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黄连-黄芩药对UPLC-MS/MS指纹图谱
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国家自然科学基金项目(81660666);贵州省优秀青年科技人才培养对象专项[黔科合人字(2011)28号];中药民族药药剂学专业学位研究生工作站项目(黔教研合YJSZ字[2013]05);国家苗药工程技术研究中心项目(2014FU125Q09)


UPLC-MS/MS Fingerprint of Coptidis Rhizoma-Scutellariae Radix Herbal Pair
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    摘要:

    目的:建立黄连-黄芩药对的UPLC-MS/MS指纹图谱分析方法,为其整体质量控制与评价、药效物质基础、配伍规律等研究提供科学依据。方法:采用UPLC-MS/MS法进行指纹图谱研究,使用ACQUITY UPLC BEH C18 色谱柱(2.1 mm×100 mm,1.7 μm),以0.2% 甲酸水-乙腈为流动相,梯度洗脱80 min,流速0.3 mL·min-1,柱温40 ℃,获得12批黄连-黄芩药对的色谱图。利用国家药典委员会颁布的“中药色谱指纹图谱相似度评价系统” 2004A 版对其进行相似度评价。结果:建立了黄连-黄芩药对UPLC-MS/MS指纹图谱的共有模式,确定了16个共有峰,通过比较对照品和参考文献,指认了7个共有峰分别为黄连碱、表小檗碱、盐酸药根碱、黄芩苷、盐酸小檗碱、盐酸巴马汀、汉黄芩苷,对12批不同产地和品种的黄连-黄芩药对相似度进行了考察,其相似度均>0.9。结论:建立了黄连-黄芩药对UPLC-MS/MS指纹图谱分析方法,其精密度、重复性及稳定性良好(RSD<3% ),该分析方法的建立对于黄连-黄芩药对的质量控制与评价、药效物质基础、配伍规律等研究具有一定的参考价值和意义。

    Abstract:

    Objective: To provide a scientific evidence for studying overall quality control and evaluation, pharmacodynamic material basis and compatibility regularity of Coptidis Rhizoma-Scutellariae Radix herbal pair by establishing an analytical method of UPLC-MS/MS fingerprint. Method: The chromatograms of twelve batches of Coptidis Rhizoma-Scutellariae Radix herbal medicine pairs were acquired by the method of UPLC-MS/MS. ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm) was adopted and eluted with the mobile phase of water (0.2% formic acid)-acetonitrile in a gradient mode for 80 min at the speed of 0.3 mL·min-1, and the column temperature was 40 ℃. The similarity was evaluated on the basis of the Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine (version 2004A) issued by Chinese Pharmacopoeia Commission. Result: The common pattern of fingerprint of Coptidis Rhizoma-Scutellariae Radix herbal pair was established, and totally 16 common peaks were identified. Compared with control substances and references, seven common peaks were identified as coptisine, epiberberine, jatrorrhizine hydrochloride, baicalin, berberine hydrochloride, palmatine hydrochloride and wogonoside. The similarities of Coptidis Rhizoma-Scutellariae Radix herbal pairs of 12 batches of different origins and species were investigated, all of which reached 0.9. Conclusion: The analytical method of UPLC-MS/MS fingerprint of Coptidis Rhizoma-Scutellariae Radix herbal pair has a good accuracy, repeatability and stability (RSD<3%). It has a certain reference value for studying overall quality control and evaluation, pharmacodynamic material basis and compatibility regularity of Coptidis Rhizoma-Scutellariae Radix herbal pair.

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王钰乐,刘文,杨道斌,卿勇军,杜平,金阳.黄连-黄芩药对UPLC-MS/MS指纹图谱[J].中国实验方剂学杂志,2017,23(13):80~85

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  • 收稿日期:2017-04-19
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  • 在线发布日期: 2017-05-23
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