用三重四级杆气质联用仪测定水产品中多种麻醉剂  

Detection of anesthetic residues in aquatic products by gas chromatography-tandem mass spectrometry

作　　者：翟纹静 朱振华 王莉莉 徐振东 ZHAI Wen-jing;ZHU Zhen-hua;WANG Li-li;XU Zhen-dong(Suzhou Entry-Exit Inspection and Quarantine Bureau,Suzhou 215104,China;Suzhou Huabo Testing Technology Company Limited.,Suzhou 215104,China)

机构地区：[1]苏州检验检疫局综合技术中心,江苏苏州215104 [2]苏州华博日化品检测服务有限公司,江苏苏州215104

出　　处：《大连海洋大学学报》2018年第6期769-774,共6页Journal of Dalian Ocean University

基　　金：江苏出入境检验检疫局科技计划项目(2017KJ21)

摘　　要：为建立能同时快速高效的检测水产品中多种麻醉剂的检测方法,以水产品中丁香酚、甲基丁香酚、异丁香酚、乙酸丁香酚酯、甲基异丁香酚、乙酸异丁香酚酯和三卡因7种麻醉剂为检测对象,采用硅胶固相萃取柱,HP-5MS UI毛细管色谱柱,电子轰击离子源多反应监测模式(MRM)进行了相关检测,建立了能同时检测这7种麻醉剂的三重四级杆气质联用质谱仪(GC-MS/MS)分析方法。结果表明:0～100μg/L范围内7种麻醉剂的浓度和峰面积线性关系良好;确定了GC-MS/MS方法的检出限为2. 0μg/kg,定量限为5. 0μg/kg,3个水平的加标回收率为73. 93%～119. 97%,且批内和批间精密度均符合GB/T 27404-2008要求。研究表明,本研究中建立的GC-MS/MS检测方法线性相关性良好、检出限低,精密度和准确度均符合要求,能够满足对水产品中麻醉剂残留量的检测要求。A gas chromatography-tandem mass spectrometry(GC-MS/MS)method was developed for the determination of anesthetic residues in fishery products.Solid-phase extraction(SPE)was used to purify and concentrate the target analytes which were separated by a HP-5MS UI column and detected in multiple-reaction monitoring(MRM)mode via positive electrospray ionization(ESI+).The results showed that the calibration curves of anesthetic residues were of good linearity in the range of 0-100μg/L,with detection limit of 2.0μg/kg and the quantification limit of 5.0μg/kg in this method.The recovery was found to be 73.93%-119.97% at three spiked levels for anesthetic residues and the relative standard deviation(RSD)to be able to meet requirement of GB/T27404-2008.The developed method is characterized by the excellent purification effect,sensitivity and accuracy,and can be used for the determination of anesthetic residues in fishery products.

关 键 词：丁香酚类 三卡因(MS-222) 固相萃取 三重四级杆气质联用 多反应监测模式(MRM) 

分 类 号：TS207.3[轻工技术与工程—食品科学]