高立红, 史亚利, 厉文辉, 刘杰民, 蔡亚岐＊

(1.中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085;2.北京科技大学土木与环境工程学院,北京100083)

高效液相色谱-电喷雾串联质谱法检测环境水样中22种抗生素类药物

高立红1,2, 史亚利1, 厉文辉1, 刘杰民2, 蔡亚岐1＊

(1.中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085;2.北京科技大学土木与环境工程学院,北京100083)

建立了高效液相色谱-电喷雾串联质谱(HPLC-ESIMS/MS)分析环境水样中22种抗生素类药物的方法。采用HLB固相萃取柱对环境水样中的目标化合物进行富集、净化,然后以6mL氨水-甲醇(5∶95,v/v)溶液洗脱。收集的洗脱液经氮气吹干至1mL,然后进行HPLC-ESIMS/MS分离分析。色谱流动相A相为甲醇-乙腈(1∶1,v/v),B相为0.3%(体积分数)甲酸水溶液(含0.1%(体积分数)甲酸铵,pH2.9);色谱柱为XTerra MS C18柱。质谱检测采用正离子扫描,多反应监测模式。分别以自来水和污水作为基质,22种抗生素类药物的加标平均回收率分别为54.9%～130%和57.4%～138%,相对标准偏差(n=3)分别为2.85%～28.6%和2.02%～23.2%;方法的检出限为0.05～0.5ng/L。将建立的方法应用于北京市高碑店湖和小清河水样的分析,结果表明在两个水样中均有部分抗生素类药物检出。

高效液相色谱-电喷雾串联质谱法;固相萃取;抗生素类药物;环境水样

Abstract:A method for the determination of22antibiotics in Environmental water samples was developed by using high perform anceliquid Chromatography-electrosp ray ionizationtandem mass spectrometry(HPLC-ESIMS/MS).The target antibiotics in water samples were enriched and cleaned-up by HLB solid-phase extraction(SPE)cartridges,and then eluted with6mL ammonium hydroxide-m ethanol(5∶95,V/V).The eluate was collected and concentrated to1 mL under a gentle stream of nitrogen gas,and then analyzed by HPLC-ESIMS/MS in positive electrospray ionization and multiple reaction monitoring(MRM)m ode.The separation was carried out on an XTerra MS C18column with mobile phases of A,m ethanol-acetonitrile(1∶1,v/v),and B,0.3%formic acid/water(containing0.1%ammonium form ate,V/V,pH2.9).The results show ed that the average recoveries of antibiotics in tap water and wastewater were54.9%-130%and57.4%-138%,respectively,and the corresponding relative standard deviations(RSD,n=3)were2.85%-28.6%and2.02%-23.2%,respectively.The method detection limits were0.05-0.5ng/L.The developed method was app lied to analyze the water samples of Gaobeidian Lake and Xiaoqinghe River in Beijing.The results show ed that some antibioticswere detected both in the two samples.

Key words:high performance liquid Chromatography-electrosp rayionizationtande mmass spectrometry(HPLC-ESI MS/MS);solid-phase extraction(SPE);antibiotics;Environmental water samples

抗生素(antibiotics)是指由细菌、霉菌或其他微生物在生活过程中所产生的具有抗病原体或其他活性的一类物质。抗生素类药物主要应用于人和动物的疾病治疗,同时也以亚治疗剂量长期添加于动物饲料中,以预防疾病和促进动物生长[1]。……