Method Validation for Qualitative and Quantitative Analysis of Pesticide Residues in Tomato
efficiencyȱofȱtheȱmethodȱforȱqualitativeȱandȱanalysisȱ Theȱ methodȱ developedȱ byȱ Anastassiadesȱ Mȱ et al .ȱ
ofȱ selectedȱ pesticidesȱ in/onȱ tomatoȱ forȱ nationalȱ (2003)ȱ forȱ fastȱ andȱ easyȱ extractionȱ proceduresȱ forȱ
monitoringȱstudies.
analysisȱ ofȱ multipleȱ pesticidesȱ inȱ foodsȱ hasȱ beenȱ
followedȱwordwideȱinȱvariousȱmatrices,ȱandȱduringȱ
Results and Discussion
theȱ presentȱ investigation,ȱ itȱ wasȱ knownȱ thatȱ theȱ
Theȱ standardȱ chromatogramȱ withȱ 64ȱ pesticidesȱ atȱ
methodȱisȱgoodȱforȱtomatoȱmatrixȱalsoȱasȱthereȱwereȱ
500ȱ ppbȱ onȱ GC-MS/MSȱ wasȱ presentedȱ inȱ Figureȱ 1ȱ
noȱ matrixȱ interferences.ȱ Sampleȱ preparationȱ isȱ anȱ
andȱtheȱdataȱonȱretentionȱtimeȱ(RT),ȱMRMȱpapmetersȱ
importantȱ stepȱ forȱ betterȱ extractionȱ andȱ cleanupȱ
wasȱpresentedȱinȱTableȱ1.ȱEightȱpointȱlinearityȱcurveȱ
forȱMSȱanalysisȱandȱinȱtheȱpresentȱinvestigationȱtheȱ
wasȱdrawnȱbyȱinjectingȱmixtureȱofȱvariousȱpesticidesȱ
methodȱdescribedȱbyȱLehoteyȱSJȱ(2011)ȱwasȱfollowedȱ
(Figureȱ 2,3,4,5)ȱ andȱ dataȱ onȱ regressionȱ valuesȱ
withȱsomeȱmodifications,ȱandȱbasedȱonȱtheȱresultsȱ
including%ȱ RSDȱ fromȱ linearityȱ forȱ eachȱ pesticideȱ
obtainedȱtheȱpresentȱstudy,ȱitȱcanȱbeȱrecommendedȱtoȱ
wasȱ givenȱ inȱ Tableȱ 2.ȱ Itȱ isȱ seenȱ thatȱ theȱ R 2 ȱ valueȱ
beȱusedȱinȱtheȱnationalȱresidueȱmonitoringȱprogramsȱ
(CoefficientȱofȱDetermination:ȱaȱmeasureȱofȱgoodnessȱ
asȱtheȱmethodȱisȱvalidatedȱasȱperȱtheȱinternationallyȱ
ofȱ fitȱ ofȱ linearȱ regression)ȱ rangedȱ fromȱ 0.990-0.999ȱ
followedȱ“Guidanceȱdocumentȱonȱanalyticalȱqualityȱ
andȱpercentageȱofȱRelativeȱStandardȱDeviationȱisȱinȱ
controlȱ andȱ validationȱ proceduresȱ forȱ pesticideȱ
betweenȱ0.55-8.11ȱexplainsȱthatȱtheȱinstrumentȱhasȱ
residuesȱ analysisȱ inȱ foodȱ andȱ feed”ȱ ofȱ Healthȱ andȱ
wideȱ linearityȱ forȱ quantitationȱ purposes.ȱ Limitȱ ofȱ
ConsumerȱProtectionȱDirectorateȱGeneral,ȱEuropeanȱ
detectionȱofȱorganoȱchlorineȱpesticidesȱisȱinȱtheȱrangeȱ
Commissionȱ(SANCO/12571/2013ȱ(2013).
