Greener bioanalytical approach for LC/MS-MS assay of enalapril and enalaprilat in human plasma with total replacement of acetonitrile throughout all analytical stages
Greener bioanalytical approach for LC/MS-MS assay of enalapril and enalaprilat in human plasma with total replacement of acetonitrile throughout all analytical stages
复制标题
DOI：
10.1016/j.jchromb.2012.11.023
复制
发表时间：
2013-05-15
影响因子：
3
通讯作者：
Medvedovici, Andrei
中科院分区：
文献类型：
--
作者：
Cheregi, Mihaela;Albu, Florin;Medvedovici, Andrei
绿色生物分析方法旨在最大限度地减少或消除与生物分析应用相关的危险化学品。通过从样品制备和色谱分离阶段消除乙腈，实现LC/MS-MS测定人血浆中的依那普利和依那普利拉。用1-辛醇液-液萃取（LLE）代替加入乙腈的蛋白质沉淀（PP），然后将有机层直接大体积进样到反相（RP）分离机制下操作的色谱柱中。同时，在移动的相中用碳酸丙烯酯/乙醇（7/3，v/v）混合物代替乙腈作为有机改性剂。验证了三种分析替代品（（I）乙腈PP+乙腈色谱洗脱;（II）1-辛醇LLE+乙腈色谱洗脱;（III）1-辛醇LLE+碳酸丙烯酯/乙醇色谱洗脱），并比较了质量特性。这些替代分析方法之间的比较也是基于通过应用Bland-Altman程序在生物等效性研究期间采集的真实样品获得的结果。(C)2012 Elsevier B. V.保留所有权利。
Green bioanalytical approaches are oriented toward minimization or elimination of hazardous chemicals associated to bioanalytical applications. LC/MS-MS assay of enalapril and enalaprilat in human plasma was achieved by elimination of acetonitrile from both sample preparation and chromatographic separation stages. Protein precipitation (PP) by acetonitrile addition was replaced by liquid-liquid extraction (LLE) in 1-octanol followed by direct large volume injection of the organic layer in the chromatographic column operated under reversed phase (RP) separation mechanism. At the mean time, acetonitrile used as organic modifier in the mobile phase was successfully replaced by a mixture of propylene carbonate/ethanol (7/3, v/v). Three analytical alternatives ((I) acetonitrile PP+ acetonitrile based chromatographic elution; (II) 1-octanol LLE+ acetonitrile based chromatographic elution; (III) 1-octanol LLE+ propylene carbonate/ethanol based chromatographic elution) were validated and the quality characteristics were compared. Comparison between these alternative analytical approaches was also based on results obtained on incurred samples taken during a bioequivalence study, through application of the Bland-Altman procedure. (C) 2012 Elsevier B.V. All rights reserved.