Huerta-Fontela Maria, Galceran Maria Teresa, Ventura Francesc
AGBAR-Aigües de Barcelona, Avinguda Diagonal 211, 08018 Barcelona, Spain.
Anal Chem. 2007 May 15;79(10):3821-9. doi: 10.1021/ac062370x. Epub 2007 Apr 17.
Ultraperformance liquid chromatography coupled to electrospray tandem mass spectrometry was used for the rapid and simultaneous analysis of 15 stimulatory drugs in water. Cocaine, amphetamine-related compounds, LSD, ketamine, PCP, fentanyl, and metabolites, among the controlled drugs, and nicotine, caffeine, and their metabolites, among the noncontrolled drugs, were studied. Chromatographic separation was achieved in less than 4.5 min, with improved peak resolution and sensitivity. Identification and quantification of the compounds of interest was performed by selected reaction monitoring, using an electrospray ionization source. Isotope dilution (except for paraxanthine) was used for quantitation. Quality parameters of the method were established, and limits of quantification were obtained for controlled drugs in surface waters from 0.1 to 3.1 ng/L and in wastewaters from 0.2 to 4.0 ng/L. Run-to-run and day-to-day precisions were evaluated in different water matrixes (Milli-Q water, surface water, wastewater). To assess the presence of these drugs in real water samples, the optimized method was applied to the analysis of wastewater and surface river water. The analysis of several samples from wastewater treatment plants in northeast Spain revealed the presence of drugs such as cocaine and amphetamine-related compounds, in both influent and effluent samples. Cocaine metabolite and MDMA (ecstasy) were also found in surface waters while nicotine and caffeine were detected in all the analyzed samples. The results obtained demonstrate that the presence of these drugs in the aquatic media must be considered a matter of environmental concern.
超高效液相色谱-电喷雾串联质谱联用技术用于快速同时分析水中的15种兴奋剂药物。研究了受控药物中的可卡因、苯丙胺类化合物、麦角酸二乙酰胺(LSD)、氯胺酮、苯环己哌啶(PCP)、芬太尼及其代谢物,以及非受控药物中的尼古丁、咖啡因及其代谢物。在不到4.5分钟内实现了色谱分离,提高了峰分辨率和灵敏度。采用电喷雾电离源,通过选择反应监测对目标化合物进行鉴定和定量。除了对甲基黄嘌呤外,采用同位素稀释法进行定量。建立了该方法的质量参数,获得了地表水和废水中受控药物的定量限,地表水为0.1至3.1纳克/升,废水为0.2至4.0纳克/升。在不同水基质(超纯水、地表水、废水)中评估了批内和批间精密度。为评估实际水样中这些药物的存在情况,将优化后的方法应用于废水和地表水分析。对西班牙东北部污水处理厂的多个样品分析表明,进水和出水样品中均存在可卡因和苯丙胺类化合物等药物。地表水还发现了可卡因代谢物和3,4-亚甲基二氧甲基苯丙胺(摇头丸),而在所有分析样品中均检测到尼古丁和咖啡因。所得结果表明,必须将这些药物在水生介质中的存在视为一个环境问题。