ofȱ0.001ȱtoȱ0.005ȱmg/kg,ȱwithȱrecoveryȱofȱ79.91%ȱtoȱ
92.00%ȱatȱ0.05ȱmg/kg,ȱ81.24ȱtoȱ94.62%ȱatȱ0.25ȱmg/kgȱ
References
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0.001ȱtoȱ0.005ȱmg/kgȱandȱrecoveryȱisȱinȱtheȱrangeȱofȱ
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79.96ȱtoȱ90.66%ȱatȱ0.05ȱmg/kg,ȱ79.02ȱtoȱ91.88%ȱatȱ0.25ȱ
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acetonitrileȱextraction/partitioningȱandȱ“dispersiveȱsolid-
pesticidesȱisȱinȱtheȱrangeȱofȱ81.02ȱtoȱ91.02%ȱatȱ0.05ȱ
phaseȱ extraction”ȱ forȱ theȱ determinationȱ ofȱ pesticideȱ
mg/kg,ȱ80.86ȱtoȱ92.08%ȱatȱ0.25ȱmg/kgȱandȱ81.89ȱtoȱ
residuesȱ inȱ produce.ȱ Journal of AOAC International 86 (2):ȱ
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93.62%ȱatȱ0.5ȱmg/kgȱfortificationȱlevel.ȱTheȱrecoveryȱ
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ofȱotherȱpesticidesȱsuchȱatȱherbicidesȱandȱfungicidesȱ
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isȱ inȱ theȱ rangeȱ ofȱ 88.81ȱ toȱ 91.69%ȱ atȱ 0.05ȱ mg/kgȱ
Programmeȱ Implementation,ȱ Governmentȱ ofȱ India.ȱ ppȱ
81.42ȱtoȱ92.12%ȱatȱ0.25ȱmg/kgȱandȱ82.64ȱtoȱ93.14%ȱ
1-1143.
atȱ0.5ȱmg/kgȱfortificationȱlevels.ȱTheȱextractionȱandȱ Fillionȱ J,ȱ Sauveȱ Fȱ andȱ Selwynȱ Jȱ 2000.ȱ Multiresidueȱ methodȱ
cleanupȱmethodologyȱfollowedȱprovedȱtoȱbeȱrapidȱ
forȱtheȱdeterminationȱofȱresiduesȱofȱ251ȱpesticidesȱinȱfruitsȱ
andȱ highlyȱ effectiveȱ forȱ extractionȱ ofȱ 64ȱ pesticidesȱ
andȱvegetablesȱbyȱgasȱchromatography/massȱspectrometryȱ
andȱ liquidȱ chromatographyȱ withȱ fluorescenceȱ detection.ȱ
fromȱ tomatoȱ withȱ aȱ recoveryȱ ofȱ variousȱ pesticidesȱ
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inȱ theȱ rangeȱ ofȱ 80-120%ȱ andȱ theȱ methodȱ usedȱ forȱ
KalraȱRLȱ2003.ȱAssessmentȱofȱhumanȱexposureȱofȱpesticideȱ
estimationȱ ofȱ pesticidesȱ usingȱ MRMsȱ methodȱ inȱ
residuesȱ throughȱ food,ȱ andȱ waterȱ andȱ otherȱ sourcesȱ inȱ
GC-MS/MSȱ(TQD)ȱisȱhighlyȱusefulȱforȱidentificationȱ
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ofȱpesticidesȱatȱveryȱlowȱlevels,ȱasȱtheȱcoefficientȱofȱ
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DC,ȱITRCȱLucknowȱandȱICMR,ȱNewȱDelhi,ȱIndia,ȱpp.ȱE1-9.
determinationȱisȱveryȱhighȱinȱtheȱlinearȱrangeȱofȱ0.01ȱ
ppmȱtoȱ0.50ȱppm,ȱwhichȱisȱveryȱusefulȱforȱmonitoringȱ
Lehoteyȱ SJȱ 2011.ȱ QuEChERSȱ sampleȱ preparationȱ approachȱ
forȱ massȱ spectrometricȱ analysisȱ ofȱ pesticideȱ residuesȱ inȱ
studiesȱareȱtheȱMRLsȱ(MaximumȱResidueȱLimits)ȱforȱ
foods.ȱ Methods in Molecular Biology 747 :ȱ65-91.
theȱtargetedȱpesticidesȱareȱ>ȱ0.01ȱmg/kgȱinȱtomato.ȱ
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