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中国药学(英文版) ›› 2014, Vol. 23 ›› Issue (4): 225-232.DOI: 10.5246/jcps.2014.04.031

• 【研究论文】 • 上一篇    下一篇

UPLC-MS/MS法同时测定消栓通络方中18种成分的含量

赵艳, 刘敏, 杨钊, 王少华, 李杨, 杜冠华*   

  1. 1. 青岛大学医学院, 山东 青岛 266071
    2. 青岛大学医学院附属青岛市市立医院, 山东 青岛 266011
    3. 青岛市药检所, 山东 青岛 266071
    4. 中国医学科学院 北京协和医学院药物研究所国家药物筛选中心, 北京 100050
  • 收稿日期:2013-11-21 修回日期:2013-12-24 出版日期:2014-04-28 发布日期:2014-01-07
  • 通讯作者: *Corresponding author. Tel./Fax: 86-10-63165184; E-mail: dugh@imm.ac.cn
  • 作者简介:*Corresponding author. Tel./Fax: 86-10-63165184; E-mail: dugh@imm.ac.cn
  • 基金资助:
    National Natural Science Foundation of China (Grant No. 30630073).

Simultaneous quantification of eighteen constituents in traditional Chinese medicine XiaoShuanTongLuo by UPLC-MS/MS  

Yan Zhao, Min Liu, Zhao Yang, Shaohua Wang, Yang Li, Guanhua Du*   

  1. 1. Medical College, Qingdao University, Qingdao 266071, China
    2. Qingdao Municipal Hospital, Affiliated Hospital of Medical College, Qingdao University, Qingdao 266011, China
    3. Qingdao Institute for Drug Control, Qingdao 266071, China
    4. National Centre for Pharmaceutical Screening, Institute of Materia Medica, Chinese Academy of Medical Science and Peking Union Medical College, Beijing 100050, China
  • Received:2013-11-21 Revised:2013-12-24 Online:2014-04-28 Published:2014-01-07
  • Contact: *Corresponding author. Tel./Fax: 86-10-63165184; E-mail: dugh@imm.ac.cn
  • About author:*Corresponding author. Tel./Fax: 86-10-63165184; E-mail: dugh@imm.ac.cn
  • Supported by:
    National Natural Science Foundation of China (Grant No. 30630073).

摘要:

栓通络方是临床应用广泛的中药复方制剂。本文建立了一种可同时检测该方剂中18种活性成分的超高效液相-串联四级杆质谱方法。采用多反应监测(MRM)模式测定, 离子化方式选择ESI+ESI。利用BEH C18 (2.1 mm×100 mm, 1.7 μm)色谱柱进行分离, 甲醇-0.1%甲酸溶液0.2 mL/min梯度洗脱。18种活性成分测定的线性范围多在0.001-0.5 μg/mL之间, r值在0.9896-0.9996之间; 高、中、低3个水平日内、日间精密度RSD<15%; 室温24 h稳定性RSD<15%。应用该方法对4种不同剂型的市售消栓通络方制剂18种活性成分进行了测定, 结果显示该方法快速、准确、灵敏、重现性好, 可用于消栓通络方制剂的质量控制。

关键词: 中药, 消栓通络, 超高效液相色谱, 三重四极杆串联质谱, 质量控制

Abstract:

XiaoShuanTongLuo (XSTL) is an important multi-herbal formula widely used as a traditional Chinese medicine (TCM). Inthis paper, an ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometric method (UPLC-ESI-MS/MS) was developed for the simultaneous identification and quantification of18chemical constituents in the extract of XSTL.The analysis was performed in multiple-reaction monitoring (MRM) mode using positive and negative electrospray ionization (ESI). A BEH C18 (2.1 mm×100 mm, 1.7 μm) column with a gradient mobile phaseof methanol–0.1% aqueous formic acid solution at a flow rate of 0.2 mL/min was used for separation. The standard curves of most components showed good linearity over the concentration range of 0.0010.5 μg/mL withr = 0.98960.9996. The relative standard deviations (RSD) of intra-day and inter-day precision were all lower than 15% at low, middle, and high concentration levels. The RSD of stability analysis in 24 h were also lower than 15%. The validated method was employed to quantify 18 active components simultaneously in four different commercial brands of XSTL products in various dosage forms. The developed method was rapid, accurate, sensitive, and reproducible for the quality control of XSTL.

Key words: Traditional Chinese medicine, XiaoShuanTongLuo, Ultra-performance liquid chromatography, Triple quadrupole tandem mass spectrometer, Quality control

中图分类号: 

Supporting: National Natural Science Foundation of China (Grant No. 30630073).