三重四级杆气质联用法测定水产品中9种麻醉剂的残留量

Determination of residual levels of nine anesthetics inaquatic products by GC-MS/MS

本文采用快速滤过净化柱,利用三重四级杆气质联用仪(GC-MS/MS),选取鱼、虾、贝3类水产品基质,构建能快速检测MS-222、苯佐卡因、利多卡因、丁香酚、甲基丁香酚、异丁香酚、乙酸丁香酚酯、甲基异丁香酚、乙酰基异丁香酚酯9种麻醉剂的检测方法。选用乙腈溶剂提取,DB-5MS毛细管色谱柱分离,电子轰击离子源动态多反应监测(d MRM)模式,外标法定量,对3种典型水产品(鱼、虾、贝)进行方法验证。研究显示,9种麻醉剂在0.01~1μg/mL范围内呈良好线性关系,并且相关系数均大于0.998 9。该方法检出限为0.005 mg/kg,方法定量限为0.015 mg/kg。3种基质中9种麻醉剂在0.01、0.05、0.50 mg/kg添加水平下的平均加标回收率为85.4%~109.4%,平均相对标准偏差为1.2%~9.2%。运用优化后的方法对鱼、虾、贝3类水产品总计80个样品中9种麻醉剂残留量进行定性定量实验。结果表明:化合物中丁香酚检出率高,且在虾类样品中检出率高。该方法前处理操作简单、净化除杂彻底,仪器响应值高,分离效果显著,适用于水产品中多种麻醉剂的痕量检测和定性定量分析。

Matrices from three types of aquatic products(fish,shrimp,and shellfish)are selected for the study.Multi-plug filtration clean-up and triple quadrupole gas chromatography-mass spectrometry(GC-MS/MS)are used to construct a rapid detection method for 9 anesthetics,including 3-aminobenzoic acid ethyl ester methanesulfonate,benzocaine,lidocaine,eugenol,methyl eugenol,isoeugenol,eugenol acetate,methyl isoeugenol and acetyl isoeugenol acetate.The method is validated on three typical aquatic samples(fish,shrimp and shellfish)by using acetonitrile solvent extraction,separation on a DB-5MS capillary column,dynamic multiple reaction monitoring(dMRM)mode with electron bombardment ionization,and quantification by external standard method.The study demonstrates that the linearity of the nine anesthetics is good in the range of 0.01~1μg/mL,and the correlation coefficients are all greater than 0.9989.The limit of detection of the method is 0.005 mg/kg,the limit of quantification of the method is 0.015 mg/kg.The average spiked recoveries of the nine anesthetics are obtained from 85.4%to 109.4%with the average relative standard deviations of 1.2%to 9.2%by adding the standard solutions at the levels of 0.01,0.05 and 0.5 mg/kg to the blank matrix.The method is used for the determination of nine anesthetics in 80 samples of three types of aquatic products.The results show that the detection rate of eugenol is high among the compounds,and the detection rate is high in shrimp samples.The method has the advantages of simple operation,thorough purification,high instrumental response value and remarkable separation effect.It is suitable for the trace detection and qualitative and quantitative analysis of various anesthetics in aquatic products.