Zuehlke Sebastian, Duennbier Uwe, Heberer Thomas
Institute of Food Chemistry, Technical University Berlin, Gustav-Meyer-Allee 25, 13355 Berlin, Germany.
Anal Chem. 2004 Nov 15;76(22):6548-54. doi: 10.1021/ac049324m.
A simple and rapid method is presented for the trace-level analysis of 10 polar pharmaceutical residues in various types of water samples from the aquatic environment. Using this method, the pharmaceuticals and several drug metabolites can be analyzed in drinking and surface waters and in wastewater (treated and untreated sewage) at concentrations down to 0.01 microg/L. Samples are prepared by a simple in situ derivatization enabling the preconcentration of very polar metabolites by automated solid-phase extraction. The analytes were separated by liquid chromatography with tandem mass spectrometric detection and quantified by comparison with an internal standard. Limits of quantification were between 0.01 and 0.02 microg/L for three phenazone-type pharmaceuticals, six of their metabolites, and the antiepileptic drug carbamazepine. Except for dimethylaminophenazone, recoveries for all analytes were between 87 and 117% for raw and purified sewage, groundwater, and surface and drinking water. Investigations of some environmental samples revealed that sewage and surface water treatment causes a slight reduction of the concentrations of some analytes whereas other compounds were persistent during water treatment. Thus, some compounds were detected at the low-microgram per liter level in sewage effluents of wastewater treatment plants in Berlin (Germany) and were also found at high-nanogram per liter concentrations in Berlin surface water samples.
本文介绍了一种简单快速的方法,用于对水环境中各类水样中的10种极性药物残留进行痕量分析。采用该方法,可对饮用水、地表水以及废水(处理后的和未处理的污水)中的药物及其几种代谢物进行分析,检测限低至0.01μg/L。通过简单的原位衍生化制备样品,可通过自动固相萃取对极性很强的代谢物进行预富集。采用液相色谱 - 串联质谱检测对分析物进行分离,并与内标比较进行定量。三种非那宗类药物、其六种代谢物以及抗癫痫药物卡马西平的定量限在0.01至0.02μg/L之间。除二甲基氨基非那宗外,所有分析物在原污水和净化污水、地下水、地表水及饮用水中的回收率在87%至117%之间。对一些环境样品的调查表明,污水和地表水的处理会使某些分析物的浓度略有降低,而其他化合物在水处理过程中具有持久性。因此,在德国柏林污水处理厂的污水排放中检测到了一些化合物,其浓度为每升几微克,在柏林地表水样品中也发现了每升高达几纳克的浓度。