School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China.
Fitoterapia. 2013 Sep;89:271-7. doi: 10.1016/j.fitote.2013.05.024. Epub 2013 Jun 4.
A rapid, sensitive and selective high-performance liquid chromatography mass spectrometric method has been developed and validated for the simultaneous determination of oxymatrine and its active metabolite matrine in human plasma after administration of oxymatrine oral solution. Analytes were extracted from the plasma by liquid-liquid extraction with chloroform. The chromatographic separation was accomplished on a Venusil C18 column (150 mm × 4.6 mm, 5 μm) protected by a C18 guard column (4.0 mm × 2.0 nm; Phenomenex, Torrance, CA, USA). Analytes were detected on a single quadruple mass spectrometer by selected ion monitoring mode via electrospray ionization source. The assay had a lower limit of quantification of 1.5 ng·mL(-1) for oxymatrine and 3 ng·mL(-1) for matrine in plasma. The calibration curves were linear in the measured range. The overall precision and accuracy for all concentrations of quality controls and standards were within ±15%. The proposed method enabled unambiguous identification and quantification of oxymatrine and its active metabolite matrine in vivo. The results provided a meaningful basis for evaluating the clinical applications of the oxymatrine oral solution.
建立并验证了一种灵敏、快速、专属性强的高效液相色谱-串联质谱法,用于测定口服氧化苦参碱溶液后人体血浆中氧化苦参碱及其活性代谢物苦参碱的浓度。以氯仿进行液-液萃取,从血浆中提取分析物。采用 Venusil C18 柱(150mm×4.6mm,5μm),保护柱为 C18 柱(4.0mm×2.0nm;Phenomenex,Torrance,CA,USA)进行色谱分离。在电喷雾离子源的选择离子监测模式下,单四极杆质谱仪进行检测。氧化苦参碱和苦参碱在血浆中的定量下限均为 1.5ng·mL(-1)。在测定范围内,校准曲线呈线性。所有质控和标准品浓度的精密度和准确度均在±15%以内。该方法能够明确鉴定和定量分析体内的氧化苦参碱及其活性代谢物苦参碱。结果为评估氧化苦参碱口服溶液的临床应用提供了有意义的依据。