同位素稀释-液相色谱-串联质谱法同时测定水产品中13种镇静剂残留

Simultaneous determination of 13 kinds of sedative residues in aquatic products by isotope dilution-liquid chromatography-tandem mass spectrometry

中文关键词:  同位素稀释  液相色谱-串联质谱法  水产品  镇静剂

英文关键词:isotope dilution  liquid chromatography-tandem mass spectrometry  aquatic products  sedative

中文摘要:

      目的 建立同位素稀释-液相色谱-串联质谱法同时测定水产品中13种镇静剂残留的方法。方法 样品采用乙腈-1%氨水溶液提取, 提取液经固相萃取柱(Oasis PRIME HLB柱)净化, 浓缩后用流动相定容。以1%甲酸水溶液和乙腈为流动相, 采用Agilent InfiniityLab Poroshell 120 SB-C18色谱柱(2.1 mm×100 mm, 2.7 μm)分离后, 在多反应监测(multiple reaction monitoring, MRM)模式下测定, 内标法定量。结果 13种镇静剂在0.2~50 μg/L浓度范围内线性关系良好(r>0.99), 检出限和定量限分别为0.1~0.2 μg/kg和0.3~0.5 μg/kg。在3个浓度加标水平下的平均回收率为84.0%~116.6%, 相对标准偏差为2.1%~9.9%。结论 该方法前处理简单、结果准确, 适用于水产品种13种镇静剂残留的快速检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 13 kinds of sedative residues in aquatic products by isotope dilution-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The samples were extracted with acetonitrile-1% ammonia solution. The extract was purified by solid phase extraction column (Oasis PRIME HLB column), and diluted with mobile phase after concentration, then separated by Agilent InfiniityLab Poroshell 120 SB-C18 column (2.1 mm×100 mm, 2.7 μm) using 1% formic acid and acetonitrile as mobile phase, determined in multiple reaction monitoring (MRM) mode and quantified by internal standard method. Results The 13 kinds of sedatives had a good linear relationship within the concentration range of 0.2? 50 μg/L (r>0.99). The limits of detection and limits of quantitation were 0.1?0.2 μg/kg and 0.3?0.5 μg/kg, respectively. Average recoveries for the analytes at 3 spiked levels ranged from 84.0% to 116.6% with relative standard deviations (RSDs) of 2.1%?9.9%. Conclusion The method has simple pretreatment and accurate results, and is suitable for the rapid detection of 13 sedative residues in aquatic products.