冷冻去脂/分散固相萃取-气相色谱-串联质谱法快速测定水产品中43种农药残留

Rapid determination of 43 kinds of pesticide residues in aquatic products by gas chromatography-tandem mass spectrometry with freezing lipid filtration and dispersed solid phase extraction

中文关键词:  冷冻去脂  分散固相萃取  内标法  气相色谱-串联质谱法  水产品  农药残留

英文关键词:freezing lipid filtration  dispersed solid phase extraction  internal standard method  gas chromatography-tandem mass spectrometry  aquatic products  pesticide residues

中文摘要:

      目的 建立冷冻去脂/分散固相萃取-气相色谱-串联质谱法测定水产品中43种农药残留的方法。方法 样品经乙腈超声提取, 冷冻去脂后经N-丙基乙二胺(N-propyl ethylenediamine, PSA)和十八烷基硅烷键合硅胶(octadecyl silane bonded silica gel, C18)净化, 在多反应监测(multiple reaction monitoring, MRM)模式下, 以目标化合物的保留时间和碎片离子丰度比定性, 采用内标法定量测定。结果 43种农药在0.005~0.500 mg/kg范围内线性关系良好, 相关系数均大于0.995, 检出限为0.002 mg/kg, 定量限为0.005 mg/kg, 3个浓度加标回收率在64.3%~119.0%之间, 相对标准偏差(relative standard deviations, RSDs, n=6)在2.6%~11.3%之间。结论 该方法具有操作简单、快速、灵敏、准确的特点, 适用于水产品中43种农药残留的快速测定。

英文摘要:

      Objective To establish a method for the determination of 43 kinds of pesticide residues in aquatic products by freezing lipid filtration/dispersed solid phase extraction-gas chromatography-tandem mass spectrometry. Methods The samples were ultrasonically extracted with acetonitrile, frozen and degreased, purified by N-propyl ethylethylenediamine (PSA) and octadecyl silane bonded silica gel (C18), in the multiple reaction monitoring (MRM) mode, the retention time of the target compound and the fragment ion abundance ratio were used for qualitative analysis and the internal standard method was used for quantitative determination. Results The linear relationships were good within the range of 0.005?0.500 mg/kg, with correlation coefficients greater than 0.995, the detection limit and quantitation limit were 0.002 mg/kg and 0.005 mg/kg, respectively, the recoveries at the 3 spiked concentrations were within the range of 64.3%?119.0%, and the relative standard deviations (RSDs, n=6) was within the range of 2.6%?11.3%. Conclusion This method is simple, rapid, sensitive and accurate, and is suitable for the rapid determination of 43 kinds of pesticide residues in aquatic products.