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

Chinese Science Bulletin (Impact Factor: 1.37). 07/2009; 54(24):4633-4643. DOI: 10.1007/s11434-009-0413-y

ABSTRACT 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, gem-fibrozil, indomethacin, ketoprofen, mefenamic acid, metoprolol, nalidixic acid, N,N-diethyl-meta-tol-uamide, 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 ana-lyzed 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 Bei-jing, China and the results demonstrated that most target compounds were detectable in both the in-fluent and effluent, with the mean concentrations ranging from 20.5 to 5775.6 ng/L and 4.6 to 418.6 ng/L, respectively. pharmaceuticals, solid phase extraction, tandem mass spectrometry, UPLC, wastewater

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    ABSTRACT: The application of appropriate advanced treat-ment process in the municipal wastewater treatment plants (WWTPs) has become an important issue considering the elimination of emerging contaminants, such as pharma-ceutical and personal care products (PPCPs). In the present study, the removal of 13 PPCPs belonging to different therapeutic classes by the sequential ultraviolet (UV) and ozonation process in a full-scale WWTP in Beijing was investigated over the course of ten months. Most of the target PPCPs were effectively removed, and the median removal efficiencies of individual PPCPs, ranging from – 13% to 89%, were dependent on their reaction rate constants with molecular ozone. Noticeable fluctuation in the removal efficiencies of the same PPCPs was observed in different sampling campaigns. Nevertheless, the sequential UV and ozonation process still made a significant contribution to the total elimination of most PPCPs in the full-scale WWTP, by compensating for the poor or fluctuant removal performance of PPCPs by biologic treatment process.
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May 22, 2014