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目的采用液相色谱-串联质谱法测定人血浆中二甲双胍的浓度。方法血浆样品用乙腈(含0.1%甲酸)沉淀蛋白后用二氯甲烷反洗后进行分析。使用Agilent C8(75 mm×4.6 mm,3.5μm)色谱柱。流动相:A泵:5 mmol/L醋酸铵(三乙胺调pH值至7.5),B泵:乙腈。线性梯度洗脱,流速0.4 mL/min。采用电喷雾离子源,多反应离子监测。用于定量分析的离子对二甲双胍为130.2/71.1,内标吗啉胍为172.2/60.2。结果线性范围为50～2 000 ng/mL,最低定量限为50 ng/mL,预处理回收率为81.7%～98.0%,二甲双胍的基质效应<9.97%,日内和日间相对标准偏差均<5.2%。结论液相色谱-串联质谱法快速、简便、灵敏度高,是一种适用于人血浆中药物浓度的测定及药物动力学和生物利用度研究的方法。
Objective To determine the concentration of metformin in human plasma by liquid chromatography-tandem mass spectrometry. Methods Plasma samples were analyzed by acetonitrile (containing 0.1% formic acid) after precipitation of protein and back-washing with methylene chloride. Use an Agilent C8 (75 mm × 4.6 mm, 3.5 μm) column. Mobile phase: A pump: 5 mmol / L ammonium acetate (triethylamine adjusted to pH 7.5), B pump: acetonitrile. Linear gradient elution, flow rate 0.4 mL / min. Electrospray ionization, multi-reactive ion monitoring. The ion pair metformin used for the quantitative analysis was 130.2 / 71.1, and the internal standard Moroxydine was 172.2 / 60.2. Results The linear range was 50-2 000 ng / mL, the lowest limit of quantification was 50 ng / mL, the pretreatment recovery was 81.7% -98.0%, the matrix effect of metformin was <9.97%, and the relative standard deviations were <5.2 %. Conclusion Liquid chromatography-tandem mass spectrometry is rapid, simple and sensitive. It is a suitable method for the determination of drug concentration and pharmacokinetics and bioavailability in human plasma.