UPLC-MS/MS法测定腰息痛胶囊中川续断皂苷Ⅵ的含量

Content Determination of AsperosaponinⅥin Yaoxitong Capsules by UPLC-MS/MS

目的建立超高效液相色谱串联质谱法(UPLC-MS/MS)测定腰息痛胶囊中川续断皂苷Ⅵ的含量。方法液相条件为Waters ACQUITY UPLC®BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相为乙腈-0.1%甲酸溶液(梯度洗脱),流速为0.3 mL/min,柱温35℃,进样量5μL;质谱条件为电喷雾离子源(ESI)、正离子扫描模式,以多反应监测模式(MRM)进行数据采集,川续断皂苷Ⅵ的定量离子对为m/z 946.4→455.3。结果川续断皂苷Ⅵ在0.0787~3.9327μg/mL浓度范围内呈良好的线性关系(r=0.9987),精密度、重复性、稳定性的RSD分别为2.5%、4.1%、5.3%,平均加标回收率为95.9%。16批样品中川续断皂苷Ⅵ的含量范围为18.07~659.78μg/g。结论所建立的方法能对腰息痛胶囊中川续断皂苷Ⅵ的含量进行快速测定,有助于提升该制剂的质量。

Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of asperosaponinⅥin yaoxitong capsules.Methods The liquid phase was performed on a Waters ACQUITY UPLC®BEH C18 column(2.1 mm×100 mm,1.7μm)with mobile phase consisted of acetonitrile-0.1%formic acid(gradient elution)at the flow rate of 0.3 mL/min.The column temperature was 35℃,and the sample size was 5μL.The mass spectrometry conditions were electrospray ion source(ESI),positive ion scanning mode,and multi-reaction monitoring mode(MRM).The quantitative ion pair of asperosaponinⅥwas m/z 946.4→455.3.Results AsperosaponinⅥshowed a good linear relationship(r=0.9987)in the concentration range of 0.0787 to 3.9327μg/mL.RSDs of precision,repeatability and stability were 2.5%,4.1%and 5.3%,respectively,and the average recovery rate was 95.9%.The content of asperosaponinⅥin 16 batches of samples ranged from 18.07 to 659.78μg/g.Conclusion The method can be used to determine the content of asperosaponinⅥin yaoxitong capsules,which is helpful to improve the quality of the preparation.