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

作　　者：黄招光 周彩丽 谢婷 邓杰华 黄炳泉 周云峰 HUANG Zhaoguang;ZHOU Caili;XIE Ting;DENG Jiehua;HUANG Bingquan;ZHOU Yunfeng(The Inspection and Testing Center of Yichun,Yichun Jiangxi 336000,China;The Second Affiliated Hospital of Yichun University,Yichun Jiangxi 336000,China;Yichun People's Hospital,Yichun Jiangxi 336000,China.)

机构地区：[1]宜春市检验检测中心,江西宜春336000 [2]宜春学院第二附属医院,江西宜春336000 [3]宜春市人民医院,江西宜春336000

出　　处：《药品评价》2024年第5期546-548,共3页Drug Evaluation

摘　　要：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.

关 键 词：腰息痛胶囊 续断 川续断皂苷Ⅵ 超高效液相色谱串联质谱法 含量 

分 类 号：R286.0[医药卫生—中药学]