perform criteria requir confirmatori method refer fortifi materi amount analyt maximum permit limit decis limit compliant control sampl compliant control materi reagent blank prefer carri entir procedur simultan batch test sampl analys recommend order inject extract analyt instrument reagent blank compliant control sampl sampl confirm compliant control sampl final compliant control sampl variat justifi gener analyt techniqu requir complet digest organ matrix obtain solut prior determin analyt achiev microwav mineralis procedur minimis risk loss contamin analyt interest decontamin teflon vessel good qualiti wet dry digest method resort document evid exclud potenti loss contamin phenomena altern digest separ procedur extract circumst chosen separ analyt matrix compon concentr analyt order introduc analyt equip calibr extern base standard addit method care exce work rang establish analysi case extern calibr mandatori calibr standard prepar solut match close composit sampl solut background correct appli requir specif analyt circumst addit perform criteria requir quantit method analysi trueness quantit method case repeat analys certifi refer materi element deviat experiment determin content certifi lie limit crm accept trueness measur assess recoveri addit amount element unknown sampl attent drawn fact unlik analyt ad element chemic bound real matrix result obtain approach lesser valid achiev crm recoveri data accept target precis quantit method case repeat analysi sampl carri laboratori reproduc condit intra laboratori coeffici variat cv exce valu tabl cv quantit method rang element mass fraction gt tabl gt specif requir differenti puls anod strip voltametri dpasv complet destruct organ matter sampl prior dpasv determin greatest import broad signal due presenc organ materi voltamogram inorgan matrix constitu influenc peak height dpasv quantif method standard addit specimen typic voltamogram sampl solut suppli method specif requir atom absorpt spectrometri aa techniqu basic mono element requir optimis experiment set depend element quantifi result check qualit quantit resort altern absorpt line ideal line select calibr standard prepar solut matrix match close sampl measur solut acid concentr modifi composit minimis blank valu reagent highest puriti depend mode chosen vaporis atomis sampl type aa distinguish specif requir flame aa instrument set optimis element ga composit flow rate check continuum sourc corrector avoid interfer caus background absorpt case unknown matric check made background correct requir specif requir graphit furnac aa contamin laboratori affect accuraci work ultra trace level graphit furnac high puriti reagent deionis water inert plastic ware sampl standard handl instrument set element optimis pre treatment atomis condit temperatur time matrix modif check work isotherm atomis condit transvers heat graphit tube integr lvov platform reduc influenc matrix atomis analyt combin matrix modif zeeman background correct quantif mean calibr curv base measur aqueou standard solut allow specif requir hydrid gener atom absorpt spectrometri organ compound element arsen bismuth germanium lead antimoni selenium tin tellurium stabl requir oxid decomposit obtain correct result total element content microwav digest high pressur ash strong oxid condit recommend greatest care devot complet reproduc convers element hydrid format arsen hydrid hydrochlor acid solut nabh depend oxid state arsen iii fast format longer format period avoid loss sensit determin flow inject techniqu caus short reaction time system reduc iii oxid decomposit potassium iodid ascorb acid cystein suitabl purpos blank calibr solut sampl solut treat work batch system determin arsen speci affect accuraci due delai format hydrid calibr perform peak area integr instrument set optimis ga flow transfer hydrid atomis import check specif requir cold vapour atom absorpt spectrometri cold vapour case mercuri due volatilis adsorpt loss element mercuri special care analysi contamin reagent environ avoid carefulli organ compound mercuri requir oxid decomposit obtain correct result total mercuri content decomposit seal system microwav digest high pressur asher special care requir clean equip contact mercuri work flow inject techniqu advantag lower decis limit adsorpt element mercuri gold platinum adsorb thermal desorpt recommend contact adsorb cell moistur disturb measur avoid specif requir induct coupl plasma atom emiss spectrometri icp ae induct coupl plasma atom emiss spectrometri multi element method simultan measur element icp ae sampl digest decompos organ matric seal system microwav digest high pressur ash meaning icp ae analysi instrument calibr element wavelength select plai essenti role instrument calibr case linear calibr curv measur calibr solut concentr icp ae calibr curv gener linear order magnitud concentr calibr icp ae system perform multi element standard prepar solut acid concentr measur solut linear curv element concentr check select wavelength measur emiss analyt concentr element determin analyt concentr fall work rang emiss line emiss line sensit emiss line interf chosen sensit line work detect limit sensit line respect analyt choic spectral background interfer caus major difficulti icp ae interfer simpl background shift slope background shift direct spectral overlap complex background shift interfer remedi depend matric interfer correct optimis oper paramet appli interfer avoid dilut adapt matric batch test sampl analys refer fortifi materi amount analyt blank materi treat test