黄敏烨;李振雨;童培珍;曹斯琼;魏梅;孙冬梅;潘礼业;陈向东;
HUANG Min-ye;LI Zhen-yu;TONG Pei-zhen;CAO Si-qiong;WEI Mei;SUN Dong-mei;PAN Li-ye;CHEN Xiang-dong;Guangdong Provincial Key Laboratory of Traditional Chinese Medicine Formula, Guangdong Yifang Pharmaceutical Co., Ltd.;

• 1:广东一方制药有限公司广东省中药配方颗粒企业重点实验室

摘要(Abstract)：

建立土贝母药材UPLC指纹图谱,并采用一测多评法(QAMS)测定其中3种皂苷类成分的含量,为土贝母药材质量评价提供依据。采用Waters Cortecs T3色谱柱(2.1 mm×100 mm,1.6μm),乙腈-0.1%磷酸溶液为流动相进行梯度洗脱,流速0.3 mL·min~(-1),检测波长203 nm,柱温30℃,进样量1μL,建立土贝母药材UPLC指纹图谱,并采用相似度计算、聚类分析和主成分分析法对指纹图谱进行评价。以土贝母苷甲为内参物,测定土贝母苷乙、土贝母苷丙的相对校正因子,利用相对校正因子计算含量,建立一测多评法,并将一测多评的计算结果与外标法(ESM)测定结果进行比较,从而确定一测多评的准确性及可行性。结果显示,19批土贝母药材指纹图谱有4个共有峰,相似度在0.754～1.000,聚类分析及主成分分析将19批药材分为3类,与相似度评价结果一致;采用一测多评法计算的19批土贝母药材土贝母苷乙、土贝母苷丙的含量与外标法测定的实际含量的相对偏差均小于5.0%,说明2种方法无明显差异。因此,UPLC指纹图谱结合一测多评法可以有效用于土贝母药材的质量评价。
The present study was performed to establish the UPLC fingerprints of Bolbostemmatis Rhizoma and determine the contents of three saponins by quantitative analysis of multi-components by single marker(QAMS), and provide basis for quality evaluation of Bolbostemmatis Rhizoma. The analysis was carried out on an analytical column of Waters Cortecs T3(2.1 mm×100 mm,1.6 μm)with gradient elution by acetonitrile-0.1% phosphoric acid solution, at a flow rate of 0.3 mL·min~(-1). The detection wavelength was 203 nm, the column temperature was 30 ℃ and the injection volume was 1 μL. The UPLC fingerprints of Bolbostemmatis Rhizoma were established and evaluated by similarity calculation, cluster analysis and principal component analysis. The relative calibration factors of toberoside B and toberoside C were determined with toberoside A as internal reference. The content was calculated by relative calibration factors to develop a method of QAMS. Comparing the results of QAMS with those of ESM, the accuracy and feasibility of one-eva-luation and multi-evaluation can be determined. Results showed that the fingerprints of 19 batches of Bolbostemmatis Rhizoma have four common peaks with similarities ranging from 0.754 to 1.000. Cluster analysis and principal component analysis classified 19 batches of Bolbostemmatis Rhizoma into three categories, which was consistent with the similarity evaluation results. The relative deviation between the content of tubeicosides B and C in 19 batches of Bolbostemmatis Rhizoma determined by QAMS and ESM is less than 5.0%, indicating that there was no significant difference between the two methods. Therefore, the UPLC fingerprints combined with QAMS and similarity evaluation can be effectively used to evaluate the quality of Bolbostemmatis Rhizoma.

关键词(KeyWords)： 土贝母;UPLC指纹图谱;一测多评法;质量评价
Bolbostemmatis Rhizoma;UPLC fingerprints;quantitative analysis of multi-components by single marker(QAMS);quality evaluation

Abstract:

Keywords:

基金项目(Foundation): 广东省省级科技计划项目(2018B030323004)

作者(Author): 黄敏烨;李振雨;童培珍;曹斯琼;魏梅;孙冬梅;潘礼业;陈向东;
HUANG Min-ye;LI Zhen-yu;TONG Pei-zhen;CAO Si-qiong;WEI Mei;SUN Dong-mei;PAN Li-ye;CHEN Xiang-dong;Guangdong Provincial Key Laboratory of Traditional Chinese Medicine Formula, Guangdong Yifang Pharmaceutical Co., Ltd.;

Email:

DOI:

参考文献(References)：

• [1] 朱晓丹,安超,姜敏,等.从文献角度探索中药土贝母药用源流[J].环球中药,2018,11(6):884.
• [2] 国家药典委员会.中华人民共和国药典.一部[S].北京:中国医药科技出版社,2015:17.
• [3] 马挺军,李军,屠鹏飞,等.土贝母的化学成分研究[J].西北植物学报,2005,25(6):1163.
• [4] 刘文庸,陈伟光,张卫东,等.土贝母化学成分研究[J].中国中药杂志,2004,29(10):28.
• [5] 向梅先,吴丽,范亚,等.土贝母乙酸乙酯部位化学成分研究[J].中南民族大学学报:自然科学版,2017,36(2):56.
• [6] 郑春辉,付红伟,裴月湖.土贝母化学成分的分离与鉴定[J].中国药物化学杂志,2005,15(5):291.
• [7] 李娟,何峰,尹娴,等.土贝母正丁醇部位化学成分研究[J].华中师范大学学报:自然科学版,2016,50(5):721.
• [8] 孙健,温庆辉.土贝母的化学成分及药理作用研究进展[J].中国药物警戒,2010,7(7):430.
• [9] 王智民,高慧敏,付雪涛,等.“一测多评”法中药质量评价模式方法学研究[J].中国中药杂志,2006,31(23):1925.
• [10] 曾滟棱,谭宁,高艳,等.不同产地土贝母中皂苷类成分的HPLC特征图谱及3种主要皂苷的含量测定[J].药物评价研究,2018,41(10):1816
• [11] 侯文文,石燕红,宋嬿,等.一测多评法同步测定何首乌中4种蒽醌类成分的含量[J].中国中药杂志,2020,45(1):133.
• [12] 邰艳妮,翁艳鸿,张苏萍,等.一测多评法测定不同等级泽泻药材中7个萜类成分的含量[J].中国中药杂志,2019,44(11):2292.
• [13] 木盼盼,安琪,张彦昭,等.一测多评法测定葛根药材中9个异黄酮成分的含量[J].中国中药杂志,2019,44(22):4888.
• [14] 张影,许华客,李军山,等.基于一测多评法的茵陈标准汤剂中8种成分同时定量研究[J].药学学报,2019,54(9):1661.