Xu Renai, Xu Tao, Wang Zhe, Zhan Haichao, Chen Xiaole, Wang Xianqin, Hu Lufeng, Zhang Xiuhua
Department of Pharmacy, The First Affiliated Hospital of Wenzhou Medical College, Wenzhou, China.
Pharmazie. 2012 Jun;67(6):485-9.
A highly selective and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for quantitating dextromethorphan (DXM) and its metabolite dextrophan (DXO) in rat plasma using pirfenidone as an internal standard. Protein precipitation with acetonitrile was employed for the sample preparation. Chromatographic separation was achieved on a SB-C18 column at 25 degrees C, with a gradient elution programme of which acetonitrile-0.1% formic acid in water as mobile phase. The flow rate was 0.4 mL/min. Detection is carried out by multiple reaction monitoring (MRM) on a ion-trap LC-MS/MS system with an electrospray ionization interface. The assay is linear over the range 1-500 ng/mL for DXM and 1-250 ng/mL for DXO, with a lower limit of quantitation of 1 ng/mL for both. Intra- and inter-day precision of the assay were less than 9.80% and the accuracy were in the range 96.35-106.39%. The developed method was successfully applied to analyze the drug in samples of rat plasma for pharmacokinetic study.
建立了一种高选择性和灵敏的液相色谱 - 串联质谱（LC-MS/MS）方法，并以吡非尼酮为内标物，用于定量大鼠血浆中的右美沙芬（DXM）及其代谢物右啡烷（DXO）。采用乙腈沉淀蛋白的方法进行样品制备。在25℃下于SB-C18柱上进行色谱分离，以乙腈 - 0.1%甲酸水溶液为流动相的梯度洗脱程序。流速为0.4 mL/min。通过具有电喷雾电离接口的离子阱LC-MS/MS系统上的多反应监测（MRM）进行检测。该测定法在1 - 500 ng/mL范围内对DXM和1 - 250 ng/mL范围内对DXO呈线性，两者的定量下限均为1 ng/mL。该测定法的日内和日间精密度均小于9.80%，准确度在96.35 - 106.39%范围内。所建立的方法成功应用于大鼠血浆样品中药物的分析，用于药代动力学研究。
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