采用脉冲安培检测和膜反应器的反相色谱法测定环糊精和支链环糊精。

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

作者信息

Haginaka J, Nishimura Y, Wakai J, Yasuda H, Koizumi K, Nomura T

机构信息

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

出版信息

Anal Biochem. 1989 Jun;179(2):336-40. doi: 10.1016/0003-2697(89)90139-5.

DOI:10.1016/0003-2697(89)90139-5

PMID:2774181

Abstract

A high-performance liquid chromatographic method has been developed for the determination of cyclodextrins (CDs) and branched CDs. The method involves their separation on a reversed-phase column using a mixture of water and acetonitrile as an eluant, eluant pH modification with a cation-exchange membrane reactor surrounded by 1.5 M sodium hydroxide solutions, and pulsed amperometric detection with a gold working electrode. The calibration graphs constructed by peak height versus injected amount were linear over the ranges 50-1000 pmol. The detection limits for CDs and branched CDs were about 1-5 pmol at a signal-to-noise ratio of 3. The method was successfully applied to the assay of beta-CD in serum samples.

摘要

已开发出一种高效液相色谱法用于测定环糊精（CDs）和支链环糊精。该方法包括在反相柱上使用水和乙腈的混合物作为洗脱剂进行分离，通过被1.5 M氢氧化钠溶液包围的阳离子交换膜反应器调节洗脱剂的pH值，以及使用金工作电极进行脉冲安培检测。通过峰高与进样量构建的校准曲线在50 - 1000 pmol范围内呈线性。在信噪比为3时，CDs和支链环糊精的检测限约为1 - 5 pmol。该方法已成功应用于血清样品中β-环糊精的测定。