Department of Excellence-Biomedical Sciences and Public Health, Università Politecnica delle Marche, 60121 Ancona, Italy.
Phenomenex Inc., 411 Madrid Ave., Torrance, 90501 CA, USA.
J Pharm Biomed Anal. 2023 Jun 15;230:115384. doi: 10.1016/j.jpba.2023.115384. Epub 2023 Mar 31.
In the present work an isocratic enantioselective high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the separation and quantitative determination of dextro - and levo -methorphan and their pharmacologically relevant metabolites, dextrorphan and levorphanol, respectively, in human blood samples. The separation of enantiomers of methorphan and metabolites was performed on the polysaccharide-based chiral column Lux AMP in combination with acetonitrile and 5 mM aqueous ammonium bicarbonate pH 11 in the ratio 50:50 (%, v/v) as mobile phase with the flow rate 1 mL/min. The mass spectrometer was operated in scheduled multiple reaction monitoring (MRM) mode, with four transitions for each dextromethorpan, levomethorphan, dextrorphan and dextromethorphan-d3 and two transitions for each levorphanol, levorphanol-d3 and dextrorphan-d3. Application of this method to human post-mortem blood samples confirmed cases of severe overdosing with dextromethorphan, levomethorphan, and less commonly with both.
本工作建立了一种等度对映选择性高效液相色谱-串联质谱（LC-MS/MS）方法，用于分离和定量测定人血样中右美沙芬和左美沙芬及其相关药理学代谢物右旋-和左-去甲啡烷、右啡烷和左啡烷。在多糖手性柱 Lux AMP 上，以乙腈和 5 mM 碳酸氢铵 pH 11（体积比 50:50，%，v/v）为流动相，流速为 1 mL/min，实现了对映体的分离。质谱仪以预定多重反应监测（MRM）模式运行，每个右美沙芬、左美沙芬、右啡烷和右美沙芬-d3 有四个转换，每个左啡烷、左啡烷-d3 和右啡烷-d3 有两个转换。该方法应用于人死后血样，证实了严重过量服用右美沙芬、左美沙芬的情况，且较少见地同时服用这两种药物。
