基于超高效合相色谱对黄芪中5种主要黄酮类化合物的快速检测

引用本文: 王波, 周围, 刘小花, 柳小亚, 陈亚丽, 封士兰. 基于超高效合相色谱对黄芪中5种主要黄酮类化合物的快速检测[J]. 分析化学, 2016, 44(5): 731-739. doi: 10.11895/j.issn.0253-3820.150788 shu

Citation: WANG Bo, ZHOU Wei, LIU Xiao-Hua, LIU Xiao-Ya, CHEN Ya-Li, FENG Shi-Lan. Rapid Separation and Determination of 5 Kinds Flavonoids in Astragali Radix Based on Ultra-performance Convergence Chromatography[J]. Chinese Journal of Analytical Chemistry, 2016, 44(5): 731-739. doi: 10.11895/j.issn.0253-3820.150788 shu

基于超高效合相色谱对黄芪中5种主要黄酮类化合物的快速检测

王波 ^1,2, ,
周围 ^2, ,
刘小花 ^1, ,
柳小亚 ^1, ,
陈亚丽 ^1, ,
封士兰 ^1,

1.
兰州大学药学院, 兰州 730000;
2.
甘肃出入境检验检疫局综合技术中心, 兰州 730000
基金项目:
本文系国家"十二五"科技支撑计划课题项目(No.2011BAI05B02)资助

摘要: 建立了利用超高效合相色谱法(Ultra performance convergence chromatography,UPC²)快速分离和测定黄芪中5种主要黄酮类化合物(毛蕊异黄酮、毛蕊异黄酮苷、美的紫檀素、芒柄花苷、芒柄花素)的方法。黄芪样品采用80%乙醇提取后,以超临界CO₂-0.2% H₃PO₄-甲醇溶液为流动相,梯度洗脱,色谱柱为Waters ACQUITY UPC² CSH柱(100 mm×3.0 mm,1.8μm),柱温为40℃,流速为0.4 mL/min,进样量为1μL,检测波长为280 nm。整个分析过程仅需15 min,分析速度是传统液相色谱的3倍以上。结果表明:毛蕊异黄酮、毛蕊异黄酮苷、美的紫檀素、芒柄花苷与芒柄花素的检出限及定量限范围分别在0.3~0.5 mg/kg和1.0~2.0 mg/kg之间,5种黄酮类成分的加标平均回收率均高于99.7%,相对标准偏差(RSD)小于2.2%(n=6);在最优条件下,对13批不同产地的黄芪进行检测,毛蕊异黄酮、毛蕊异黄酮苷、美的紫檀素、芒柄花苷与芒柄花素的含量范围分别在4.8~102 mg/kg、14~277 mg/kg、0~135 mg/kg、5.3~119 mg/kg及2.8~41 mg/kg之间;本方法简便快速,重复性良好,结果准确可靠,可用于黄芪药材中5种主要黄酮类成分的含量测定。

关键词:

English

Rapid Separation and Determination of 5 Kinds Flavonoids in Astragali Radix Based on Ultra-performance Convergence Chromatography

1.
Department of Pharmacy, Lanzhou University, Lanzhou 730000, China;
2.
Central Laboratory of Technical Center of Gansu Entry-Exit Inspection and Quarantine Bureau, Lanzhou 730000, China
Received Date: 10 October 2015
Revised Date: 09 December 2015
Fund Project:
This work was supported by the Key Project in National Science and Technology Pillar Program during the Twelfth Five Year Great Research Projects of (NO. 2011BAI05B02) of the Ministry of Science and Technology of China.

Abstract: A method was developed for the rapid separation and determination of 5 kinds flavonoids (calycosin, calycosin-7-O-β-D-glucoside, ononin, medicarpin and formononetin) in Astragali Radix based on ultra-performance convergence chromatography. After extracting by 80% ethanol, the flavonoids were separated on a Waters Acquity UPC² CSH (100 mm×3.0 mm i.d., 1.8 μm) column at 40℃ by using supercritical CO₂-methanol (contain 0.2% H₃PO₄) acetonitrile as the mobile phase at a flow rate of 0.4 mL/min, and then analyzed by a UV detector at wavelength of 280 nm, the whole analysis progress was only 15 min. The results showed that the limits of detection (LOD) and the limits of quantitation (LOQ) of five flavonoids were between 0.3 and 0.5 mg/kg, and 1.0 and 2.0 mg/kg, respectively. The spiked recoveries were more than 99.7%, and the relative standard deviations (RSD) were less than 2.2% (n=6). Under the optimal conditions, 13 groups of Astragali Radix from different producing areas were detected. The contents of calycosin, calycosin-7-O-β-D-glucoside, medicarpin, ononin and formononetin were 4.8-102 mg/kg, 14-277 mg/kg, 0-135 mg/kg, and 5.3-119 mg/kg, 2.8-41 mg/kg, respectively. This method is simple, fast, accurate and reproducible, and the result is reliable. The method is applicable for the determination of 5 flavonoids in Astragali Radix.

