高等学校化学学报

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高效液相色谱电生Mn(Ⅲ)化学发光法检测人体血清和尿样中的卡托普利

张琰图1,2, 章竹君1, 孙永华1, 魏月1   

    1. 陕西师范大学化学与材料科学学院, 西安 710062;
    2. 延安大学化学与化工学院, 延安 716000
  • 收稿日期:2006-07-06 修回日期:1900-01-01 出版日期:2007-05-10 发布日期:2007-05-10
  • 通讯作者: 章竹君

Determination of Captopril in Human Serum and Urine Samples by HPLC with On-line Electrogenerated Mn(Ⅲ) Chemiluminescence Detection

ZHANG Yan-Tu1,2, ZHANG Zhu-Jun1*, SUN Yong-Hua1, WEI Yue1   

    1. School of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, China;
    2. School of Chemistry and Chemical Engineering, Yan'an University, Yan'an 716000, China
  • Received:2006-07-06 Revised:1900-01-01 Online:2007-05-10 Published:2007-05-10
  • Contact: ZHANG Zhu-Jun

摘要: 设计了一个HPLC在线电生Mn(Ⅲ)化学发光检测器, 实现在线电化学反应, 从而产生反应活性很高的初生态氧化剂Mn(Ⅲ), 并与色谱柱后CP混合产生化学发光. 同时还能够根据需要调节电极反应和发光反应两者的介质, 满足柱后发光反应的最佳环境. 在优化流动相和化学发光检测条件的基础上, 将该检测器应用于人体血清和尿液中CP的测定.

关键词: 高效液相色谱, 化学发光检测器, 在线电生Mn(Ⅲ), 卡托普利, 人体血清, 尿样

Abstract: The separation and determination of captopril in human serum and urine samples by means of high performance liquid chromatography(HPLC) with on-line electrogenerated Mn(Ⅲ) chemiluminescence detection was carried out. The method was based on the direct chemiluminescence reaction between captopril and Mn(Ⅲ), which was on-line electrogenerated by constant current electrolysis. The chromatographic separation was performed on a nucleosil RP-C18(250 mm×4.6mm i.d., 5 μm) column with an isocratic mobile phase consisting of acetonitrile-1% aqueous acetic acid(volume ratio 6∶4) at a flow-rate of 1.2 mL/min. The temperature was 25 ℃. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. Under the optimal conditions, the linear range and detection limit for captopril are 5—800 ng/mL and 0.9 ng/mL, respectively. The relative standard derivation for 10.0 ng/mL captopril is 2.2%(n=11). The average recoveries for captopril in human serum and urine samples ranged from 94.8% to 103.2%, and the relative standard deviations of the quantitative results are below 3.4%. The proposed method had been applied to the determination of captopril in human serum and urine samples.

Key words: High performance liquid chromatography, Chemiluminescence detector, On-line electrogenerated Mn(Ⅲ), Human serum, Urine sample

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