sampl test drift standard check sampl reagent plasma ga highest puriti specif requir induct coupl mass spectrometri icp ms determin trace element averag atom mass chromium copper nickel subject strong interfer isobar polyatom ion circumv resolut power difficulti ms techniqu includ instrument drift matrix effect molecular ion interfer amp lt multipl intern standardis cover mass rang element determin requir correct instrument drift matrix effect complet decomposit organ matter sampl prior icp ms measur requir aa digest seal vessel volatil element iodin transfer stabl oxid state sever interfer result molecular ion combin argon plasma ga hydrogen carbon nitrogen oxygen dissolut acid plasma ga impur entrain atmospher gase sampl matrix complet digest background measur choic analyt mass lower abund poorer detect limit dissolut acid nitric acid requir avoid interfer element determin interfer exclud choic specif analyt mass includ confirm isotop ratio instrument respons fano factor check measur intern standard valid valid demonstr analyt method compli criteria applic relev perform characterist control purpos requir categori method tabl determin perform characterist verifi type method tabl classif analyt method perform characterist determin gt tabl gt screen method confirmatori method determin mandatori valid procedur chapter exampl refer valid procedur analyt method approach demonstr analyt method compli perform criteria perform characterist provid achiev level qualiti inform valid perform conduct interlaboratori studi establish codex alimentariu iso iupac altern method singl laboratori studi hous valid part focus singl laboratori studi hous valid modular approach approach consist set common perform characterist independ valid model specif model depend procedur tabl tabl model independ model depend perform paramet gt tabl gt model independ perform characterist irrespect valid approach chosen perform characterist determin minimis workload carefulli design statist sound approach combin experi perform determin paramet specif analyt method power discrimin analyt close relat substanc isom metabolit degrad product endogen substanc matrix constitu import approach check interfer potenti interf substanc chosen relev blank sampl analys detect presenc interfer estim effect interfer select rang chemic relat compound metabolit deriv substanc encount compound interest present sampl analys number repres blank sampl amp gt check interfer signal peak ion trace region interest target analyt expect elut addition repres blank sampl fortifi relev concentr substanc interfer identif quantif analyt analysi investig presenc lead fals identif identif target analyt hinder presenc interfer quantif influenc notabl trueness paragraph determin trueness compon accuraci trueness establish mean certifi refer materi crm crm procedur detail iso analys replic crm accord test instruct method determin concentr analyt present sampl replic calcul standard deviat coeffici variat concentr calcul trueness divid detect concentr certifi measur concentr multipli express result percentag trueness recoveri correct concentr detect certifi crm trueness recoveri determin applic rugged minor studi deliber introduct minor reason variat laboratori observ consequ pre investig studi carri select factor sampl pre treatment clean analysi influenc measur result factor includ analyst sourc ag reagent solvent standard sampl extract rate heat temperatur ph factor occur laboratori factor modifi order magnitud match deviat encount laboratori identifi factor influenc result vari factor slightli conduct rugged test approach youden approv method point youden approach requir time effort minimum youden approach fraction factori design interact factor detect factor found influenc measur result significantli conduct experi decid accept limit factor factor significantli influenc result identifi method protocol basic idea studi alter time introduc variat denot nomin valu factor influenc result nomin valu chang slightli altern valu denot lower case letter result combin choos subset combin balanc capit small letter tabl determin made combin chosen factor result determin shown tabl tabl experi design rugged studi minor gt tabl gt calcul exampl rugged test stabil observ insuffici stabil analyt matrix constitu sampl storag analysi give rise signific deviat outcom result analysi stabil calibr standard solut check analyt stabil characteris storag condit monitor storag condit form part normal laboratori accredit system exampl stabil determin stabil analyt solut prepar fresh stock solut analyt dilut test instruct yield suffici aliquot select concentr minimum requir perform limit substanc permit limit establish permit limit substanc prepar solut analyt fortif final analysi solut solut interest derivatis standard measur analyt content freshli prepar solut test instruct dispens volum suitabl contain label store scheme tabl scheme determin analyt stabil solut gt tabl gt store time select week longer degrad phenomena observ identif quantif maximum store time optimum store condit record calcul concentr analyt aliquot carri solut analyt freshli prepar time analysi gt refer graphic gt ci concentr time point cfresh concentr fresh solut stabil analyt matrix incur sampl incur materi matrix fortifi analyt incur materi concentr materi determin materi fresh aliquot materi week concentr determin tissu store minu lower requir incur materi blank materi homogenis divid materi aliquot fortifi aliquot analyt prefer prepar small quantiti aqueou solut analys