Key words:

Ultra-performance convergence chromatography
/ Flavonoids
/ Astragali Radix

1. [1]
  ZHOU Wei, WANG Bo, LIUQian-Qian, YANG Sheng-Xin, WANG Li-Ting. Chinese J. Anal. Chem., 2015,43(1):115-120 周围, 王波, 刘倩倩, 杨盛鑫, 王丽婷.分析化学,2015,43(1):115-120
2. [2]
  WANG Bo, YAN Heng, WANG Su-Jun,LIU A-Jing, YANG Sheng-Xin, ZHOU Wei. Journal of Instrumental Analysis, 2015,34(7):824-828 王波, 闫衡, 王肃军, 刘阿静, 杨盛鑫, 周围.分析测试学报,2015,34(7):824-828
3. [3]
  XU Yong-Wei, SUN Qing-Long, HUANG Jing, TAN Xiao-Jie. Modern Instruments, 2012,18(5):45-48 徐永威, 孙庆龙, 黄静, 谭晓杰.现代仪器,2012,18(5):45-48
4. [4]
  Grand-Guillaume Perrenoud A, Veuthey J L, Guillarme D. J. Chromatogr. A, 2012,1266:158-167
5. [5]
  WANG Li-Ting, WANG Bo, ZHOU Wei, LIU Qian-Qian, YANG Sheng-Xin, ZHANG Ya-Heng. Chinese J. Anal. Chem., 2015,43(7):1047-1052 王丽婷, 王波, 周围, 刘倩倩, 杨盛鑫, 张雅珩.分析化学,2015,43(7):1047-1052
6. [6]
  National Pharmacopoeia Committee. Pharmacopoeia of the People's Republic of China (Part Ⅰ). Beijing:China Medical Science and Technology Press, 2010:284 国家药典委员会.中华人民共和国药典(一部). 北京:中国医药科技出版社, 2010:284
7. [7]
  HU Fang-Di, FENG Shi-Lan, ZHAO Jian-Xiong. Journal of Chinese Medicinal Materials, 2003,26(9):634 胡芳弟, 封士兰, 赵健雄.中药材,2003,26(9):634
8. [8]
  QIU Yong-Bo, LIU Jin, WU Fei. Chinese Journal of Convalescent Medicine, 2011,5:435-436 邱勇波, 刘锦, 武飞.中国疗养医学,2011,5:435-436
9. [9]
  CHEN Jian-Zhen, LV Gui-Yuan, YE Lei, CHEN Jian-Ming. Herald of Medicine, 2009,28(10):1314-1316 陈建真, 吕圭源, 叶磊, 陈建明.医药导报, 2009,28(10):1314-1316
10. [10]
  LIANG Jin, FENG Shi-Lan, LIU Xiao-Hua, DANG Zi-Long, LIANG Jian-Di, YANG Chun-Xia. Northwest Pharmaceutical Journal, 2012,27(5):490-493 梁瑾, 封士兰, 刘小花, 党子龙, 梁建娣, 杨春霞.西北药学杂志, 2012,27(5):490-493
11. [11]
  LUO Chun-Xia, LIN Ping-Chuan, GU Li-Hua, WU Tao, WU Da-Zheng, WANG Zheng-Tao, HU Zhi-Bi. China Journal of Chinese Materia Medica, 2003,28(7):603-605 罗春霞, 林平川, 谷丽华, 吴弢, 吴大正, 王峥涛, 胡之璧.中国中药杂志,2003,28(7):603-605
12. [12]
  WANG Xiao-Hui, LIU Tao, LI Qing, CHEN Xiao-Hui, BI Kai-Shun. Chinese Journal of Chromatography, 2006, 24(6):486-488 王晓辉, 刘涛, 李清, 陈晓辉, 毕开顺.色谱,2006, 24(6):486-488
13. [13]
  LIU Xiao-Qing, LI Jun, HU Jing-Lian, LI Xiao-Yan, MEN Qi-Ming, KANG Ting-Guo. Journal of Liaoning University of Traditional Chinese Medicine, 2013,15(07):53-55 刘晓庆, 李军, 胡景莲, 李晓艳, 门启鸣, 康廷国.辽宁中医药大学学报,. 2013,15(07):53-55
14. [14]
  LIANG Cong-Qing, ZHOU Xuan, SONG Fen-Yun, ZHONG Zhao-Jian. Chinese Journal of Experimental Traditional Medical Formulae, 2004,10(5):9-11 梁从庆, 周漩, 宋粉云, 钟兆健.中国实验方剂学杂志,2004,10(5):9-11
15. [15]
  LIANG Xu-Ming, TANG Yao-Shu, ZHANG Xiao-Mei. LiShiZhen Medicine and Materia Medica Research, 2007,18(1):22-25 梁旭明, 唐耀书, 张小梅.时珍国医国药,2007,18(1):22-25
16. [16]
  WU Ding-Hui, CHEN Guan-Jian. Journal of Practical Traditional Chinese Medicine, 2012,28(1):65-67 吴定慧, 陈关键.实用中医药杂志, 2012,28(1):65-67
17. [17]
  ZHANG Jia-Yu, QIAO Yan-Jiang, ZHANG Qian, GAO Xiao-Yan, LU Jian-Qiu. Chinese Journal of Pharmaceutical Analysis, 2013,27(2):349-354 张加余, 乔延江, 张倩, 高晓燕, 卢建秋.药物分析杂志,2013,27(2):349-354
18. [18]
  TANG Gui-Bao, CHEN Nan, PAN Xin. Strait Pharmaceutical Journal, 2013,23(12):7-11 唐瑰宝, 陈楠, 潘馨.海峡药学, 2013,23(12):7-11
19. [19]
  CHEN Ting, TIAN Feng, TANG Yue-Nian, LIU Yan, LIN Zhi-Yan, WANG Ye-Chen. China Pharmacist, 2014,17(4):593-596 陈婷, 田丰, 唐跃年, 刘艳, 林志燕, 王晔尘.中国药师, 2014,17(4):593-596

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基于超高效合相色谱对黄芪中5种主要黄酮类化合物的快速检测

English

Rapid Separation and Determination of 5 Kinds Flavonoids in Astragali Radix Based on Ultra-performance Convergence Chromatography

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基于超高效合相色谱对黄芪中5种主要黄酮类化合物的快速检测

English

Rapid Separation and Determination of 5 Kinds Flavonoids in Astragali Radix Based on Ultra-performance Convergence Chromatography

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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