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目的:建立快速、灵敏的液相色谱-串联质谱方法测定大鼠血浆中6,7-二甲氧基香豆素浓度。方法:40μl血浆样品中药物经含内标的甲醇溶液蛋白沉淀,于12000 rpm离心取上清液稀释后,以乙腈-0.1%甲酸10 mmol/L甲酸铵溶液为流动相,梯度洗脱方式分离。使用电喷雾电离源以多反应监测(MRM)方式进行正离子检测。结果:确定丰度最高的2对离子m/z 207.2→m/z 107.0(6,7-二甲氧基香豆素)和m/z 147.0→m/z 91.0(香豆素),用于定性定量分析。该方法在0.5 ng/ml~2500 ng/ml的浓度范围内线性良好,相关系数r=0.9951。结论:本文首次建立了简便、快速、灵敏、专属的测定大鼠血浆中6,7-二甲氧基香豆素的LC-MS/MS分析方法。
OBJECTIVE: To establish a rapid and sensitive LC-MS / MS method for the determination of 6,7-dimethoxycoumarin in rat plasma. METHODS: The drug was precipitated in 40 μl of plasma sample by centrifugation and centrifuged at 12000 rpm. The supernatant was diluted with acetonitrile-0.1% formic acid in 10 mmol / L ammonium formate solution and separated by gradient elution. Electrospray ionization sources are used for positive ion detection in multiple reaction monitoring (MRM) mode. Results: Two pairs of ions m / z 207.2 → m / z 107.0 (6,7-dimethoxycoumarin) and m / z 147.0 → m / z 91.0 (coumarin) with the highest abundance were identified for Qualitative and quantitative analysis. The method was linear over a concentration range of 0.5 ng / ml to 2500 ng / ml with a correlation coefficient of r = 0.9951. Conclusion: This study established the simple, rapid, sensitive and specific LC-MS / MS method for the determination of 6,7-dimethoxycoumarin in rat plasma for the first time.