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Multiresidue Analysis of Pesticides in Straw Roughage by Liquid Chromatography-Tandem Mass Spectrometry

机译:液相色谱-串联质谱法对秸秆粗饲料中的农药进行多残留分析

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摘要

A multiresidue analytical method using a modification of the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) sample preparation approach combined with liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis was established and validated for the rapid determination of 69 pesticides at different levels (1-100 ng/g) in wheat and rice straws. In the quantitative analysis, the recoveries ranged from 70 to 120%, and consistent RSDs <= 20% were achieved for most of the target analytes (53 pesticides in wheat straw and 58 in rice straw). Almost all of the analytes achieved good linearity with R-2 > 0.98, and the limit of validation levels (LVLs) for diverse pesticides ranged from 1 to 10 ng/g. Different extraction and cleanup conditions were evaluated in both types of straw, leading to different options. The use of 0.1% formic acid or not in extraction with acetonitrile yielded similar final outcomes, but led to the use of a different sorbent in dispersive solid-phase extraction. Both options are efficient and useful for the multiresidue analysis of targeted pesticides in wheat and rice straw samples.
机译:建立了一种改进的“快速,简便,便宜,有效,坚固和安全”(QuEChERS)样品制备方法与液相色谱串联质谱法(LC-MS / MS)分析相结合的多残留分析方法,并验证了该方法的有效性。快速测定小麦和稻草中69种不同含量(1-100 ng / g)的农药。在定量分析中,回收率从70%到120%不等,大多数目标分析物(小麦秸秆中53种农药和稻草秸秆中58种农药)的RSD均≤20%。几乎所有分析物都具有良好的线性关系,R-2> 0.98,各种农药的验证水平(LVL)的极限范围为1至10 ng / g。在两种类型的秸秆中评估了不同的提取和净化条件,从而导致了不同的选择。在乙腈萃取中使用或不使用0.1%甲酸会产生相似的最终结果,但导致在分散固相萃取中使用不同的吸附剂。这两种选择对于小麦和稻草样品中目标农药的多残留分析都是有效且有用的。

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