固相萃取-液相色谱串联质谱法测定鸡蛋中16种氨基甲酸酯类杀虫剂残留量

Simultaneous determination of 16 kinds of carbamate insecticides in egg by solid phase extraction coupled with liquid chromatography tandem mass spectrometry

中文关键词:  鸡蛋  氨基甲酸酯类杀虫剂  代谢物  固相萃取  液相色谱串联质谱法  残留

英文关键词:egg  carbamate insecticide  metabolite  solid phase extraction  liquid chromatography-tandem mass spectrometry  residues

中文摘要:

      目的 建立液相色谱-串联质谱法测定鸡蛋中16种氨基甲酸酯类杀虫剂和6种代谢产物残留的分析方法。方法 样品用乙腈分2次提取, 提取液采用液液分配净化后再用氨基小柱净化, 净化液吹干复溶后进行液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)分析, 分析时液相色谱用0.1%甲酸溶液和乙腈作为流动相进行梯度洗脱, 22种化合物均采用正离子模式进行监测, 外标法定量。结果 方法的检出限(limit of detection, LOD)和定量限(limit of quantitation, LOQ)分别在0.02~0.3 μg/kg和0.05~ 1.0 μg/kg范围之间。22种化合物在2.0~500 μg/L浓度范围内呈良好线性关系, 相关系数(r)均高于0.9990, 在1.0、5.0和50 μg/kg浓度水平下添加回收率在78.7%~92.6%之间, 批内相对标准偏差为1.3%~7.1%, 批间相对标准偏差为2.5%~7.1%。结论 该方法简单、准确, 适用于鸡蛋样品中氨基甲酸酯类杀虫剂的确证分析。

英文摘要:

      Objective To establish a method for simultaneous determination of 16 kinds of carbamate insecticides and 6 kinds of metabolites residues in egg samples by solid phase extraction (SPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The egg sample was extracted twice with acetonitrile, purified by liquid-liquid extraction (LLE) and SPE method with aminopropyl SPE cartridge. The purified solution was dried and redissolved in 25% acetonitrile solution and then determined by liquid chromatography- tandem mass spectrometry. The sample was separated by gradient elution with a mixture of 0.1% formic acid solution and acetonitrile as the mobile phase. All of 22 kinds of compounds were monitored in the positive ion mode and quantified with external standard calibration curves. Results The limits of detection and limits of quantitation were in the range of 0.020.3 μg/kg and 0.051.0 μg/kg, respectively. The good linearities were obtained for the 22 compounds at a concentration range of 2.0500 μg/L. The recoveries of the 22 compounds in egg samples were in the range of 78.7%92.6% at 1.0, 5.0 and 50 μg/kg with intra-assay relative standard deviations of 1.3%7.1% and inter-assay relative standard deviations of 2.5%7.1%. Conclusion This method is simple and accurate, and it is suitable for determination and confirmation of carbamate insecticides in egg samples.