基于定量核磁共振技术的人参皂苷对照品质量评价方法研究  

Quality evaluation of ginsenoside reference substances based on qNMR spectroscopy

作　　者：潘坚扬[1,2] 赵芳[1,2,3] 李文竹[1,2] 瞿海斌 PAN Jian-yang;ZHAO Fang;LI Wen-zhu;QU Hai-bin(Pharmaceutical Informatics Institute,College of Pharmaceutical Sciences,Zhejiang University,Hangzhou 310058,China;Innovation Center in Zhejiang University,State Key Laboratory of Component-Based Chinese Medicine,Hangzhou 310058,China;Hisun Biopharmaceutical Co.,Ltd.,Hangzhou 311400,China)

机构地区：[1]浙江大学药学院药物信息学研究所,浙江杭州310058 [2]组分中药国家重点实验室浙江大学交叉创新中心,浙江杭州310058 [3]海正生物制药有限公司,浙江杭州311400

出　　处：《中国中药杂志》2022年第3期575-580,共6页China Journal of Chinese Materia Medica

基　　金：国家“重大新药创制”科技重大专项(2018ZX09201011-002)。

摘　　要：建立基于定量核磁共振(quantitative nuclear magnetic resonance,qNMR)技术的人参皂苷对照品质量评价方法。采用Bruker AvanceⅢ500 MHz核磁共振仪,配备5 mm BBO探头,采集定量氢谱,30°脉冲,弛豫延迟时间D_(1)为20 s,探头温度为303 K,采样次数为32次。采用绝对定量法,选择高纯度的定量核磁共振用内标对苯二甲酸二甲酯,以灵敏度相对较好的甲基峰作为定量峰,结合线性拟合解卷积处理提高积分结果的准确性,建立了基于qNMR技术的人参皂苷对照品质量评价方法,并完成方法学验证。采用建立的qNMR对5种人参皂苷类对照品人参皂苷Rg_(1)、人参皂苷Re、人参皂苷Rb_(1)、人参皂苷Rd和三七皂苷R;进行质量评价研究,结果表明5种人参皂苷对照品qNMR测定值低于厂家提供的HPLC归一化含量。该方法可以保障人参皂苷对照品的质量,同时也为相关中药材及其制剂质量评价的准确性提供有力支持。基于qNMR技术的中药对照品质量评价方法简单、快捷、结果准确,值得推广用于中药对照品的质量值定量测定。The present study established a quality evaluation method for ginsenoside reference substances based on quantitative nuclear magnetic resonance(qNMR)spectroscopy.^(1)H-NMR spectra were collected on Bruker AvanceⅢ500 MHz NMR spectrometer equipped with a 5 mm BBO probe.The acquire parameters were set up as follows:pulse sequence of 30°,D_(1)=20 s,probe temperature=303 K,and the scan number=32.Dimethyl terephthalate,a high-quality^(1)H-qNMR standard,was used as the internal standard and measured by the absolute quantitative method.Methyl peaks of comparatively good sensitivity were selected for quantification,and linear fitting deconvolution was adopted to improve the accuracy of integration results.The qNMR spectroscopy-based method was established and validated,which was then used for the quality evaluation of ginsenoside Rg_(1),ginsenoside Re,ginsenoside Rb_(1),ginsenoside Rd,and notoginsenoside R;.The results suggested that the content of these ginsenoside reference standards obtained from the qNMR spectroscopy-based method was lower than that detected by the normalization method in HPLC provided by the manufacturers.In conclusion,the qNMR spectroscopy-based method can ensure the quality of ginsenoside reference substances and provide powerful support for the accurate quality evaluation of Chinese medicine and its preparations.The qNMR spectroscopy-based method is simple,rapid,and accurate,which can be developed for the quantitative assay of Chinese medicine standard references.

关 键 词：定量核磁共振法 人参皂苷RG 人参皂苷RE 人参皂苷RB 人参皂苷RD 三七皂苷R 对苯二甲酸二甲酯 

分 类 号：R284.1[医药卫生—中药学]