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)

• 1:沈阳药科大学中药学院基于靶点的药物设计与研究教育部重点实验室
• 2:军事医学科学院毒物药物研究所
• 3:河南宛西制药股份有限公司
• 4:ABSCIEX公司亚太技术支持中心

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

Abstract:

Keywords:

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)

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