液相色谱串联质谱法优化水产养殖底泥中磺胺类抗生素的提取  

Optimization on the Extraction of Sulfonamide Antibiotics from Aquiculture Sediment by Liquid Chromatography Tandem Mass Spectrometry

作　　者：陈玉婷 李桂滢 宋成 伍仕权 龙思雨 朱良茂 杨孝容[1] Chen Yuting;Li Guiying;Song Cheng;Wu Shiquan;Long Siyu;Zhu Liangmao;Yang Xiaorong(College of New Energy Materials and Chemistry,Leshan Normal University,Sichuan,614000)

机构地区：[1]乐山师范学院新能源材料与化学学院,四川614000

出　　处：《当代化工研究》2023年第15期35-37,共3页Modern Chemical Research

基　　金：2022年国家级大学生创新创业训练计划项目“液相色谱串联质谱研究水产养殖底泥抗生素的提取方法”(项目编号:202210649060);2021年国家级大学生创新创业训练计划项目“水产养殖尾水排放对水体抗生素污染水平的影响”(项目编号:202110649032)。

摘　　要：通过样品加标回收率优化磺胺类提取条件,建立水产养殖底泥中磺胺类抗生素的提取方法。以冷冻干燥的底泥,用不同缓冲溶液和甲醇、不同体积比、提取液过HLB小柱pH等优化提取条件,以实验方法制备分析液,用甲醇和0.2%甲酸水溶液作流动相梯度洗涤色谱分离,电喷雾正离子和多反应监测模式质谱分析。结果表明,用0.1mol/L的柠檬酸溶液与甲醇(含0.1g Na_(2)EDTA)6:4提取,pH3过HLB小柱,17种磺胺的3个加标水平的回收率在61%~97%,相对平均偏差为1.1%~8.9%(n=4)。该方法简单、回收率高,可为水产养殖底泥磺胺类抗生素的测定提供参考。A method for extracting sulfa antibiotics from aquaculture sediment was established by optimizing the extraction conditions of sulfa antibiotics through sample spiking recovery.The bottom mud was freeze-dried.The extraction conditions were optimized using different buffer solutions and methanol,different volume ratios,and the pH of the extraction solution through the HLB column.The analytical solution was prepared according to the experimental method.The chromatographic separation was completed to separate of target sulfonamides with 0.2%formic acid solution and acetonitrile as mobile phase gradient washing.Electrospray ionization positive ion and multiple reaction monitoring mode were used for mass spectrometry analysis.The results showed that the volume ratio of 0.1 mol/L citric acid solution to methanol was 6:4(containing 0.1 g Na_(2)EDTA),and the pH was 3 through the HLB column.The spiked recoveries of 17 target sulfonamides at three spiked concentration levels were 61%to 97%,with a relative average deviation of 1.1%to 8.9%(n=4).The method is simple and has a high recovery rate,which can provide a reference for the determination of sulfa antibiotics in aquiculture sediment.

关 键 词：液相色谱-串联质谱 底泥 磺胺类抗生素 

分 类 号：TQ[化学工程]