水溶剂快速萃取-超高效液相-串联质谱测定土壤中磺胺类抗生素  

Determination of Sulfonamide Antibiotics in Soil by Aqueous Solvent Rapid Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：罗火焰 皮施施 吉义平 宋洲 周宇齐 钟旭 杨杰 LUO Huo-yan;PI Shi-shi;JI Yi-ping;SONG Zhou;ZHOU Yu-qi;ZHONG Xu;YANG Jie(Hubei Huaxiang Geological Environment Testing Technology Co.,Ltd.,Hubei Wuhan 430000;China University of Geosciences(Wuhan),Hubei Wuhan 430074;Hubei Province Geological Experimental Testing Center,Hubei Wuhan 430034;Hubei Key Laboratory of Resources and Eco-environment Geology(Hubei Geological Bureau),Hubei Wuhan 430034,China)

机构地区：[1]湖北华祥地质环境检测科技有限公司,湖北武汉430000 [2]中国地质大学(武汉),湖北武汉430074 [3]湖北省地质实验测试中心,湖北武汉430034 [4]资源与生态环境地质湖北省重点实验室(湖北省地质局),湖北武汉430034

出　　处：《广州化工》2023年第8期100-104,共5页GuangZhou Chemical Industry

基　　金：湖北省地质局科研项目(KJ2020-30);水溶剂绿色提取超高效液相色谱串联质谱法测定土壤中典型极性有机污染物研究(KJ2022-36);湖北省地质局科研项目(KJ2021-18);湖北典型水生态环境监测关键技术研究与应用(KJ2023-39)。

摘　　要：建立了水溶剂萃取-超高效液相色谱-串联质谱测定土壤中10种磺胺类抗生素的方法。使用加速溶剂萃取仪高温高压条件下萃取,HLB小柱富集净化,经ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm×1.7μm)色谱柱分离,MRM模式监测,内标法定量。10种磺胺类在0.1~50μg/L的范围内具有良好的线性,相关系数均>0.997,方法检出限为0.03~0.06μg/kg,实际土壤样品的3个加标水平样品的平均回收率在63.1%~112%之间,测定结果的相对标准偏差为0.70%~14.7%(n=6)。该方法前处理简单,分离效果好,灵敏度高,准确、稳定,能够满足土壤中痕量磺胺类抗生素的测定。A method was developed for the determination of 10 sulfonamide antibiotics in soil by aqueous solvent extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).10 sulfonamides had good linearity in the range of 0.1~50μg/L with correlation coefficients>0.997.The limits of detection were 0.03~0.06μg/kg.The average recoveries of the actual soil samples at the three spiked levels ranged from 63.1%to 112%,and the relative standard deviations of the determination results were 0.70%~14.7%(n=6).The method is simple in pre-treatment,good in separation,sensitive,accurate and stable,and can meet the determination of trace amounts of sulfonamide antibiotics in soil.

关 键 词：磺胺类抗生素 水溶剂 加速溶剂萃取 土壤 

分 类 号：TQ914.1[化学工程]