超高效液相色谱-串联质谱法检测东寨港海水中磺胺类药物残留  

Analysis of Sulfonamides Residues in Seawater of Dongzhai Harbor, Hainan Based on Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：张腾云 徐文 张鸣姗 赵洪伟 ZHANG Tengyun;XU Wen;ZHANG Mingshan;ZHAO Hongwei(Institute of Tropical Agriculture and Forestry,Hainan University,Haikou,Hainan 570228,China;Hainan Academy of Environmental Science&Hainan Environmental Monitoring Center,Haikou,Hainan 570100,China;State Key Laboratory of Utilization of Marine Resources in South China Sea,Hainan University,Haikou,Hainan 570228,China)

机构地区：[1]海南大学热带农林学院,海口570228 [2]海南省环境科学研究院和海南省环境监测中心,海口570228 [3]海南大学南海海洋资源利用国家重点实验室,海口570228

出　　处：《热带生物学报》2019年第2期197-203,共7页Journal of Tropical Biology

基　　金：海南省自然科学基金(417053、317302);海南省重大科技项目(ZDKJ2017002)

摘　　要：优化并建立了一种同时检测海水中13种磺胺类药物的超高效液相色谱-串联质谱(UPLC-MS/MS)的方法,并使用优化的方法对海南省东寨港表层海水进行了检测分析。结果表明:采用流动相A:V甲醇∶V乙腈=1∶1与B:V 0.1%甲酸∶V 10 mmol·L^-1乙酸铵=10∶90水溶液作为流动相且以5%的A和95%的B为初始流动相用来定容时色谱图中的磺胺类药物的峰型都较好,无杂峰影响且标准曲线的相关系数都较高(R 2≥0.996),待测的13种磺胺类药物在14 min内出峰,回收率在70.4%~103%范围,相对标准偏差(RSD)为1.2%~12.8%。此方法灵敏度高,重现性好,适用于水体中磺胺类药物的同时检测。海南省东寨港水样中共检测到5种磺胺类药物,检出率在60%~100%之间,其中磺胺甲恶唑(SMX)检出频率最高,10个样点都检测出含有SMX,同时磺胺对甲氧嘧啶(SME)和磺胺氯达嗪(SCP)这两种在其他报道中不作为检测对象的磺胺类药物在东寨港地区有较高的检出率(都为70%),另外检出的两种为磺胺甲嘧啶(SMA)和磺胺嘧啶(SDZ)。5种药物的检出质量浓度为nd^3.35 ng·L^-1,与国内其他水域相比,海南省东寨港水体中磺胺类药物的检出浓度处于较低水平。A method for simultaneous detection of 13 sulfonamides drugs in seawater by using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established and optimized,and used for analysis of the surface seawater samples collected from Dongzhai Harbour,Hainan.The results show that in case of the peak types of sulfonamides in the chromatogram are better and the correlation coefficient of the standard curve is high(R 2≥0.996)when the sulfaonamides in the sea water were determined by using UPLC-MS/MS with mobile phase A:methanol-acetonitrile(V∶V=1∶1)and mobile phase B:0.1%formic acid-10 mM ammonium acetate as the mobile phase and the initial mobile phase(5%mobile phase A and 95%mobile phase B)as the reconstituted solvent.Thirteen sulfonamides were separated well in 14 minutes and trheir recovery rates were from 70.4 to 103%,with a relative standard deviation(RSD)of between 1.2%and 12.8%.This method had high sensitivity and good reproducibility,and is suitable for simultaneous detection of sulfonamides in seawater.At the same time,five sulfonamides were detected in the water samples of the Dongzhai Harbour.The detection rates were from 60%to 100%.The highest detection frequency of sulfamethoxazole(SMX)was 100%,sulfameter(SME)and sulfachloropyridazine(SCP)had high detection rates(around 70%)in the Dongzhai Harbor,and the other two detected were sulfamethazine(SMA)and sulfadiazine(SDZ).The highest concentration of sulfonamides detected was up to 3.35 ng·L^-1.Compared with other areas,the concentrations of sulfonamides detected in Dongzhai Harbor was at a relatively low level.

关 键 词：超高效液相色谱串联质谱法(UPLC-MS/MS) 东寨港 表层海水 磺胺类药物 

分 类 号：X502[环境科学与工程—环境工程]