色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 79-82.DOI: 10.3724/SP.J.1123.2012.08038

• 技术与应用 • 上一篇    下一篇

高效液相色谱法定量测定中药千层塔提取物中的石杉碱甲

张敬彩1, 魏杰2, 钟虹敏1, 郭志谋2*, 张华1*   

  1. 1. 大连理工大学化学学院, 辽宁 大连 116023; 2. 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2012-08-23 修回日期:2012-09-26 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者: 郭志谋
  • 基金资助:

    国家杰出青年基金项目(20825518);国家自然科学基金项目(21005077).

Determination of Huperzine A in the extract of Huperzia serrata by high performance liquid chromatography

ZHANG Jingcai1, WEI Jie2, ZHONG Hongmin1, GUO Zhimou2*, ZHANG Hua1*   

  1. 1. College of Chemistry, Dalian University of Technology, Dalian 116023, China； 2. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2012-08-23 Revised:2012-09-26 Online:2013-01-28 Published:2013-01-21

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280

被引次数

21

摘要： 建立了高效液相色谱快速定量测定中药千层塔提取物中石杉碱甲含量的分析方法。千层塔提取物经甲醇/水/甲酸(10/90/0.2, v/v/v)提取并定容后,过滤膜后直接分析。色谱分离选用XCharge C18色谱柱(150 mm×4.6 mm, 5 μm),以水(含0.1%三氟乙酸)和乙腈(含0.09%三氟乙酸)为流动相进行梯度洗脱,流速为2 mL/min,于310 nm波长下检测,可在10 min内完成石杉碱甲的快速分离分析。结果表明,石杉碱甲在2.12～106 mg/L范围内线性关系良好(相关系数为0.9999);平均加标回收率为102.34%,相对标准偏差(RSD)为0.46%;日内及日间精密度均小于2%,满足定量要求。该方法简便、快速,结果可靠,重现性好,可作为千层塔提取物质量评价的依据。

关键词: 高效液相色谱法, 千层塔, 生物碱, 石杉碱甲, 中草药

Abstract: A high performance liquid chromatographic (HPLC) method was established to determine the Huperzine A in the extract of Huperzia serrata. After extracted by methanol/water/formic acid (10/90/0.2, v/v/v), the sample was filtered for HPLC analysis. The separation was performed on an XCharge C18 column (150 mm×4.6 mm, 5 μm) by gradient elution with water (containing 0.1% （v/v） trifluoroacetic acid) and acetonitrile (containing 0.09%（v/v） trifluoroacetic acid) as the mobile phases. Rapid separation was achieved within 10 min at a flow rate of 2 mL/min with ultraviolet absorption detection at a wavelength of 310 nm. Under the optimized conditions, good linearity was obtained in the range of 2.12-106 mg/L with the correlation coefficient (R2) of about 0.9999. The average recovery was 102.34% with the relative standard deviation (RSD) of 0.46%. The intraday and interday precisions were all below 2%. The results demonstrate that this method is simple, rapid and accurate with good reproducibility, and can be used to evaluate the quality of Huperzia serrata.

Key words: alkaloid, Chinese medicinal herb, Huperzia serrata, Huperzine A, high performance liquid chromatography (HPLC)