UPLC-MS/MS法测定腰息痛胶囊中川续断皂苷Ⅵ的含量
Content Determination of Asperosaponin Ⅵ in Yaoxitong Capsules by UPLC-MS/MS
黄招光 1周彩丽 2谢婷 3邓杰华 1黄炳泉 1周云峰1
作者信息
- 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
- 折叠
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,1.7 μm),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5 μL;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 0.078 7～3.932 7 μg/mL浓度范围内呈良好的线性关系(r=0.998 7),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 18.07～659.78 μg/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.
Abstract
Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of asperosaponinⅥ in yaoxitong capsules.Methods The liquid phase was performed on a Waters ACQUITY UPLC® BEH C18 column(2.1 mm×100 mm,1.7 μm)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 5 μL.The mass spectrometry conditions were electrospray ion source(ESI),positive ion scanning mode,and multi-reaction monitoring mode(MRM).The quantitative ion pair of asperosaponin Ⅵ was m/z 946.4→455.3.Results Asperosaponin Ⅵ showed a good linear relationship(r=0.998 7)in the concentration range of 0.078 7 to 3.932 7 μg/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 asperosaponin Ⅵin 16 batches of samples ranged from 18.07 to 659.78 μg/g.Conclusion The method can be used to determine the content of asperosaponin Ⅵ in 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Key words
Yaoxitong capsules/Dipsaci radix/Asperosaponin Ⅵ/UPLC-MS/MS/Content引用本文复制引用
出版年
2024
NETL
NSTL
万方数据