固相萃取-超高效液相色谱-三重四极杆/线性离子阱质谱法检测水中大环内酯类抗生素  

Determination of Macrolide Antibiotics in Water by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Quadrupole Linear Ion Trap Mass Spectrometry

作　　者：范素素[1] 蔡萌 方烨渟 王丽婕 石健[1] FAN Susu;CAI Meng;FANG Yeting;WANG Lijie;SHI Jian(Analysis and Testing Center of Nantong University,Nantong 226019;School of Chemistry and Chemical Engineering,Nantong University,Nantong 226019)

机构地区：[1]南通大学分析测试中心,江苏南通226019 [2]南通大学化学化工学院,江苏南通226019

出　　处：《分析科学学报》2024年第3期293-299,共7页Journal of Analytical Science

基　　金：南通市社会民生科技计划(MS12020048);江苏省水利科技项目(2020043);江苏省大型科学仪器开放共享自主研究课题(TC2021A021)。

摘　　要：采用固相萃取-超高效液相色谱-三重四极杆线性离子阱质谱技术(SPE-UPLC-QTRAP MS)建立了环境水样中阿奇霉素、林可霉素、克林霉素、红霉素及替米考星5种大环内酯类抗生素的检测方法。调节水样pH为10后经HLB固相萃取柱净化、富集,然后用Kinetex F5色谱柱进行分离,用0.1%甲酸水溶液和0.1%甲酸乙腈溶液进行洗脱,采用电喷雾正离子源(ESI+),多反应监测(MRM)-信息依赖采集(IDA)-增强子离子(EPI)扫描模式对样品进行检测,用多反应监测(MRM)进行定量,增强子离子(EPI)谱图库辅助定性。结果表明:5种大环内酯类抗生素线性关系良好,相关系数均大于0.9992;检出限为0.01~0.30μg·L^(-1),定量限为0.10~0.50μg·L^(-1);3种不同浓度的水样加标回收率为71.60%~111.05%,相对标准偏差均在10%以内,EPI谱库比对纯度值均大于90%。该方法将传统的MRM扫描模式结合EPI谱图库检索,实现了同时定性和定量分析,对未知物准确定性定量检测提供了重要参考。Five macrolide antibiotics detection methods,including azithromycin,lincomycin,clindamycin,erythromycin and tilmicosin,in water were established by using solid phase extraction-ultra performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry(SPE-UPLC-QTRAP MS).The macrolide antibiotics in water samples were enriched with HLB solid phase extraction column at pH=10,then separated by Kinetex F5 chromatographic column,and eluted in gradient with 0.1% formic acid aqueous solution and 0.1%formic acid acetonitrile,respectively.The water samples were detected by multiple reaction monitoring(MRM)-information-dependent acquisition(IDA)-enhancer ion(EPI)scan mode using electrospray positive ion source(ESI+),and the EPI library and MRM were employed for the rapid confirmation and quantitative determination.The results showed that good linearity for five macrolide antibiotics and the correlation coefficient was higher than 0.9992.The limits of detection were 0.01-0.30μg·L^(-1),and the limits of quantification were 0.10-0.50μg·L^(-1).The recoveries of spiked water samples with three different concentrations were 71.60%-111.05%,and the relative standard deviations(RSD)were within 10%.The purity of EPI spectrum library was greater than 90%.This method combined traditional MRM scanning mode with EPI spectrum library retrieval,and achieved simultaneous qualitative and quantitative analysis.It can provide an important reference for the laboratory on deterministic and quantitative detection of unknown substance.

关 键 词：大环内酯类抗生素 固相萃取 线性离子阱 液质联用 残留检测 

分 类 号：O657.63[理学—分析化学]