天然产物研究与开发 ›› 2016, Vol. 28 ›› Issue (8): 1233-1237.doi: 10.16333/j.1001-6880.2016.8.011

• 研究简报 • 上一篇    下一篇

UPLC-MS/MS同时测定白及中6个指标成分的含量

梅朝叶1,4,向文英1,杨武1,黄勇1,2,王永林1,2,王爱民1,3*   

  1. 1 贵州医科大学 贵州省药物制剂重点实验室;2 贵州医科大学药学院;3 贵州医科大学 民族药与中药开发应用教育部工程研究中心;4 国家苗药工程技术研究中心,贵阳 550004
  • 出版日期:2016-08-30 发布日期:2017-01-17

Simultaneous Determination of Six Components in Bletilla striata by UPLC-MS/MS

MEI Chao-ye1,4,XIANG Wen-ying1,YANG Wu1,HUANG Yong1,2,WANG Yong-lin1,2,WANG Ai-min1,3*   

  1. 1 Guizhou Provincial Key Laboratory of Pharmaceutics,School of Pharmacy;2School of Pharmacy,Guizhou Medical University;3Engineering Research Center for the Development and Application of Ethnic Medicine and TCM (Ministry of Education),Guizhou Medical University;4National Engineering Research Center of Miaos Medicines,Guiyang 550004,China
  • Online:2016-08-30 Published:2017-01-17

摘要: 建立UPLC-MS/MS同时测定白及药材中的α-异丁基苹果酸(B6)、4-(葡萄糖氧基)-肉桂酸葡萄糖氧基苄酯(B12)、1,4-二[4-(葡萄糖氧)苄基-2-异丁基苹果酸酯(B14)、1-[4-(葡萄糖氧)苄基]-2-异丁基苹果酸(B17)、二氢菲1(B19)和1,4-二[4-(葡萄糖氧)苄基]-2-异丁基苹果酸酯-2-[4-O-肉桂酰基-6-O-乙酰基]葡萄糖苷(B23)含量的分析方法,采用Acquity UPLC BEH C18柱(2.1 mm×50 mm,1.7 μm);流动相0.1 %甲酸乙腈溶液(A)-0.1 %甲酸水溶液(B)为流动相,梯度洗脱,采用电喷雾离子源(ESI),多反应离子监测(MRM)模式进行正负离子同步监测。各指标成分之间分离度良好,在选定的浓度范围内线性关系良好(r≥0.9974),平均加样回收率为98.07%~103.19%,RSD<3.04%为,重复性、精密度和稳定性良好。此方法操作简便,快速,灵敏度高,可用于白及药材中主要活性成分的含量测定,并为白及药材的质量控制提供了新方法。

关键词: 白及, UPLC-MS/MS, 多反应离子监测模式, 含量测定

Abstract: To establish an UPLC-MS/MS method for the simultaneous determination of α-isobutylmalic acid (B6),blestroside (B12),militarine (B14),gymnosides V (B17),dihydrophenanthrenes 1 (B19) and gymnosides IX (B23) in Bletilla striata. An Acquity UPLC BEH C-18 column(2.1 mm×50 mm,1.7 μm)was used with the mobile phase of 0.1% formic acid in acetonitrile-0.1% formic acid in water by gradient elution.Multiple reaction monitoring (MRM) mode was used for the detection by electro-spray ionization (ESI) source.The results showed that six components can be well resolved and that in the selected linear range,all calibration curves of the six components showed good linearity (r≥0.9974).The average recoveries were 98.07%-103.19%,with RSDs <3.04%. Repeatability,precision and stability were good.The developed method was simple,rapid,sensitive and suitable for the determination of the main active constituents in B.Striata.It provided a new method for the quality control of B.Striata.

Key words: Bletilla striata, UPLC-MS/MS, multiple reaction monitoring, content determination

中图分类号: 

R927.2