高效液相色谱法同时测定三黄片中黄芩苷、小檗碱和大黄酸的含量

高效液相色谱法同时测定三黄片中黄芩苷、小檗碱和大黄酸的含量

李奕, 高建平, 许旭^*

1.中国科学院上海有机化学研究所金属化学国家重点实验室分析测试中心, 上海 200032;
2.上海中医药大学中药学院, 上海 201203

收稿日期:2005-02-02 修回日期:2005-05-10 出版日期:2005-06-15 发布日期:2005-06-15
通讯作者: 许旭*

Simultaneous Determination of Baicalin, Berberine and Rhein by HPLC in Traditional Chinese Patent Medicine Sanhuang Tablets

LI Yi, GAO Jian-Ping, XU Xu^*

1.Laboratory of Analytical Chemistry, State Key Laboratory of Organometallic Chemistry, Shanghai Institute of Organic Chemistry, CAS, Shanghai 200032, China; Graduate School of Chinese Academy of Sciences, Beijing 100039, China;
2.School of Pharmacy, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China

Received:2005-02-02 Revised:2005-05-10 Online:2005-06-15 Published:2005-06-15
Contact: XU Xu*

摘要/Abstract

摘要： 目的建立一种反相液相色谱法用于三黄片中黄芩苷、小檗碱和大黄酸含量的同时测定。方法采用Kromasil C18色谱柱, 以0.02 mol·L^-1 H3PO4(三乙胺调节pH = 6.78)乙腈甲醇(40:9:7)为流动相, 检测波长254 nm, 流速1.0 mL·min^-1。考虑到酸性化合物和碱性化合物之间可能的相互作用, 进行回收率实验时三个标准品被分别加入样品溶液中, 并且将体积扩大了一倍。结果三个化合物的峰面积与浓度之间都呈现很好的线性关系, 线性相关系数均超过0.9998。各成分的平均回收率分别为黄芩苷96.1%(RSD = 2.1%)、小檗碱98.5%(RSD = 2.5%)、大黄酸101.5%(RSD = 1.3%)。结论该方法可用于三黄片质量的全面评价。

关键词: 三黄片, 三黄片, 三黄片, 黄芩苷, 黄芩苷, 黄芩苷, 大黄酸, 大黄酸, 大黄酸, 小檗碱, 小檗碱, 小檗碱, 高效液相色谱法, 高效液相色谱法, 高效液相色谱法

Abstract: Aim To establish a reversed phase liquid chromatographic method for simultaneous determination of three main medicinal constituents, baicalin, berberine and rhein, in Sanhuang tablets. Methods The separation was performed on a Kromasil C18 column with TEA-adjusted 0.02 mol·L^-1 H3PO4 (pH 6.78)-acetonitrile-methanol (40:9:7) as mobile phase at a flow-rate of 1.0 mL·min^-1, with detection at 254 nm. Considering interaction between acidic and alkaline compounds, three standard markers were added respectively and the volume of sample solution was doubled in recovery experiments. Results Three regression equations revealed excellent linear relationship between the peak areas and concentrations and the correlation coefficients all surpassed 0.999 8. The average recovery was 96.1% (RSD = 2.1%) baicalin, 98.5% (RSD = 2.4%) for berberine, and 101.5% (RSD = 1.3%) for rhein. Conclusion The method developed can be used to control the quality of Sanhuang tablets comprehensively.

Key words: Sanhuang tablets, Sanhuang tablets, baicalin, baicalin, rhein, rhein, berberine, berberine, HPLC, HPLC

中图分类号:

R917.01

R927.2

Supporting: Foundation item: Innovation Fund of Chinese Academy of Sciences (KGCX2-SW-213-05).
^*Corresponding author. Tel.: 86-21-54925320

李奕, 高建平, 许旭^*. 高效液相色谱法同时测定三黄片中黄芩苷、小檗碱和大黄酸的含量[J]. .

LI Yi, GAO Jian-Ping, XU Xu^*. Simultaneous Determination of Baicalin, Berberine and Rhein by HPLC in Traditional Chinese Patent Medicine Sanhuang Tablets[J]. .

