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首页> 外文期刊>Journal of Agricultural and Food Chemistry >Single-Laboratory Ruggedness Testing and Validation of a Modified QuEChERS Approach To Quantify 185 Pesticide Residues in Salmon by Liquid Chromatography - and Gas Chromatography - Tandem Mass Spectrometry
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Single-Laboratory Ruggedness Testing and Validation of a Modified QuEChERS Approach To Quantify 185 Pesticide Residues in Salmon by Liquid Chromatography - and Gas Chromatography - Tandem Mass Spectrometry

机译：单实验室耐用性测试和改良QuEChERS方法的验证，通过液相色谱-气相色谱-串联质谱法定量鲑鱼中的185种农药残留

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摘要

In this study, we successfully applied a previously modified version of the QuEChERS approach to quantify pesticide residues in samples of fresh salmon. Analysis was performed using a combination of liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The validated QuEChERS method used ethyl acetate for the extraction solvent and involved two freezing steps and a C18 dispersive solid phase extraction for removal of lipids. Of the 228 pesticides initially screened, only 185 passed the method validation criteria (103 on LC-MS/MS and 82 on GC-MS/MS). In a quantitative validation, acceptable performances were achieved with overall recoveries of 70-120% and <20% RSD for 179 analytes (n = 7) over the course of five different extractions at 2 times the limit of quantification. Over 12 months, this method was used in the analysis of 708 salmon samples collected as part of the U.S. Department of Agriculture's Pesticide Data Program. Ruggedness testing conducted throughout the entire study showed this method to be robust and suitable for long-term use.
机译：在这项研究中，我们成功地使用了QuEChERS方法的先前修改版本来量化新鲜鲑鱼样品中的农药残留。使用液相色谱和气相色谱串联质谱分析法（LC-MS / MS和GC-MS / MS）进行分析。经过验证的QuEChERS方法使用乙酸乙酯作为萃取溶剂，包括两个冷冻步骤和一个C18分散固相萃取以去除脂质。最初筛选的228种农药中，只有185种通过了方法验证标准（LC-MS / MS为103种，GC-MS / MS为82种）。在定量验证中，在五次不同萃取过程中，以两倍于定量极限的浓度，对179种分析物（n = 7）的总体回收率达到70-120％，相对标准偏差（RSD）小于20％，获得了可接受的性能。在12个月的时间里，该方法用于分析708种鲑鱼样品，这是美国农业部农药数据计划的一部分。在整个研究过程中进行的耐用性测试表明，该方法坚固耐用，适合长期使用。

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