高效液相色譜-電噴霧串聯質譜法檢測環境水樣中22種抗生素類藥物

高立紅, 史亞利, 厲文輝, 劉杰民, 蔡亞岐＊

(1.中國科學院生態環境研究中心環境化學與生態毒理學國家重點實驗室,北京100085;2.北京科技大學土木與環境工程學院,北京100083)

高效液相色譜-電噴霧串聯質譜法檢測環境水樣中22種抗生素類藥物

高立紅1,2, 史亞利1, 厲文輝1, 劉杰民2, 蔡亞岐1＊

(1.中國科學院生態環境研究中心環境化學與生態毒理學國家重點實驗室,北京100085;2.北京科技大學土木與環境工程學院,北京100083)

建立了高效液相色譜-電噴霧串聯質譜(HPLC-ESIMS/MS)分析環境水樣中22種抗生素類藥物的方法。采用HLB固相萃取柱對環境水樣中的目標化合物進行富集、凈化,然后以6mL氨水-甲醇(5∶95,v/v)溶液洗脫。收集的洗脫液經氮氣吹干至1mL,然后進行HPLC-ESIMS/MS分離分析。色譜流動相A相為甲醇-乙腈(1∶1,v/v),B相為0.3%(體積分數)甲酸水溶液(含0.1%(體積分數)甲酸銨,pH2.9);色譜柱為XTerra MS C18柱。質譜檢測采用正離子掃描,多反應監測模式。分別以自來水和污水作為基質,22種抗生素類藥物的加標平均回收率分別為54.9%～130%和57.4%～138%,相對標準偏差(n=3)分別為2.85%～28.6%和2.02%～23.2%;方法的檢出限為0.05～0.5ng/L。將建立的方法應用于北京市高碑店湖和小清河水樣的分析,結果表明在兩個水樣中均有部分抗生素類藥物檢出。

高效液相色譜-電噴霧串聯質譜法;固相萃取;抗生素類藥物;環境水樣

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)是指由細菌、霉菌或其他微生物在生活過程中所產生的具有抗病原體或其他活性的一類物質。抗生素類藥物主要應用于人和動物的疾病治療,同時也以亞治療劑量長期添加于動物飼料中,以預防疾病和促進動物生長[1]。……