Tbilisi State University, Institute of Physical and Analytical Chemistry, School of Exact and Natural Sciences, Tbilisi 0179, Georgia.
Tbilisi State University, Institute of Physical and Analytical Chemistry, School of Exact and Natural Sciences, Tbilisi 0179, Georgia; Department of Excellence-Biomedical Sciences and Public Health, Università Politecnica delle Marche, Ancona 60121, Italy.
J Pharm Biomed Anal. 2024 Jan 5;237:115769. doi: 10.1016/j.jpba.2023.115769. Epub 2023 Oct 5.
Recently we proposed an isocratic enantioselective high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the separation and quantitative determination of dextro- (DXM) and levo-methorphan (LVM) and their pharmacologically relevant metabolites, dextrorphan and levorphanol, respectively, in human blood samples. This method was based on the polysaccharide-based chiral column Lux AMP, a specialty column characterized with high stability in mobile phases of pH 11.0 and above. The use of a single-source column is a limitation for any analytical method. Therefore, the major goal of the present study was to develop an enantioselective method for the differentiation of dextro- and levo-methorphan, as well as their metabolites dextrorphan and levorphanol, using Lux Cellulose-3 as alternative chiral column with methanol containing 0.1 % diethylamine mobile phase. A newly developed method uses a chiral selector part of HPLC columns available from multiple manufacturers and a fairly common mobile phase. The method was validated and applied to post-mortem blood samples. Out of 50 analyzed new samples, dextromethorphan (DXM) was detected in 17 samples. Of these 17 cases DXM was accompanied with LVM in 7 samples. The proposed analytical method is relatively simple, accurate and fast and can be adopted for routine use in forensic and clinical toxicology laboratories.
最近，我们提出了一种等度手性高效液相色谱-串联质谱（LC-MS/MS）方法，用于分离和定量测定人体血液样本中的右旋（DXM）和左甲吗喃（LVM）及其相应的药理学代谢物，即右旋苯丙胺和左旋羟吗啡。该方法基于多糖基手性柱 Lux AMP，该专用柱在 pH 值为 11.0 及以上的流动相中具有高稳定性。使用单一来源的色谱柱是任何分析方法的局限性。因此，本研究的主要目标是开发一种手性方法，用于区分右旋和左甲吗喃，以及它们的代谢物右旋苯丙胺和左旋羟吗啡，使用 Lux Cellulose-3 作为替代手性柱，以甲醇和 0.1%二乙胺作为流动相。一种新开发的方法使用来自多个制造商的 HPLC 柱的手性选择器部分和相当常见的流动相。该方法经过验证并应用于死后血液样本。在分析的 50 个新样本中，有 17 个样本检测到了右美沙芬（DXM）。在这 17 个病例中，有 7 个病例同时伴有 LVM。所提出的分析方法相对简单、准确、快速，可用于法医和临床毒理学实验室的常规使用。
