2013•Journal of Instrumental AnalysisRequires access

Determination of 27 Pesticide Residues in Raisins Using Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

Zhiguo Gong

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Abstract

An ultra-high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of 27 pesticide residues in raisins,include carbamate insecticides,triazole fungicides and other fungicides,pesticides.The samples were directly extracted with 0.1% glacial acetic acid-acetonitrile,and purified by QuEChERS method.The analysis of 27 pesticides was carried out under positive electrospray ionization(ESI+) mode and multiple reaction monitoring(MRM) mode,quantified by matrix matching curve external standard method.The results showed that the calibration curves of 27 pesticides were linear(r≥0.993) in the concentration range of 5-100 μg/kg.The average recoveries at three spiked levels of 10,20 and 50 μg/kg were in the ranges of 60%-97%,62%-97% and 64%-99%,respectively,with relative standard deviations(RSDs) of 3.0%-13.0%,1.6%-9.6% and 3.3%-9.6%,respectively.The quantitation limit(S/N≥10) was 10 μg/kg.The method is simple,rapid,sensitive and accurate,and was suitable for the confirmation and quantitative determination of multiple pesticide residues in raisins.

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What this paper is about

An ultra-high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of 27 pesticide residues in raisins,include carbamate insecticides,triazole fungicides and other fungicides,pesticides.The samples were directly extracted with 0.1% glacial acetic acid-acetonitrile,and purified by QuEChERS method.The analysis of 27 pesticides was carried out under positive electrospray ionization(ESI+) mode and multiple reaction monitoring(MRM) mode,quantified by matrix matching curve external standard method.The results showed that the calibration curves of 27 pesticides were linear(r≥0.993) in the concentration range of 5-100 μg/kg.The average recoveries at three spiked levels of 10,20 and 50 μg/kg were in the ranges of 60%-97%,62%-97% and 64%-99%,respectively,with relative standard deviations(RSDs) of 3.0%-13.0%,1.6%-9.6% and 3.3%-9.6%,respectively.The quantitation limit(S/N≥10) was 10 μg/kg.The method is simple,rapid,sensitive and accurate,and was suitable for the confirmation and quantitative determination of multiple pesticide residues in raisins.

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Available abstract

An ultra-high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of 27 pesticide residues in raisins,include carbamate insecticides,triazole fungicides and other fungicides,pesticides.The samples were directly extracted with 0.1% glacial acetic acid-acetonitrile,and purified by QuEChERS method.The analysis of 27 pesticides was carried out under positive electrospray ionization(ESI+) mode and multiple reaction monitoring(MRM) mode,quantified by matrix matching curve external standard method.The results showed that the calibration curves of 27 pesticides were linear(r≥0.993) in the concentration range of 5-100 μg/kg.The average recoveries at three spiked levels of 10,20 and 50 μg/kg were in the ranges of 60%-97%,62%-97% and 64%-99%,respectively,with relative standard deviations(RSDs) of 3.0%-13.0%,1.6%-9.6% and 3.3%-9.6%,respectively.The quantitation limit(S/N≥10) was 10 μg/kg.The method is simple,rapid,sensitive and accurate,and was suitable for the confirmation and quantitative determination of multiple pesticide residues in raisins.

Key concepts: Chemistry, Quechers, Chromatography, Detection limit, Pesticide residue, Pesticide, Selected reaction monitoring, Tandem mass spectrometry

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