色谱

色谱 ›› 2015, Vol. 33 ›› Issue (2): 152-157.DOI: 10.3724/SP.J.1123.2014.11006

• 研究论文 • 上一篇    下一篇

非水毛细管电泳法测定藤黄中藤黄酸的含量

欧婉露1, 李玉娟1, 石冬冬2, 屈锋1   

  1. 1. 北京理工大学生命学院, 北京 100081;
    2. 中国农业科学院饲料研究所, 北京 100081
  • 收稿日期:2014-11-05 修回日期:2014-12-18 出版日期:2015-02-08 发布日期:2015-01-24
  • 通讯作者: 屈锋
  • 基金资助:

    国家重点基础研究发展计划项目("973"项目)(2012CB910603);国家自然科学基金项目(21175011,21375008,81202996).

Determination of gambogic acid in Gamboge by non-aqueous capillary electrophoresis

OU Wanlu1, LI Yujuan1, SHI Dongdong2, QU Feng1   

  1. 1. School of Life Science, Beijing Institute of Technology, Beijing 100081, China;
    2. Feed Research Institute, Chinese Academy of Agricultural Sciences, Beijing 100081, China
  • Received:2014-11-05 Revised:2014-12-18 Online:2015-02-08 Published:2015-01-24

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160

被引次数

3

摘要：

藤黄酸(gambogic acid, GA)等环氧杂蒽酮类化合物的水溶性差,可通过非水毛细管电泳(non-aqueous capillary electrophoresis, NACE)分析。本文系统地考察了添加20%~60%(v/v)的甲醇或乙腈的运行电解质溶液对藤黄提取液中藤黄酸分离的影响。比较了不同的运行电解质溶液、运行电解质溶液浓度、pH、添加剂 β-环糊精的浓度、分离温度及分离电压的影响,建立了测定藤黄药材中藤黄酸含量的非水毛细管电泳方法。在40%乙腈、10 mmol/L β-环糊精、20 mmol/L四硼酸钠(pH 9.86)为运行电解质溶液、分离电压为10 kV、分离温度为30 ℃、检测波长为280 nm的条件下进行测定。结果表明,藤黄酸在2~2000 mg/L范围内线性关系良好,相关系数为0.9996,检出限(S/N=3)为2 mg/L。将本方法应用于越南、泰国、缅甸、印度4个产地的藤黄药材中藤黄酸的含量测定,测得含量为1.67~472.40 mg/g(相对标准偏差(RSD)为1.12%~2.60%),其中越南产藤黄中藤黄酸含量低,其他产地藤黄中藤黄酸的含量高。实际藤黄样品中藤黄酸的加标回收率为95.2%~105.6%。非水毛细管电泳方法简单、快速、重现性好,可用于藤黄药材中藤黄酸的含量测定。

关键词: 非水毛细管电泳, 藤黄, 藤黄酸

Abstract:

Gambogic acid (GA), a kind of caged xanthones, has low solubility in water. A non-aqueous capillary electrophoresis (NACE) was established for the determination of GA in Gamboge based on the optimized conditions. The effect of 20%-60% methanol or acetonitrile spiked in running solution was investigated. The effects of compositions, concentration, pH, additives like β-cyclodextrin in running buffer were thoroughly studied. Applied voltage and applied temperature were also observed. Optimal electrophoretic conditions were as follows: 20 mmol/L sodium borohydride solution (pH 9.86) containing 40% (v/v) acetonitrile, 10 mmol/L β-cyclodextrin as running buffer, applied voltage of 10 kV, capillary temperature of 30 ℃ and detection wavelength of 280 nm. The calibration curve had good linearity in the range of 2-2000 mg/L with the correlation coefficient of 0.9996. The limit of quantification (S/N=3) of the method was 2 mg/L. The quantifications of GA in Gamboge from different producing places including Vietnam, Thailand, Burma, India were 1.67-472.40 mg/g with the RSD (n=3) of 1.12%-2.60%. The content of Gamboge from Vietnam is obviously low while the others are high. The recoveries of GA spiked in real samples ranged from 95.2% to 105.6%. The method of NACE is simple, efficient and of good reproducibility, can be served as a novel reference to identify and control the quality of Gamboge.

Key words: Gamboge, gambogic acid, non-aqueous capillary electrophoresis (NACE)

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