aliquot immedi store remain aliquot minu lower requir analys week calibr curv calibr curv quantif level includ construct curv work rang curv mathemat formula curv good fit data curv accept rang paramet curv serial calibr base standard solut accept rang paramet calibr curv vari seri seri convent valid procedur calcul paramet accord convent method requir perform individu experi perform characterist determin major chang applic rugged multi analyt method analyt analys simultan long possibl relev interfer rule previous perform characterist determin similar minimis workload advis combin experi repeat laboratori reproduc specif analysi blank sampl determin decis limit test specif recoveri crm recoveri determin experi fortifi blank matrix scheme select aliquot blank materi fortifi aliquot time minimum requir perform limit time permit limit analys sampl calcul concentr present sampl equat calcul recoveri sampl calcul recoveri cv result level recoveri measur content fortif level convent method determin recoveri variant standard addit method sampl consid blank sampl sampl analys consid yield recoveri similar test portion test sampl mass test portion extract volum amount calibr standard ad spike test portion note xadd xadd ρa va measur blank measur spike test portion recoveri xadd condit suppos achiev complet procedur determin recoveri standard addit method perform repeat prepar set sampl ident matric fortifi analyt yield concentr equival time minimum requir perform limit time permit limit level analysi perform replic analys sampl calcul concentr detect sampl find concentr standard deviat coeffici variat fortifi sampl repeat step occas calcul concentr cv fortifi sampl laboratori reproduc prepar set sampl test materi ident matric fortifi analyt yield concentr equival time minimum requir perform limit time permit limit level analysi perform replic repeat step occas oper environment condit batch reagent solvent room temperatur instrument analys sampl calcul concentr detect sampl find concentr standard deviat coeffici variat fortifi sampl reproduc reproduc verifi laboratori particip collabor studi iso decis limit ccα decis limit establish requir identif identif quantif defin quot perform criteria requir analyt method quot part case substanc permit limit establish ccα establish calibr curv procedur iso refer critic net state variabl case blank materi fortifi minimum requir perform level equidist step analys sampl identif plot signal ad concentr concentr intercept time standard deviat laboratori reproduc intercept equal decis limit applic quantit assai analys blank materi matrix calcul signal nois ratio time window analyt expect time signal nois ratio decis limit applic quantit qualit assai case substanc establish permit limit ccα establish calibr curv procedur iso refer critic net state variabl case blank materi fortifi permit limit equidist step analys sampl identif plot signal ad concentr concentr permit limit time standard deviat laboratori reproduc equal decis limit analys blank materi matrix fortifi analyt permit limit concentr permit limit time standard deviat equal decis limit articl point detect capabl ccβ detect capabl determin requir screen identif identif quantif defin part case substanc permit limit establish ccβ establish calibr curv procedur iso refer minimum detect net state variabl case repres blank materi fortifi minimum requir perform level equidist step analys sampl identif plot signal ad concentr concentr decis limit time standard deviat laboratori reproduc measur content decis limit equal detect capabl analys blank materi matrix fortifi analyt decis limit analys sampl identifi analyt decis limit time standard deviat laboratori reproduc measur content equal detect capabl quantit result detect capabl determin investig fortifi blank materi decis limit case concentr level amp lt fals compliant result remain equal detect capabl method investig concentr level carri order ensur reliabl basi determin case substanc permit limit establish ccâ establish calibr curv procedur iso refer minimum detect net state variabl case repres blank materi fortifi permit limit equidist step analys sampl identifi analyt calcul standard deviat measur content decis limit concentr decis limit time standard deviat laboratori reproduc equal detect capabl analys blank materi matrix fortifi analyt decis limit decis limit time standard deviat equal detect capabl section rugged major analyt method test experiment condit includ speci matric sampl condit introduc major import evalu instanc youden approach perform characterist determin major shown signific effect perform assai valid altern model altern valid procedur appli underli model strategi respect prerequisit assumpt formula laid valid protocol refer avail altern approach appli hous valid model perform characterist determin manner permit valid major valid procedur requir design experiment plan valid experiment plan experiment plan design depend number speci factor investig step entir valid procedur sampl popul analys laboratori futur order select import speci factor influenc measur result subsequ concentr rang chosen purpos adapt level interest analyt investig simultan analyt method valid variat lead factor identifi lead factor form basi factor level combin lead factor includ factor speci matrix lead factor vari level speci speci consid gener vari lead factor level increas number analys perform select factor vari level tabl exampl factor consid import valid procedur gt tabl gt tabl experiment plan gt tabl gt sampl factor level