UPLC-ELSD同时测定贝母类药材中6种生物碱的含量Simultaneous determination of six major isosteroidal alkaloids in Beimu by UPLC-ELSD
车朋;刘久石;齐耀东;强亭燕;宋奕辰;魏雪苹;刘海涛;张本刚;
CHE Peng;LIU Jiu-shi;QI Yao-dong;QIANG Ting-yan;SONG Yi-chen;WEI Xue-ping;LIU Hai-tao;ZHANG Ben-gang;Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences and Peking Union Medical College;
摘要(Abstract):
建立UPLC-ELSD方法同时测定5种贝母类药材中贝母辛、西贝母碱苷、西贝母碱、贝母素乙、贝母素甲和湖贝甲素6种生物碱成分。采用Waters Acquity UPLC(TM) CSH C_(18)柱(2.1 mm×100 mm,1.7μm);0.02%二乙胺水溶液和甲醇为流动相,梯度洗脱(0~2 min,45%A;2~5 min,45%~25%A;5~7 min,25%A;7~17 min,25%~10%A;17~20 min,10%A),流速0.3 mL·min(TM) CSH C_(18)柱(2.1 mm×100 mm,1.7μm);0.02%二乙胺水溶液和甲醇为流动相,梯度洗脱(0~2 min,45%A;2~5 min,45%~25%A;5~7 min,25%A;7~17 min,25%~10%A;17~20 min,10%A),流速0.3 mL·min(-1),柱温35℃,样品室温度20℃,漂移管温度45℃,喷雾器参数40%,进样量为1μL,同时测定贝母类药材中6种生物碱活性成分;并采用聚类分析(HCA)和主成分分析(PCA)对不同种类贝母类药材的质量进行评价。该方法操作简单,结果准确,稳定可靠,能快速分析5种贝母类药材中6种生物碱的含量,为贝母类药材的质量控制提供了依据。
An UPLC method was established for the direct determination of six major bioactive isosteroidal alkaloids, namely peimisine, imperialine, sipeimine-3-D-glucoside, verticinone, verticine and hupehenine from the bulbus of Fritillaria(Beimu), a commonly used antitussive traditional Chinese medicinal(TCM) herb. An Acquity UPLC(-1),柱温35℃,样品室温度20℃,漂移管温度45℃,喷雾器参数40%,进样量为1μL,同时测定贝母类药材中6种生物碱活性成分;并采用聚类分析(HCA)和主成分分析(PCA)对不同种类贝母类药材的质量进行评价。该方法操作简单,结果准确,稳定可靠,能快速分析5种贝母类药材中6种生物碱的含量,为贝母类药材的质量控制提供了依据。
An UPLC method was established for the direct determination of six major bioactive isosteroidal alkaloids, namely peimisine, imperialine, sipeimine-3-D-glucoside, verticinone, verticine and hupehenine from the bulbus of Fritillaria(Beimu), a commonly used antitussive traditional Chinese medicinal(TCM) herb. An Acquity UPLC(TM) CSH C_(18) column(2.1 mm×100 mm, 1.7 μm) was used for all analysis. The investigated six compounds were all separated with gradient mobile phase consisting of 0.02% diethylamine-water-methanol at a flow rate of 0.3 mL·min(TM) CSH C_(18) column(2.1 mm×100 mm, 1.7 μm) was used for all analysis. The investigated six compounds were all separated with gradient mobile phase consisting of 0.02% diethylamine-water-methanol at a flow rate of 0.3 mL·min(-1). The temperature of sample manager was set at 20 ℃. Drift tube temperature was 45 ℃, and spray parameter was 40% with injection volume of 1 μL. Then, the further quality assessment of Beimu was carried out by cluster analysis(CA) and principal component analysis(PCA). The investigated all had good linearity(r≥0.998 9) over the tested ranges. The method is simple, accurate and reproducible, and can be used for determining the content of six major bioactive isosteroidal alkaloids.
关键词(KeyWords):
贝母;UPLC-ELSD;生物碱;含量测定;统计分析
Beimu;UPLC-ELSD;alkaloids;quantitative analysis;statistical analysis
基金项目(Foundation): 国家自然科学基金项目(81573531);; 中国医学科学院与健康科技创新工程项目(2016-IZM-2-003);; 常用道地药材及其产区的特征、标准及数字化(2015FY1115000)
作者(Authors):
车朋;刘久石;齐耀东;强亭燕;宋奕辰;魏雪苹;刘海涛;张本刚;
CHE Peng;LIU Jiu-shi;QI Yao-dong;QIANG Ting-yan;SONG Yi-chen;WEI Xue-ping;LIU Hai-tao;ZHANG Ben-gang;Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences and Peking Union Medical College;
DOI: 10.19540/j.cnki.cjcmm.20191223.201
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- 车朋
- 刘久石
- 齐耀东
- 强亭燕
- 宋奕辰
- 魏雪苹
- 刘海涛
- 张本刚
CHE Peng- LIU Jiu-shi
- QI Yao-dong
- QIANG Ting-yan
- SONG Yi-chen
- WEI Xue-ping
- LIU Hai-tao
- ZHANG Ben-gang
- Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine
- Ministry of Education
- Institute of Medicinal Plant Development
- Chinese Academy of Medical Sciences and Peking Union Medical College
- 车朋
- 刘久石
- 齐耀东
- 强亭燕
- 宋奕辰
- 魏雪苹
- 刘海涛
- 张本刚
CHE Peng- LIU Jiu-shi
- QI Yao-dong
- QIANG Ting-yan
- SONG Yi-chen
- WEI Xue-ping
- LIU Hai-tao
- ZHANG Ben-gang
- Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine
- Ministry of Education
- Institute of Medicinal Plant Development
- Chinese Academy of Medical Sciences and Peking Union Medical College