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A fast and easy GC-MS/MS method for simultaneous analysis of 73 pesticide residues in vegetables and fruits

机译:快速简便的GC-MS / MS方法可同时分析蔬菜和水果中的73种农药残留

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A simple and easy method was established for the simultaneous determination of 73 pesticide residues in vegetables and fruits by gas chromatography-tandem mass spectrometry (GC-MS/MS). After samples were ultrasonically extracted with hexane and centrifuged, the analytes in sample solution were separated with DB-5MS column (30 m ?— 0.25 mm, 0.25 ??m). Qualitative determination of the analytes was based on characteristic ion pairs and retention time using multiple reactions monitoring (MRM) mode. The mixed-matrices standard curves were used for quantification. The calibration curves were mostly in the range of 10a€“1000 ??g La?’1. The limits of detection (LODs) of the method were from 0.012 to 18.8 ??g kga?’1 and limits of quantification (LOQs) were in the range of 0.042a€“61.8 ??g kga?’1, which were much lower than the maximum residue levels (MRLs) established by European legislation. The average recoveries of the method ranged from 86.7% to 124%, 85.6% to 117%, 89.2% to 111% at three spiked levels of 0.10, 0.20, 0.50 mg kga?’1 in leek samples, with relative standard deviations (RSDs) of 1.84% to 11.3%, 2.40% to 9.50%, 0.79% to 8.30%, respectively. Additionally, the method was more favorable than gas chromatography-mass spectrometry (GC-MS) in the analysis of 15 spiked samples, including ten vegetables and five fruits. Three pesticides were detected in the samples of celery and apple by the established method and the GC-MS method.
机译:建立了一种简便易行的气相色谱-串联质谱法(GC-MS / MS)同时测定蔬菜和水果中73种农药残留的方法。样品用己烷超声提取并离心后,样品溶液中的分析物用DB-5MS色谱柱(30 m?-0.25 mm,0.25?m)分离。使用多反应监测(MRM)模式基于特征离子对和保留时间对分析物进行定性测定。混合矩阵标准曲线用于定量。校准曲线大多在10a€1000 g La?1的范围内。该方法的检出限(LOD)为0.012至18.8 ?? g kga?'1,定量限(LOQ)在0.042a?61.8?g kga?'1的范围内。低于欧洲法规规定的最大残留量(MRL)。在韭菜样品中三个加标水平分别为0.10、0.20、0.50 mg kga?1的情况下,该方法的平均回收率范围为86.7%至124%,85.6%至117%,89.2%至111%,并具有相对标准偏差(RSD) )分别为1.84%至11.3%,2.40%至9.50%,0.79%至8.30%。此外,该方法在分析15个加标样品(包括10种蔬菜和5种水果)中比气相色谱-质谱(GC-MS)更有利。通过建立的方法和GC-MS方法在芹菜和苹果样品中检测到三种农药。

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