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采用带脉冲安培检测的反相色谱法及膜反应器测定血清中的环糊精。

Determination of cyclodextrins in serum by reversed-phase chromatography with pulsed amperometric detection and a membrane reactor.

作者信息

Haginaka J, Nishimura Y, Yasuda H

机构信息

Faculty of Pharmaceutical Sciences, Mukogawa Women's University, Hyogo, Japan.

出版信息

J Pharm Biomed Anal. 1993 Oct;11(10):1023-6. doi: 10.1016/0731-7085(93)80064-8.

DOI:10.1016/0731-7085(93)80064-8
PMID:8305583
Abstract

A high-performance liquid chromatographic method has been developed for the determination of cyclodextrins (CDs) in serum. The method involves solid-phase extraction of CDs, separation on a C18 reversed-phase column using a mixture of water, tetrahydrofuran and methanol as an eluent, eluent pH modification with a cation-exchange membrane reactor surrounded by 1.5 M sodium hydroxide solutions, and pulsed amperometric detection (PAD) with a gold working electrode. The solid-phase extraction on a C18 bonded-silica column was effective for removing the PAD sensitive components in serum. The calibration graphs constructed by internal standard method were linear over the range 6.25-200 pmol of CDs in serum. The detection limits for CDs were about 5 pmol at a signal-to-noise ratio of 3.

摘要

已开发出一种高效液相色谱法用于测定血清中的环糊精(CDs)。该方法包括环糊精的固相萃取,使用水、四氢呋喃和甲醇的混合物作为洗脱剂在C18反相柱上进行分离,通过被1.5 M氢氧化钠溶液包围的阳离子交换膜反应器对洗脱剂pH进行调节,以及使用金工作电极进行脉冲安培检测(PAD)。在C18键合硅胶柱上的固相萃取有效地去除了血清中对PAD敏感的成分。通过内标法构建的校准曲线在血清中环糊精含量为6.25 - 200 pmol范围内呈线性。环糊精的检测限在信噪比为3时约为5 pmol。

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