固相萃取-高效液相色谱法同时测定水体中的10种磺胺类抗生素  

Simultaneous Determination of 10 Sulfonamide Antibiotics in Water by Solid-phase Extraction and High Performance Liquid Chromatography

作　　者：洪蕾洁[1] 石璐[1] 张亚雷[1,2] 周雪飞[2] 朱洪光[3] 林双双[1] 

机构地区：[1]同济大学污染控制与资源化研究国家重点实验室,上海200092 [2]同济大学长江水环境教育部重点实验室,上海200092 [3]同济大学现代农业科学与工程研究院国家设施农业工程技术研究中心,上海200092

出　　处：《环境科学》2012年第2期652-657,共6页Environmental Science

基　　金：国家自然科学基金项目(41072172;41070641);科技部农业科技成果转化资金项目(2010GB23600672);上海市科委项目(10595812500);中国博士后科学基金项目(20100480625);中国博士后科学基金特别项目(201104274)

摘　　要：建立了一种采用固相萃取-高效液相色谱法同时测定水体中10种磺胺类抗生素的方法.样品经自制PEP固相萃取小柱富集净化、乙腈-二氯甲烷(2∶1,体积比)洗脱后,用高效液相色谱-紫外检测器测定.检测波长λ=268 nm,柱温33℃,流动相为乙腈-0.4%乙酸/水(体积比),采用梯度洗脱程序,实现了10种待测组分的基线分离,线性范围为10～2 000μg.L-1.去离子水和实际水样的加标回收率范围分别为73.4%～95.6%和70.2%～92.5%(磺胺除外,分别为8.5%和8.0%).整个分析方法的检出限为1.42～7.25 ng.L-1.应用此方法对上海市黄浦江部分河段江水、崇明岛地表水及地下水的测定表明在这几种不同水体环境中,不同频率地检出了磺胺类药物,浓度范围为13.3～241.5 ng.L-1,从而证明该方法具有快速简便、灵敏高效等优点,可满足实际工作的需要.A solid-phase extraction（SPE）-high performance liquid chromatography（HPLC） method has been developed for simultaneous determination of 10 sulfonamide antibiotics in water.The analytes were first enriched and purified through a PEP solid-phase extraction column,and eluted with acetonitrile-dichloromethane solution（2∶1,V/V）,then detected by a HPLC with a UV detector.The detection wavelength was 268 nm and the column temperature was 33℃,using gradient elution process with acetonitrile-0.4% acetic acid/water（V/V） as the mobile phase to achieve baseline separations of these 10 analytes.The linearity range was 10-2 000 μg·L-1.The recovery ranges of standard addition for deionized water and real water samples were 73.4%-95.6% and 70.2%-92.5%,respectively（except for sulfonamide,were 8.5% and 8.0%）.The limit of detection was 1.42-7.25 ng·L-1.Application of this method for parts of Huangpu River in Shanghai,surface water and groundwater in Chongming Island showed that sulfonamide antibiotics were detected in different frequencies in different aqueous environments,with the concentration range of 13.3-241.5 ng·L-1,proving this method is easy,rapid,sensitive and efficient to meet the needs of actual work.

关 键 词：磺胺 固相萃取 高效液相色谱 抗生素 环境水体 

分 类 号：X830.2[环境科学与工程—环境工程]