Hilton Martin J, Thomas Kevin V
Centre for Environment, Fisheries and Aquaculture Science, Burnham Laboratory, Remembrance Avenue, Burnham on Crouch, Essex CM0 8HA, UK.
J Chromatogr A. 2003 Oct 10;1015(1-2):129-41. doi: 10.1016/s0021-9673(03)01213-5.
A simple method is presented for the analysis of 13 pharmaceutical and pharmaceutical metabolite compounds in sewage effluents and surface waters. The pharmaceutical compounds were extracted using a genetic solid-phase extraction (SPE) procedure using Phenomenex Strata X as a stationary phase. Extracts were quantitatively analysed by four separate reversed-phase high-performance liquid chromatography-electrospray tandem mass spectrometry (HPLC-ESI-MS/MS) techniques and quantified by comparison with an internal standard ([13C]-phenacetin). Recoveries and limits of detection (LOD) for sulfamethoxazole (120%, 50 ng l(-1)), acetyl-sulfamethoxazole (56%, 50 ng l(-1)), trimethoprim (123%, 10 ng l(-1)), erythromycin (73%, 10 ng l(-1)), paracetamol (75%, 50 ng l(-1)), ibuprofen (117%, 20 ng l(-1)), clofibric acid (83%, 50 ng l(-1)), mefenamic acid (24%, 50 ng l(-1)), diclofenac (62%, 20 ng l(-1)), propranolol (45%, 10 ng l(-1)), dextropropoxyphene (63%, 20 ng l(-1)) and tamoxifen (42%, 10 ng l(-1)) were all acceptable. The recovery of lofepramine (4%) was too low to be of use in a monitoring programme. Application of the method to samples collected from UK sewage effluents and surface waters showed detectable concentrations of mefenamic acid, diclofenac, propranolol, erythromycin, trimethoprim and acetyl-sulfamethoxazole in both matrices. Ibuprofen and dextropropoxyphene were detected in sewage effluents alone. All other pharmaceutical compounds were below the methods limits of detection.
本文介绍了一种分析污水和地表水中13种药物及药物代谢物化合物的简单方法。采用以菲罗门Strata X为固定相的遗传固相萃取（SPE）程序提取药物化合物。提取物通过四种单独的反相高效液相色谱 - 电喷雾串联质谱（HPLC - ESI - MS/MS）技术进行定量分析，并与内标（[13C] - 非那西丁）比较进行定量。磺胺甲恶唑（120%，50 ng l(-1)）、乙酰磺胺甲恶唑（56%，50 ng l(-1)）、甲氧苄啶（123%，10 ng l(-1)）、红霉素（73%，10 ng l(-1)）、对乙酰氨基酚（75%，50 ng l(-1)）、布洛芬（117%，20 ng l(-1)）、氯贝酸（83%，50 ng l(-1)）、甲芬那酸（24%，50 ng l(-1)）、双氯芬酸（62%，20 ng l(-1)）、普萘洛尔（45%，10 ng l(-1)）、右丙氧芬（63%，20 ng l(-1)）和他莫昔芬（42%，10 ng l(-1)）的回收率和检测限（LOD）均可以接受。洛非帕明的回收率（4%）过低，无法用于监测计划。将该方法应用于从英国污水和地表水采集的样品中，两种基质中均检测到了甲芬那酸、双氯芬酸、普萘洛尔、红霉素、甲氧苄啶和乙酰磺胺甲恶唑的可检测浓度。仅在污水中检测到了布洛芬和右丙氧芬。所有其他药物化合物均低于方法的检测限。
