LC-MS/MS法测定痰热清注射液中连翘酯苷E的含量

目的:建立高效液相色谱-四极杆串联质谱联用法(LC-MS/MS法)测定痰热清注射液中连翘酯苷E的含量。 方法:样品经稀释后,采用Agilent SB-C₁₈色谱柱(2.1 mm×15 mm,3.5 μm)进行分析,流动相为乙腈-0.01%甲酸水溶液,流速0.3 mL·min^-1,梯度洗脱;质谱采用电喷雾离子化(ESI)源,负离子-多反应监测(MRM)模式。 结果:连翘酯苷E的线性范围为47.5~950 ng·mL^-1;低、中、高浓度平均回收率(n=3)分别为99.0%、103.0%、95.2%,RSD分别为3.4%、1.5%、1.0%。13批样品的连翘酯苷E含量在0.077~0.145 mg·mL^-1之间。 结论:该方法可用于痰热清注射液中连翘酯苷E的测定。

Objective: To establish a liquid chromatography-tandem mass spectrometric method(LC-MS/MS)for the determination of forsythoside E in Tanreqing injection. Methods: After being diluted,the sample was separated on an Agilent SB-C₁₈ column(2.1 mm×15 mm,3.5 μm)for gradient elution with a mobile phase of acetonitrile-0.01% formic acid water-solution at a flow rate of 0.3 mL·min^-1.Then the processed sample was analyzed by tandem mass spectrometer with negative-electrospray ionization(ESI)source,monitored under a multiple reaction monitoring(MRM)mode. Results: The calibration curve showed a good linearity in the range of 47.5-950 ng·mL^-1.The average recoveries(n=3)of low,middle and high concentrations were 99.0%,103.0%,95.2% with RSDs of 3.4%,1.5% and 1.0%,respectively.The content of forsythoside E in 13 batches of Tanreqing injection samples was in the range of 0.077-0.145 mg·mL^-1. Conclusion: The developed method can be used for the quantitative determination of forsythoside E in Tanreqing injection.

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