Boleda Ma Rosa, Galceran Ma Teresa, Ventura Francesc
AGBAR, Aigües de Barcelona, Avinguda Diagonal 211, 08018 Barcelona, Spain.
J Chromatogr A. 2007 Dec 14;1175(1):38-48. doi: 10.1016/j.chroma.2007.10.029. Epub 2007 Oct 17.
A fast and reliable method using solid-phase extraction and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed for the simultaneous detection, identification and quantification of several central nervous system depressor drugs of abuse such as cannabinoids (Delta9-tetrahydrocannabinol, THC) and opiates (morphine, codeine, heroin, methadone, fentanyl) and their metabolites in water samples. Compounds were extracted from water by using Oasis HLB cartridges. After SPE enrichment, the selected depressor drugs, under UPLC optimized conditions, were separated in less than 8 min. Electrospray (ESI) tandem MS in positive ion mode and selected reaction monitoring was used for quantification. ESI-MS/MS conditions such as capillary and cone voltages, source and desolvation temperatures and cone and desolvation gas flow rates have been optimized and MS and MS/MS spectra of the studied compounds were obtained. At the working conditions four identification points were obtained as required by European Union guidelines for analysis by LC-MS/MS. Quality parameters (intra-day and inter-day precisions) for each analyte have been established in three different matrixes (purified, surface and waste waters). Recoveries were generally higher than 70% and instrumental quantification limits and limits of quantification were in the low pg and ng/l range, respectively. Finally, the method has been applied to the analysis of influent and effluents wastewaters and natural water samples from Catalonia (NE Spain) where the presence of several opiates such as morphine, codeine, norcodeine 2-ethylene-1,5-dimethyl-3,3-diphenylpyrrolidine and methadone and cannnabinoids such as THC and 11-nor-carboxy-Delta9-tetrahydrocannabinol has been demonstrated.
已开发出一种使用固相萃取和超高效液相色谱 - 串联质谱法(UPLC-MS/MS)的快速可靠方法,用于同时检测、鉴定和定量水样品中几种中枢神经系统抑制性滥用药物,如大麻素(Δ9-四氢大麻酚,THC)和阿片类药物(吗啡、可待因、海洛因、美沙酮、芬太尼)及其代谢物。使用Oasis HLB柱从水中萃取化合物。经过固相萃取富集后,在UPLC优化条件下,所选的抑制性药物在不到8分钟内即可分离。采用正离子模式的电喷雾(ESI)串联质谱和选择反应监测进行定量分析。对ESI-MS/MS条件,如毛细管电压、锥孔电压、源温度、脱溶剂温度、锥孔气流速率和脱溶剂气流速率进行了优化,并获得了所研究化合物的质谱和二级质谱图。在这些工作条件下,按照欧盟LC-MS/MS分析指南的要求获得了四个鉴定点。已在三种不同基质(纯化水、地表水和废水)中确定了每种分析物的质量参数(日内和日间精密度)。回收率一般高于70%,仪器定量限和定量限分别在低皮克和纳克/升范围内。最后,该方法已应用于加泰罗尼亚(西班牙东北部)进水和出水废水以及天然水样的分析,其中已证明存在几种阿片类药物,如吗啡、可待因、去甲可待因、2-乙烯基-1,5-二甲基-3,3-二苯基吡咯烷和美沙酮,以及大麻素,如THC和11-去甲-羧基-Δ9-四氢大麻酚。