色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-二极管阵列检测-电化学检测联用技术同时测定三精双黄连口服液中的4种化合物

刘琳 秦海燕 郑建斌   

  1. Institute of Analytical Science, Shaanxi Provincial Key Laboratory of Electroanalytical Chemistry, Northwest University, Xi’an 710069, China
  • 收稿日期:2005-07-01 修回日期:2006-03-20 出版日期:2006-05-30 发布日期:1987-03-25
  • 通讯作者: 郑建斌

Simultaneous Determination of Four Compounds in Sanjing Shuang-huanglian Oral Liquid by High Performance Liquid Chroma-

LIU Lin, SUO Zhirong, ZHENG Jianbin   

  1. Institute of Analytical Science, Shaanxi Provincial Key Laboratory of Electroanalytical Chemistry, Northwest University, Xi’an 710069, China
  • Received:2005-07-01 Revised:2006-03-20 Online:2006-05-30 Published:1987-03-25
  • Contact: Zheng Jianbin

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624

被引次数

35

摘要： 建立了应用高效液相色谱-二极管阵列检测-电化学检测(HPLC-DAD-ECD)联用技术同时测定三精双黄连口服液中的绿原酸、咖啡酸、黄芩甙和木樨草素的方法。以Zorbax SB-C18柱(150 mm×4.6 mm i.d., 5.0 μm)为色谱柱,柱温为30 ℃，流动相为(A)甲醇和(B)甲醇-水-冰醋酸(体积比为50∶50∶1),其梯度洗脱程序为2%A3 min3%A12 min25%A5 min80%A。流速为0.8 mL/min。二极管阵列检测波长为275 nm。电化学单安培检测器的工作电压为0.7 V。在上述条件下实现了绿原酸、咖啡酸、黄芩甙和木樨草素的分离检测。上述4种化合物的回收率为96.6%～99.6%,相对标准偏差(RSD)为2.5%～4.1%,检测限依次为1,0.2,9和7 mg/L。该方法简便、快速,重现性和准确度较好,可作为测定双黄连口服液中绿原酸、咖啡酸、黄芩甙和木樨草素的有效方法。

关键词: 电化学检测, 二极管阵列检测, 高效液相色谱法, 黄芩甙, 咖啡酸, 绿原酸, 木樨草素, 三精双黄连口服液

Abstract: Chlorogenic acid, caffeic acid, baicalin and luteolin in Sanjing Shuanghuanglian Oral Liquid were simultaneously detected and identified using a high performance liquid chromatography coupled with diode array detection and electrochemical detection (HPLC-DAD-ECD). The separation was performed on a Zorbax SB-C18 column (150 mm×4.6 mm i.d., 5.0 μm). The mobile phase consisted of (A) methanol and (B) methanol-water-acetic acid (50∶50∶1, v/v/v) using a linear gradient elution of 2%A-3%A at 0-3 min, 3%A-25%A at 3-15 min, 25%A-80%A at 15-20 min. The flow rate was 0.8 mL/min. The DAD detection was used at 275 nm. The ECD detection was done at 0.7 V. The column thermostat set at 30 ℃. The limits of detection of the 4 compounds were 1 mg/L for chlorogenic acid, 0.2 mg/L for caffeic acid, 9 mg/L for baicalin, 7 mg/L for luteolin. The average recoveries were between 96.6%-99.6% with relative standard deviations (RSDs) of 2.5%-4.1%. The method is simple, rapid, reproducible and accurate. It can be used for the routine analysis of the four compounds in Shuanghuanglian Oral Liquid.

Key words: baicalin, caffeic acid, chlorogenic acid, diode array detection (DAD), electrochemical detection (ECD), luteolin, Sanjing Shuanghuanglian Oral Liquid , high performance liquid chromatography (HPLC)