LC-MS/MS法测定痰热清注射液中连翘酯苷E的含量

Determination of forsythoside E in Tanreqing injection by LC-MS/MS

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,3.5μm)进行分析,流动相为乙腈-0.01%甲酸水溶液,流速0.3mL·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 separa- ted on an Agilent SB - C18 column（2. 1 mm × 15 mm,3.5 μm） for gradient elution with a mobile phase of aeetoni- trile -0. 01% formic acid water - solution at a flow rate of 0.3 mL · min-1. Then the processed sample was ana- lyzed 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 injec- tion 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.