通过式固相萃取净化/高效液相色谱-串联质谱法快速测定水产品中6种麻醉剂残留  

Rapid Determination of Six Anesthetics Residues in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction

作　　者：高平 杨曦 莫彩娜 陈日檬 曾丹丹 刘唤明 洪鹏志 周凯 陈营寿 GAO Ping;YANG Xi;MO Cai-na;CHEN Ri-meng;ZENG Dan-dan;LIU Huan-ming;HONG Peng-zhi;ZHOU Kai;CHEN Ying-shou(Zhanjiang Institute for Food and Drug Control,Zhanjiang 524022,China;Key Laboratory of Aquatic,Livestock and Poultry Feed Science and Technology in South China,Ministry of Agriculture and Rural Affairs,Guangdong Evergreen Feed Industry Co.,Ltd.,Zhanjiang 524094,China;Aquatic Product Processing and Safety Key Lab of Guangdong Province,College of Food Science and Technology,Guangdong Ocean University,Zhanjiang 524088,China)

机构地区：[1]湛江市食品药品检验所,广东湛江524022 [2]广东恒兴饲料实业股份有限公司农业农村部华南水产与畜禽饲料重点实验室,广东湛江524094 [3]广东海洋大学食品科技学院广东省水产品加工与安全重点实验室,广东湛江524088

出　　处：《分析测试学报》2019年第9期1059-1065,共7页Journal of Instrumental Analysis

基　　金：广东省食品药品监督管理局食品药品检验检测技术创新专项(2015ZX04);湛江市海洋经济创新发展示范市建设项目(湛海创2017C8B1);广东省促进经济发展专项资金海洋经济发展用途项目(GDME-2018C009);湛江市科技计划项目(2017A02001,2018A02001)

摘　　要：建立了一种快速测定水产品中6种麻醉剂(普鲁卡因、利多卡因、布比卡因、丁卡因、3-氨基苯甲酸乙酯甲基磺酸盐、苯佐卡因)的高效液相色谱-串联质谱分析方法。样品以水和1%甲酸乙腈提取,提取液经PRiME HLB固相萃取柱净化,以乙腈和0.1%甲酸水溶液为流动相梯度洗脱,ZORBAX Eclipse XDB-C 18色谱柱(3.0 mm×150 mm,3.5μm)分离,多反应监测(MRM)正离子模式检测,外标法定量。结果表明,6种组分在各自质量浓度范围内线性关系良好,相关系数(r^2)为0.993 8~0.998 7,方法检出限(LOD)为1.5~6.0μg/kg,定量下限(LOQ)为5.0~20μg/kg,平均加标回收率为76.8%~110%,相对标准偏差为4.2%~11%。该方法前处理操作简单、快速、准确、灵敏,适用于水产品中6种麻醉剂残留的快速测定。A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method was developed for the rapid determination of six anesthetics,e.g.procaine,lidocaine,bupivacaine,tetracaine,tricaine methanesulfonate(MS-222)and benzocaine in aquatic products.The samples were extracted with water and acetonitrile containing 1.0%formic acid,and then cleaned up with a PRiME HLB pass-through solid phase extraction column.The targets were separated on a ZORBAX Eclipse XDB-C 18 column(3.0 mm×150 mm,3.5μm)with acetonitrile-0.1%formic acid as mobile phase by gradient elution.The analytes were determined in electrospray positive ionization(ESI+)mode under multiple reaction monitoring(MRM).Results showed that there were good linear relationships for the targets in their respective concentration ranges with correlation coefficients(r^2)of 0.993 8-0.998 7.The limits of detection(LOD)and limits of quantitation(LOQ)were in the ranges of 1.5-6.0μg/kg and 5.0-20μg/kg,respectively.Average spiked recoveries for six anesthetics were in the range of 76.8%-110%with relative standard deviations of 4.2%-11%.The proposed method is simple,quick,accurate and sensitive,and is suitable for the determination of six anesthetics in aquatic products.

关 键 词：麻醉剂 通过式固相萃取 水产品 高效液相色谱-串联质谱(HPLC-MS/MS) 

分 类 号：O657.63[理学—分析化学] TS201.6[理学—化学]