六味地黄浓缩丸HPLC指纹图谱研究HPLC fingerprint of Liuwei Dihuang condensed pills
高新彪;孙磊;乔善义;高松;车彦忠;张克荣;
GAO Xin-biao1,SUN Lei2,QIAO Shan-yi2,GAO Song3,CHE Yan-zhong3,ZHANG Ke-rong4(1.Key Laboratory of Structure Based Drug Design & Discovery of Ministry of Education,School of Traditional Chinese Materia Medica,Shenyang Pharmaceutical University,Shenyang 110016,China; 2.Institute of Pharmacology and Toxicology,Academy of Military Medical Sciences,Beijing 100850,China; 3.Henan Wanxi Pharmaceutical Co.,Ltd.,Nanyang 473000,China; 4.AB SCIEX Asia Pacific Technology Support Center,Shanghai 200233,China)
摘要(Abstract):
目的:建立六味地黄浓缩丸的HPLC指纹图谱。方法:Dikma Diamonsil C18色谱柱(4.6 mm×250 mm,5μm);以乙腈(含0.05%磷酸)-水(含0.05%磷酸)为流动相梯度洗脱;柱温40℃;流速1.0 mL·min-1;检测波长276 nm(0~10min),236 nm(10~40 min),276 nm(40~60 min);进样量20μL。采用Q-TOF-MS-IDA-MS/MS进行色谱峰指认。结果:该方法精密度、稳定性、重复性良好。采用Q-TOF-MS-IDA-MS/MS对22个共有峰中的18个色谱峰进行了定性鉴别。采用该方法测定了10批六味地黄浓缩丸,其相似度均在0.96以上。结论:该研究为六味地黄浓缩丸的全面质量评价奠定了基础。
Objective: To establish HPLC fingerprints of Liuwei Dihuang condensed pills.Method: Dikma Diamonsil C18 column(4.6 mm×250 mm,5 μm) was adopted,with acetonitrile(containing 0.05% phosphoric)-water(containing 0.05% phosphoric) as the mobile phase.The column temperature was set at 40 ℃,and the flow rate was 1.0 mL·min-1.The detection wavelength was 276 nm(0-10 min),236 nm(10-40 min) and 276 nm(40-60 min).The sample size was 20 μL.Chromatographic peaks were identified by Q-TOF-MS-IDA-MS/MS method.Result: Good precision,stability and repeatability were proved.Q-TOF-MS-IDA-MS/MS method was adopted for qualitative determination of eighteen chromatographic peaks.Ten batches of Liuwei Dihuang condensed pills were determined with the method,and their similarities were above 0.96.Conclusion: The study lays a foundation for the overall quality evaluation of Liuwei Dihuang condensed pills.
关键词(KeyWords):
六味地黄浓缩丸;HPLC;指纹图谱;质量评价
Liuwei Dihuang condensed pills;HPLC;fingerprint;quality evaluation
基金项目(Foundation): 国家“重大新药创制”科技重大专项(2011ZX09201-201-13,2009ZX09301002);; 国家科技支撑计划项目(2006BAI08B03-08)
作者(Author):
高新彪;孙磊;乔善义;高松;车彦忠;张克荣;
GAO Xin-biao1,SUN Lei2,QIAO Shan-yi2,GAO Song3,CHE Yan-zhong3,ZHANG Ke-rong4(1.Key Laboratory of Structure Based Drug Design & Discovery of Ministry of Education,School of Traditional Chinese Materia Medica,Shenyang Pharmaceutical University,Shenyang 110016,China; 2.Institute of Pharmacology and Toxicology,Academy of Military Medical Sciences,Beijing 100850,China; 3.Henan Wanxi Pharmaceutical Co.,Ltd.,Nanyang 473000,China; 4.AB SCIEX Asia Pacific Technology Support Center,Shanghai 200233,China)
Email:
DOI:
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- 高新彪
- 孙磊
- 乔善义
- 高松
- 车彦忠
- 张克荣
GAO Xin-biao1- SUN Lei2
- QIAO Shan-yi2
- GAO Song3
- CHE Yan-zhong3
- ZHANG Ke-rong4(1.Key Laboratory of Structure Based Drug Design & Discovery of Ministry of Education
- School of Traditional Chinese Materia Medica
- Shenyang Pharmaceutical University
- Shenyang 110016
- China
- 2.Institute of Pharmacology and Toxicology
- Academy of Military Medical Sciences
- Beijing 100850
- China
- 3.Henan Wanxi Pharmaceutical Co.
- Ltd.
- Nanyang 473000
- China
- 4.AB SCIEX Asia Pacific Technology Support Center
- Shanghai 200233
- China)
- 高新彪
- 孙磊
- 乔善义
- 高松
- 车彦忠
- 张克荣
GAO Xin-biao1- SUN Lei2
- QIAO Shan-yi2
- GAO Song3
- CHE Yan-zhong3
- ZHANG Ke-rong4(1.Key Laboratory of Structure Based Drug Design & Discovery of Ministry of Education
- School of Traditional Chinese Materia Medica
- Shenyang Pharmaceutical University
- Shenyang 110016
- China
- 2.Institute of Pharmacology and Toxicology
- Academy of Military Medical Sciences
- Beijing 100850
- China
- 3.Henan Wanxi Pharmaceutical Co.
- Ltd.
- Nanyang 473000
- China
- 4.AB SCIEX Asia Pacific Technology Support Center
- Shanghai 200233
- China)