SPE和LC-MS/MS联用同时检测水体中的15种抗生素  

Simultaneous detection of 15 antibiotics in water by SPE and LC-MS /MS

作　　者：张兰河[1] 丘晓春[1] 薛成[1,2] 高如泰[2] 许其功[2] 席北斗[2] 

机构地区：[1]东北电力大学化学工程学院,吉林132012 [2]中国环境科学研究院,北京100012

出　　处：《环境工程学报》2013年第11期4326-4332,共7页Chinese Journal of Environmental Engineering

基　　金：国家"水体污染控制与治理"科技重大专项(2012ZX07209-003);吉林省教育厅科学技术研究项目(2012-95)

摘　　要：采用（SPE）固相萃取柱进行分离富集，使用LC—MS／MS联用仪进行检测，建立了一种高效、低成本的可同时检测水体中多种抗生素的方法，并在河北省子牙河流域汪洋沟水体抗生素污染现状调查中得到应用。实验结果表明，（1）最优实验条件的选择为：水样体积为1L，洗脱剂用量为10mL，pH为3．0；（2）回收率达到69．2％～86．3％，相对标准偏差在1．8％～8．4％之间，表明检测结果准确度和灵敏度均较高；（3）在所检测的15种抗生素中，头孢西丁、土霉素、氯唑西林和布洛芬4种抗生素是该河流的主要抗生素污染物，其含量比重（中位数）高达73．5％，检测浓度最高（中位数）的是磺胺类抗生素，浓度为100．4ng／L；（4）各抗生素的含量从上游到下游大体呈逐渐衰减的趋势，这主要归因于下游支流的稀释作用，但水体中抗生素浓度仍远高于已有报道的地区；（5）污染源解析表明，水体中抗生素主要来源于制药企业的废水，部分来源于附近居民的生活污水。An efficient detection method was established using LC-MS/MS spectrometer after the solid phase extraction column for separation and enrichment, which was low-cost and could simultaneously detect mul- tiple antibiotics in waters. This method was applied in the antibiotics pollution investigation of Wangyang River in Ziya River basin of Hebei Province. The experimental results showed that the optimal experimental conditions as follows ： the sample volume of 1 L, and the eluent of 10 mL, and the pH of 3.0. In the test, recovery of sample arranged from 69.2% to 86. 3% , the relative standard deviation was between 1.8% and 8.4% , indicating that the test results were higher accuracy and sensitivity. In the detection of 15 kinds of antibiotics, four antibiotics including cefoxitin, oxytetracycline, cloxacillin, and ibuprofen were the main antibiotics pollutants in the river, the content（median） proportion of which was up to 73.5%. The highest detectable concentration （median） was sulfa antibiotic, its concentration was 100.4 ng/L. The content of each antibiotic gradually from upstream to downstream generally decreased, which was mainly due to the dilution effect of the downstream tributaries, but the antibiotic concentration in this water was still higher than the results of other areas which were reported. The pollution sources analysis results showed that antibiotic in the waters mainly derived from the wastewater of the pharmaceutical companies, while partly from the sewage of the nearby residents.

关 键 词：抗生素 固相萃取 检测方法 多种 

分 类 号：X830.2[环境科学与工程—环境工程]