Rapid determination of pharmaceuticals from multiple therapeutic classes in wastewater by solid-phase extraction and ultra-performance liquid chromatography tandem mass spectrometry  

作　　者：SUI Qian HUANG Jun DENG ShuBo YU Gang 

机构地区：[1]POPs Research Centre, Department of Environmental Science and Engineering, Tsinghua University, Beijing 100084, China

出　　处：《Chinese Science Bulletin》2009年第24期4633-4643,共11页

基　　金：Supported by by the National Science Fund for Distinguished Young Scholars (Grant No. 50625823) ;National Natural Science Foundation of China (Grant No. 50538090)

摘　　要：A new analytical method utilizing ultra-performance liquid chromatography (UPLC) tandem mass spectrometry (MS/MS) has been developed to determine 16 pharmaceuticals from 8 therapeutic classes in wastewater: bezafibrate, clofibric acid, carbamazepine, caffeine, chloramphenicol, diclofenac, gemfibrozil, indomethacin, ketoprofen, mefenamic acid, metoprolol, nalidixic acid, N,N-diethyl-metatoluamide, propranolol, sulpiride and trimethoprim. Key parameters of MS/MS, UPLC and solid phase extraction (SPE) were optimized. In general, recovery of target pharmaceuticals was over 70% for the wastewater effluent samples and 50% for the influent samples. The effects of matrix suppression, loss during the pretreatment as well as instrument variability were successfully corrected by two internal standards, and acceptable relative recovery was obtained. Target compounds were quantitatively analyzed using multiple reaction monitoring (MRM) mode, and the detection limits ranged from 0.3 to 20 ng/L. A detailed study, matrix effect in effluent wastewater was also present. The method was applied to detecting pharmaceuticals in the wastewater from three wastewater treatment plants (WWTPs) in Beijing, China and the results demonstrated that most target compounds were detectable in both the influent and effluent, with the mean concentrations ranging from 20.5 to 5775.6 ng/L and 4.6 to 418.6 ng/L, respectively.A new analytical method utilizing ultra-performance liquid chromatography （UPLC） tandem mass spectrometry （MS/MS） has been developed to determine 16 pharmaceuticals from 8 therapeutic classes in wastewater： bezafibrate, clofibric acid, carbamazepine, caffeine, chloramphenicol, diclofenac, gemfibrozil, indomethacin, ketoprofen, mefenamic acid, metoprolol, nalidixic acid, N,N-diethyl-metatoluamide, propranolol, sulpiride and trimethoprim. Key parameters of MS/MS, UPLC and solid phase extraction （SPE） were optimized. In general, recovery of target pharmaceuticals was over 70% for the wastewater effluent samples and 50% for the influent samples. The effects of matrix suppression, loss during the pretreatment as well as instrument variability were successfully corrected by two internal standards, and acceptable relative recovery was obtained. Target compounds were quantitatively analyzed using multiple reaction monitoring （MRM） mode, and the detection limits ranged from 0.3 to 20 ng/L. A detailed study, matrix effect in effluent wastewater was also present. The method was applied to detecting pharmaceuticals in the wastewater from three wastewater treatment plants （WWTPs） in Beijing, China and the results demonstrated that most target compounds were detectable in both the influent and effluent, with the mean concentrations ranging from 20.5 to 5775.6 ng/L and 4.6 to 418.6 ng/L, respectively.

关 键 词：高效液相色谱 串联质谱法 固相萃取 废水 药品 快速测定 治疗 污水处理厂 

分 类 号：TQ463.4[化学工程—制药化工] O657.72[理学—分析化学]