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目的:建立LC-MS/MS同时检测大鼠血浆中5种酚酸类成分的分析方法,为丹参提取物血浆样品的测定提供参考。方法:采用LC-MS/MS同时检测丹酚酸A,B,C和紫草酸、迷迭香酸含量,流动相0.1%甲酸水溶液-甲醇和乙腈等体积混合液(含0.1%甲酸)梯度洗脱,流速0.6 m L·min-1。质谱条件采用多反应监测方式进行负离子监测。定量分析的离子对m/z分别为493.3/295.1,717.5/519.1,491.2/293.2,537.3/295.1,359.1/161.0,5种成分的定量分析可在7 min内完成。结果:丹酚酸A,B和紫草酸线性范围均为0.78~100μg·L-1,丹酚酸C和迷迭香酸线性范围均为0.39~50μg·L-1。日内及日间精密度RSD均<15%,准确度92%~112%。结论:该法选择性强、灵敏度高、操作简便,适用于丹参总酚酸中5种酚酸类成分在大鼠血浆中的药代动力学研究。
OBJECTIVE: To establish a method for the simultaneous determination of five phenolic acids in rat plasma by LC-MS / MS, and to provide a reference for the determination of plasma samples of Salvia miltiorrhiza extract. Methods: LC-MS / MS simultaneous detection of salvianolic acid A, B, C and lithospermate, rosmarinic acid content, mobile phase 0.1% formic acid aqueous solution - methanol and acetonitrile volume mixture (containing 0.1% formic acid) Off, the flow rate of 0.6 m L · min-1. The conditions of mass spectrometry were monitored by means of multiple reaction monitoring. Quantitative analysis of the ion pair m / z were 493.3 / 295.1,717.5 / 519.1,491.2 / 293.2,537.3 / 295.1,359.1 / 161.0 quantitative analysis of five components can be completed within 7 min. Results: The linear range of salvianolic acid A, B and lithospermic acid were 0.78 ~ 100μg · L-1, the linear range of salvianolic acid C and rosmarinic acid were 0.39 ~ 50μg · L-1. Intra-day and intra-day precision RSD <15%, accuracy 92% ~ 112%. Conclusion: The method is selective, sensitive and easy to operate. It is suitable for the pharmacokinetic study of five phenolic acids in plasma of rat salvianolic acid.