combin spike concentr level interest blank sampl analys level analys perform entir valid experi measur result comput recoveri repeat concentr level sir laboratori reproduc concentr level sir decis limit ccα detect capabl ccβ power curv error rate versu concentr rugged major rugged minor determin paragraph sampl relat calibr curv calibr curv predict interv calibr curv matrix induc deviat smat run induc deviat srun effect individu factor measur result perform characterist comprehens evalu perform level method influenc individu factor investig relev combin factor experi design decid select factor exclud calibr curv significantli deviat standard deviat factor power curv power curv inform detect capabl method chosen concentr rang refer error risk appli investig method power curv calcul detect capabl respect categori screen confirm type qualit quantit method error figur power curv gt pic file quot en tif quot gt figur show graphic establish detect capabl ccβ analyt method method remain risk take fals decis concentr μg kg concentr μg kg risk take fals compliant decis decreas reproduc determin method reproduc singl laboratori studi hous valid concept requir repeat particip profici studi accord iso guid laboratori allow choos method provid method routin condit standard deviat laboratori assess reproduc method graphic represent analyt limit figur substanc permit limit establish gt pic file quot en tif quot gt figur substanc establish permit limit gt pic file quot en tif quot gt calcul rugged test minor youden approach comparison averag gt tabl gt gt tabl gt standard deviat differ di sdi gt pic file quot en tif quot gt sdi significantli larger standard deviat method carri laboratori reproduc condit foregon conclus factor effect result singl factor show signific influenc method suffici robust chosen modif calcul exampl hous valid procedur exampl calcul hous valid protocol valid altern model exampl standard addit method test sampl content analyt divid test portion respect mass test portion spike volum va solut concentr ρa analyt extract test portion respect volum obtain extract purif step method recoveri analyt suppos rc extract assai measur method sensit give analyt respons assum rc analyt nativ sampl spike sampl content calcul gt refer graphic gt method determin recoveri rc addit assai part extract test portion volum spike amount ρb vb analyt assai analyt respons recoveri gt refer graphic gt calcul sensit gt refer graphic gt condit applic detail abbrevi aa atom absorpt spectrometri ae atom emiss spectrometri aoac associ offici analyt chemist intern bound fraction immunoassai ci chemic ionis crm certifi refer materi cv coeffici variat dimension dad diod arrai detect dpasv differenti puls anod strip voltametri ecd electron captur detect ei electron impact ionis gc ga chromatographi hplc high perform liquid chromatographi hptlc high perform thin layer chromatographi hrm high resolut mass spectrometri icp ae induct coupl plasma atom emiss spectrometri icp ms induct coupl plasma mass spectrometri ir infrar iso intern standard organis lc liquid chromatographi lr ms low resolut mass spectrometri mrpl minimum requir perform limit ms mass spectrometri mass charg ratio rf rel migrat solvent front tlc rsdl rel standard deviat laboratori sim select ion monitor tlc thin layer chromatographi uv ultra violet light vi visibl light refer iso gener requir compet calibr test laboratori iso statist method qualiti control vol vocabulari symbol iso guid profici test interlaboratori comparison part develop oper profici test scheme iso guid profici test interlaboratori comparison part select profici test scheme laboratori accredit bodi iso accuraci trueness precis measur method result part gener principl definit iso part basic method determin repeat reproduc standard measur method part basic method determin trueness standard measur method iso chemistri layout standard part method chemic analysi de ruig weseman quot approach confirm infrar spectrometri quot chemometr brumbaugh matrix modifi vov platform elimin matrix interfer analysi fish tissu lead graphit furnac atom absorpt spectrometri analyt chemistri applic zeeman graphit furnac atom absorpt spectrometri chemic laboratori toxicolog minoia caroli ed pergamon press oxford pp xxvi induct coupl plasma analyt atom spectrometri montas golighti ed vch publish york plasma sourc mass spectrometri develop applic holland tanner ed royal societi chemistri iupac protocol design conduct interpret method perform studi pure amp appli chem jülicher gowik uhlig assess detect method trace analysi mean statist base hous valid concept analyst gowik jülicher uhlig multi residu method steroid anti inflammatori drug plasma high perform liquid chromatographi photodiod arrai detect method descript comprehens hous valid chromatogr oac peer verifi method polici procedur aoac intern wilson blvd suit arlington virginia usa youden steiner quot statist manual aoac associ offici analyt chemist quot aoac washington dc ff iso capabl detect part term definit part methodolog linear calibr case part methodolog linear calibr case stephani amp van ginkel quot yield recoveri world differ quot proceed euro food chem vienna austria septemb feder european chemic societi event isbn page direct eec octob approxim law member state relat unit measur oj iso quantiti unit part gener principl yield fraction mass analyt contain sampl present final extract recoveri fraction mass analyt ad sampl present final extract rest document assum yield recoveri equal term quot recoveri quot