色谱

色谱

• 研究简报 • 上一篇    下一篇

复方丹参片中四种成分的高效液相色谱-电化学检测-紫外检测法分析

索志荣1,秦海燕2,曹炜1,刘文哲2,郑建斌1

  

  1. 1. Shaanxi Provincial Key Lab of Electro-Analytical Chemistry, Institute of Analytical Science, Northwest University, Xi’an 710069, China; 2. College of Life Science, Northwest University, Xi’an 710069, China

  • 收稿日期:2004-10-10 修回日期:1900-01-01 出版日期:2005-11-30 发布日期:1987-12-25
  • 通讯作者: 郑建斌

Analysis of Four Components in Fufang Danshen Tablets by High Performance Liquid Chromatography with Electrochemical and Ultraviolet Detections

SUO Zhirong1, QIN Haiyan2, CAO Wei1, LIU Wenzhe2, ZHENG Jianbin1   

  1. 1. Shaanxi Provincial Key Lab of Electro-Analytical Chemistry, Institute of Analytical Science, Northwest University, Xi’an 710069, China; 2. College of Life Science, Northwest University, Xi’an 710069, China

  • Received:2004-10-10 Revised:1900-01-01 Online:2005-11-30 Published:1987-12-25

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摘要：

建立了电化学检测器与二极管阵列检测器联用的液相色谱(HPLC-ECD-DAD)同时分离和测定复方丹参片中原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA 等4种成分的分析方法。采用Zorbax SB-C18柱(150 mm×4.6 mm i.d.,5.0 μm),以甲醇和0.4%磷酸为流动相(流速1.0 mL/min)进行梯度洗脱;ECD检测电压0.7 V,DAD检测波长270 nm,柱温30 ℃。实验结果表明,原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA质量浓度分别为0.3～9.0 mg/L,1.1～54.0 mg/L,1.1～11.1 mg/L和5.2～52.0 mg/L时与其峰面积呈良好的线性关系(线性相关系数均高于0.999),原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA的平均回收率(n=6)分别为97.8%(相对标准偏差(RSD)为2.15%),98.2%(RSD为2.07%),97.6%(RSD为2.18%)和97.2%(RSD为2.07%)。该法同时利用了ECD和DAD的优点,是一种快速、灵敏、准确的分析方法,可以为复方丹参片的质量控制提供科学依据。

关键词: 丹参酮ⅡA, 复方丹参片 , 高效液相色谱-电化学检测-紫外检测法, 咖啡酸, 原儿茶醛, 原儿茶酸

Abstract:

A rapid and accurate method for the simultaneous separation and determination of protocatechuic acid, protocatechuic aldehyde, caffeic acid and tanshinone ⅡA in Fufang Danshen Tablets by high performance liquid chromatography has been established. The former three constituents were detected by electrochemical array detector (ECD) and the last one by ultraviolet diode array detector (DAD). The separation was performed on a Zorbax SB-C18 column (150 mm×4.6 mm i.d., 5.0 μm) by gradient elution with methanol and 0.4% aqueous phosphoric acid as mobile phase at a flow rate of 1.0 mL/min. The detections were done at 0.7 V, 270 nm and 30 ℃. The results showed that the linear ranges were 0.3-9.0 mg/L for protocatechuic acid, 1.1-54.0 mg/L for protocatechuic aldehyde, 1.1-11.1 mg/L for caffeic acid and 5.2-52.0 mg/L for tanshinone ⅡA. The average recoveries (n= 6) were 97.8% with relative standard deviation (RSD) of 2.15% for protocatechuic acid, 98.2% with RSD of 2.07% for protocatechuic aldehyde, 97.6% with RSD of 2.18% for caffeic acid and 97.2% with RSD of 2.07% for tanshinone ⅡA. These four components were separated successfully from each other. The sensitivities of detection of protocatechuic acid, protocatechuic aldehyde and caffeic acid with ECD were 11.0-25.3 times greater than those with DAD. The study provides a scientific basis for the quality control of Fufang Danshen Tablets.

Key words: tanshinone ⅡA, caffeic acid, Fufang Danshen Tablets , protocatechuic acid, protocatechuic aldehyde, high performance liquid chromatography-electrochemical and ultraviolet detections