Chiral analysis of metoprolol and two of its metabolites, α-hydroxymetoprolol and deaminated metoprolol, in wastewater using liquid chromatography-tandem mass spectrometry
Chiral analysis of metoprolol and two of its metabolites, α-hydroxymetoprolol and deaminated metoprolol, in wastewater using liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/j.chroma.2012.09.090
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发表时间：
2012-12-21
影响因子：
4.1
通讯作者：
Pettersson, Curt E.
中科院分区：
文献类型：
--
作者：
Barclay, Victoria K. H.;Tyrefors, Niklas L.;Pettersson, Curt E.
建立了环境水样中美托洛尔及其主要代谢产物α-羟基美托洛尔（alpha-OH-Met）和脱氨基美托洛尔（COOH-Met）的LC-MS/MS手性分离方法。目标碱，美托洛尔和α-OH-Met，以及酸性代谢产物（COOH-Met），采用Oasis HLB柱固相萃取法从水样中提取。地表水中所有化合物的萃取回收率均>= 73%。研究了四种不同类型的手性固定相对美托洛尔及其代谢物Chiralcel OD-H、Chirobiotic V. Chiral AGP和Chiral CBH的8种立体异构体的分离。在最后一种方法中，美托洛尔和α-OH-Met的四个立体异构体被手性CBH拆分，COOH-Met的对映体被手性AGP拆分。通过三重四极杆质谱法在SRM模式下检测分析物。该方法适用于手性分析的分析物在处理后的废水样品从乌普萨拉，瑞典。检测并分析了样品中α-OH-Met的对映异构体和非对映异构体。α-OH-Met的三种第一洗脱立体异构体的浓度在54和61 pM之间。有趣的是，发现最后洗脱的立体异构体在相同的采样时间以151 pM的浓度存在。据作者所知，这是第一次在废水样品中检测到α-OH-Met的立体异构体。美托洛尔的对映体在相同基质中测定为1.77和1.86 nM。COOH-Met的对映体在处理后的废水样品中未检测到高于方法检测限（42 pM）。开发的LC-MS/MS方法在废水样品中进行了验证。(C)2012 Elsevier B. V.保留所有权利。
A LC-MS/MS method for the chiral separation of metoprolol and two of its main metabolites, alpha-hydroxymetoprolol (alpha-OH-Met) and deaminated metoprolol (COOH-Met), in environmental water samples has been developed. The target bases, metoprolol and alpha-OH-Met, as well as the acidic metabolite (COOH-Met) were extracted from water samples by a solid phase extraction method employing Oasis HLB cartridges. The extraction recoveries were >= 73% for all compounds in surface water. Four different types of chiral stationary phases were investigated for the separation of the eight stereoisomers of metaprolol and its metabolites, Chiralcel OD-H, Chirobiotic V. Chiral AGP and Chiral CBH. In the final method, the enantiomers of metoprolol and four stereoisomers of alpha-OH-Met were separated using Chiral CBH, the enantiomers of COOH-Met were separated employing Chiral AGP. The analytes were detected in SRM mode by triple quadrupole mass spectrometry. The method was applied for the chiral analysis of the analytes in treated wastewater samples from Uppsala, Sweden. The enantiomers and diastereoisomers of alpha-OH-Met were detected and analyzed in the samples. The concentrations of the three first eluting stereoisomers of alpha-OH-Met were between 54 and 61 pM. Interestingly, the last eluting stereoisomer was found to be present at a concentration of 151 pM at the same sampling occasion. This is, to the best of the authors' knowledge, the first time the stereoisomers of alpha-OH-Met have been detected in wastewater samples. The enantiomers of metoprolol were determined to be 1.77 and 1.86 nM in the same matrix. The enantiomers of COOH-Met were not detected above the method detection limit (42 pM) in treated wastewater samples. The developed LC-MS/MS methods were validated in wastewater samples. (C) 2012 Elsevier B.V. All rights reserved.