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采用 LC/ESI/sSRM 法测定薰衣草精油中 256 种农药的多残留量:氮气蒸发法采样的优缺点。

Multiresidue determination of 256 pesticides in lavandin essential oil by LC/ESI/sSRM: advantages and drawbacks of a sampling method involving evaporation under nitrogen.

机构信息

Groupement Interrégional de Recherche sur les Produits Agropharmaceutiques, 8 rue Becquerel, Angers Technopole, 49070, Beaucouze, France.

出版信息

Anal Bioanal Chem. 2014 Feb;406(5):1541-50. doi: 10.1007/s00216-013-7553-2. Epub 2013 Dec 24.

DOI:10.1007/s00216-013-7553-2
PMID:24366405
Abstract

The determination of 256 multiclass pesticides in lavandin essential oil has been performed by liquid chromatography-electrospray ionization tandem mass spectrometry using the scheduled selected reaction monitoring mode available on a quadrupole-linear ion trap mass spectrometer. With the aim of improving the limits of quantification (LOQs) of the target molecules, a sampling step based on evaporation of the essential oil under a nitrogen flow assisted by controlled heating was tested. The LOQs determined in this case were compared with the values obtained with the classic dilution preparation method. With sampling by dilution, 247 pesticides were detected and quantified at low concentration, with 74 % of the pesticides having LOQs of 10 μg L(-1) or less. With the evaporation method, a global improvement of the LOQs was observed, with lower LOQs for 92 active substances and LOQs of 10 μg L(-1) or less for 82.8 % of the pesticides. Almost twice as many active substances had an LOQ of 1 μg L(-1) or less when the evaporation method was used. Some pesticides exhibited poor recovery or high variance caused by volatilization or degradation during the evaporation step. This behavior was evidenced by the case of thiophanate-methyl, which is degraded to carbendazim.

摘要

采用配有四极杆-线性离子阱质谱仪的预定选择反应监测模式的液相色谱-电喷雾串联质谱法测定了拉文德精油中的 256 种多类农药。为了提高目标分子的定量限 (LOQ),测试了一种基于氮气流辅助控制加热蒸发精油的采样步骤。在这种情况下确定的 LOQ 与使用经典稀释制备方法获得的值进行了比较。通过稀释采样,可以在低浓度下检测和定量 247 种农药,其中 74%的农药的 LOQ 为 10μg/L 或更低。使用蒸发法,LOQ 得到了全面改善,92 种活性物质的 LOQ 降低,82.8%的农药的 LOQ 为 10μg/L 或更低。当使用蒸发方法时,几乎有两倍数量的活性物质的 LOQ 为 1μg/L 或更低。在蒸发过程中,一些农药由于挥发或降解而表现出回收率差或方差大。这种行为在噻菌灵降解为多菌灵的情况下得到了证明。

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