分散固相萃取-超高效液相色谱-串联质谱法测定海龙中11种磺胺类抗菌药物残留  

Determination of 11 Sulfonamide Antibacterial Drug Residues in Syngnathus by Ultra-Performance Liquid Chromatography-Mass Spectrometry Combined with Dispersed Solid Phase Extraction

作　　者：王小乔 李坚 许晓辉 李剑勇[2] 吴福祥 张虹艳 潘秀丽 李赟 WANG Xiaoqiao;LI Jian;XU Xiaohui;LI Jianyong;WU Fuxiang;ZHANG Hongyan;PAN Xiui;LI Yun(Lanzhou Institute for Food and Drug Control/Key Laboratory of Pesticides and Veterinary Drugs Monitoring for State Market Regulation,Lanzhou 730050,China;Lanzhou Institute of Husbandry and Pharmaceutical Sciences of CAAS,Lanzhou 730050,China)

机构地区：[1]兰州市食品药品检验检测研究院/食品中农药兽药残留监控国家市场监管重点实验室,甘肃兰州730050 [2]中国农业科学院兰州畜牧与兽药研究所,甘肃兰州730050

出　　处：《分析测试技术与仪器》2023年第1期16-22,共7页Analysis and Testing Technology and Instruments

基　　金：甘肃省市场监督管理局科技计划资助项目(SSCJG-SP-A202204)。

摘　　要：采用超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)技术,建立了测定海龙中11种磺胺类抗菌药物残留量的分析方法.样品经2%甲酸-乙腈超声提取,增强型脂质去除分散固相萃取净化管(EMR-Lipid dSPE)净化,采用Waters ACQUITY BEH C 18色谱柱(1.7µm,2.1 mm×100 mm)分离,电喷雾离子源电离,正离子多反应监测模式(MRM)检测,以含2 mmol/L乙酸铵-0.1%甲酸的水溶液和含0.1%甲酸的乙腈溶液为流动相进行梯度洗脱,外标法定量.11种磺胺类抗菌药物在0~30 ng/mL的质量浓度范围内线性关系良好,相关系数(R2)均不低于0.9959,检出限(LOD)与定量限(LOQ)分别在0.11~1.30µg/kg和0.37~4.40µg/kg之间,11种磺胺类抗菌药物在质量浓度为20.0、50.0、100.0µg/kg时的三个加标水平的平均回收率为62.5%~118.1%,相对标准偏差为2.1%~9.2%.方法前处理简便、准确性好,可用于海龙中11种磺胺类抗菌药物残留的快速筛查.An analytical method for the determination of 11 sulfonamide antibacterial drug residues in Syngnathus by ultra-performance liquid chromatography-mass spectrometry(UPLC-MS/MS)has been established.The samples were extracted by ultrasonication with 2%formic acid-acetonitrile,purified by an enhanced matrix removal lipid-dispersed solid phase extraction(EMR-Lipid dSPE),and separated on a Waters ACQUITY BEH C 18 column(1.7µm,2.1 mm×100 mm).The analytes were detected by mass spectrometry using the positive electrospray ionization mode under multiple reaction monitoring mode(MRM),with 2 mmol/L ammonium acetate-0.1%formic acid in aqueous solution and 0.1%formic acid in acetonitrile as mobile phases by a gradient elution program,and quantified by the external standard method.The results showed that the 11 antibacterial sulfonamides had good linearity in the range of 0~30 ng/mL,the correlation coefficient(R2)were all greater than 0.9959,the limit of detection(LOD)and quantitation(LOQ)were in the range of 0.11~1.30μg/kg and 0.37~4.40μg/kg,respectively.At three spiked levels of 20.0,50.0 and 100.0μg/kg,the spiked average recoveries of the analytes were in the range of 62.5%~118.1%,and the relative standard deviation was 2.1%~9.2%.The method is accurate,straightforward,and is suitable for the rapid screening of 11 sulfonamide antibacterial drug residues in Syngnathus.

关 键 词：海龙 超高效液相色谱-三重四极杆质谱联用法 磺胺类药物 分散固相萃取 残留量 

分 类 号：O657.63[理学—分析化学]