参考文献

[1] Meng XS. Analysis of Chinese Patent Medicinse [M]. 2nd ed. Beijing : People’s Medical Publishing House, 1998. 5.
[2] Lin SJ, Tseng HH, Wen KC, et al. Determination of gentiopicroside, mangiferin, palmatine, berberine, baicalin, wogonin and glycyrrhizin in the traditional Chinese medicinal preparation Sann-Joong-Kuey-Jian-Tang by high-performance liquid chromatography [J]. J Chromatogr A, 1996, 730 : 17-23.
[3] Lee YC, Huang CY, Wen KC, et al. Determination of liquiritin, glycyrrhizin, hesperidin, cinnamic acid, cinnamaldehyde, honokiol and magnolol in the traditional Chinese medicinal preparation Wuu-Ji-San by high-performance liquid chromatography [J]. J Chromatogr A, 1995, 692 : 137-145.
[4] State Pharmacopoeia Committee of the People’s Republic of China. Pharmacopoeia of the People’s Republic of China [S]. 2000 ed, Part I. Beijing : Chemical Industry Press. 2000, 164-165.
[5] Li SY, Guo ZJ, Wang L. Determination of emodin, chrysophanol and baicalin in Sanhuang tablets by HPLC [J]. Chin Tradit Pat Med, 2001, 23 (6) : 445-448.
[6] Duan ZH, Dong LF, Zhang WJ, et al. HPLC determination of berberine hydrochloride in Sanhuang tablets [J]. J Yunnan Coll Tradit Chin Med, 2003, 26 (4) : 17-19.
[7] Chen NG, Huang XS. Determination of emodin, chrysophanol in Sanhuang tablets by HPLC [J]. China Pharm, 1999, 8 (8) : 33.
[8] Wu HJ. Determination of the content of baicalin in Sanhuang tablets by HPLC [J]. Strait Pharm J, 2003, 15 (2) : 34-36.
[9] Li XY. Assay of berberine hydrochloride in Sanhuang tablets by HPLC [J]. Chin Tradit Pat Med, 2002, 24 (9) : 679-680.
[10] Yu BT, Zhang ZR, Liu WS, et al. Studies on stability of baicalin [J]. Chin Tradit Herb Drugs, 2002, 33 (3) : 218-220.
[11] Li Y, Xu X. Study on precipitation reaction between baicalin and berberine by HPLC [J]. J Chromatogr B, 2004, 810 : 165-168.
[12] Xu X, Dong XW, Mao P. Study on the precipitation reaction between berberine and rheinic acid by capillary electrophoresis [J]. Acta Pharm Sin, 2003, 38 (10) : 779-782.
[13] Majors RE. The cleaning and regeneration of reversed-phase HPLC columns [J]. LC-GC Asia Pacific, 2003, 6 (1) : 8-12.

[1]	杨杰, 景彩芳, 李少创, 刘思彤, 李董明, 李钦青, 贺文彬. 复方党参颗粒制备工艺优化及4种成分的同时测定[J]. 中国药学(英文版), 2023, 32(8): 665-676.
[2]	李莹, 文周, 刘永玲, 赵治兵, 王磊, 程泽能. 高效液相色谱法测定大鼠血浆中阿昔洛韦浓度及其与吉非替尼药物相互作用的研究[J]. 中国药学(英文版), 2021, 30(6): 495-504.
[3]	余飞, 周文莉, 阚家义, 彭灿. 11种盐酸小檗碱片剂在不同溶出度介质中溶出度曲线特征的比较[J]. 中国药学(英文版), 2020, 29(2): 102-112.
[4]	蒋雯, 孙超, 王珏, 辛倩, 李开霖, 亓同钢, 栾云. 黄芩苷通过抑制血管重构对实验性肺动脉高压的治疗作用研究[J]. 中国药学(英文版), 2020, 29(10): 719-728.
[5]	侯海涛, 宋子冰, 丁婕琴, 位灯国, 胡胜, 翟倩倩, 岳霞丽. 小檗碱通过靶向端粒G-四链体增强舒尼替尼的活性[J]. 中国药学(英文版), 2019, 28(5): 289-297.
[6]	庞雨浓, 梁英文, 王玉刚, 雷帆, 袁梽漪, 邢东明, 李俊, 杜力军. 小檗碱通过调节PPARγ启动子甲基化对缺血再灌注脑损伤的作用[J]. 中国药学(英文版), 2018, 27(3): 170-182.
[7]	王环鑫, 孙亚欣, 徐善森, 路童, 陈亚南, 肇丽梅. 高效液相色谱法测定人血浆中游离拉莫三嗪的血药浓度[J]. 中国药学(英文版), 2018, 27(12): 832-839.
[8]	卢希, 袁梽漪, 姜敬非, 雷帆, 冯天师, 王玉刚, 王欣佩, 邢东明, 李俊, 杜力军. 通过调控NFE2响应元件增强低温时Ucp1基因的表达: 小檗碱作用于棕色脂肪组织产热的新机制[J]. 中国药学(英文版), 2017, 26(4): 237-254.
[9]	费文波, 梁晓霞, 何敏. 不同藏医炮制方法对诃子中诃子酸含量的影响[J]. 中国药学(英文版), 2017, 26(3): 230-234.
[10]	袁梽漪, 卢希, 雷帆, 胡珺, 王玉刚, 柴玉爽, 姜敬非, 李慧玉, 邢东明, 杜力军. 通过促进poly A 和PABP蛋白结合抑制mRNA降解: 小檗碱作用的新机制[J]. 中国药学(英文版), 2017, 26(1): 53-62.
[11]	俞璐, 姚国栋, 马卫成. 大黄酸: 一种新型潜在抗肿瘤药物[J]. 中国药学(英文版), 2016, 25(5): 321-328.
[12]	陈伟, 袁琴, 程军平, 葛惠男, 江国荣, 陈蓉. 曲面响应法优化超声辅助提取升麻中酚性物质的研究[J]. 中国药学(英文版), 2016, 25(5): 373-379.
[13]	刘嵩, 吕晓慧, 孙宗喜, 苏瑞强. 黄芩苷抗氧化活性及对四氯化碳致大鼠肝损伤的保护作用[J]. 中国药学(英文版), 2015, 24(8): 538-544.
[14]	薛清丹, 王鹏, 康宇红, 李秋红. 高效液相色谱法同时测定大鼠血浆中人参皂苷Rg1, Re, Rb1及其在参麦注射液药动学研究中的应用[J]. 中国药学(英文版), 2015, 24(7): 475-481.
[15]	陈中芬, 刘文, 陈大业, 施晓伟, 王群. 戊己胃漂浮缓释片HPLC指纹图谱定性及定量分析[J]. 中国药学(英文版), 2015, 24(5): 310-317.