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采用间接紫外和电导检测的毛细管电泳法测定环糊精及其衍生物

Determination of cyclodextrins and their derivatives by capillary electrophoresis with indirect UV and conductivity detection.

作者信息

Pumera M, Jelínek I, Jindrich J

机构信息

Department of Analytical Chemistry, Charles University, Faculty of Science, Prague, Czech Republic.

出版信息

Fresenius J Anal Chem. 2001 Apr;369(7-8):666-9. doi: 10.1007/s002160100721.

Abstract

A fast and simple capillary electrophoretic method suitable for the determination of native alpha-, beta-, gamma-cyclodextrins, their randomly substituted tert-butyl derivatives (average degree of substitution 3.8-4.4), heptakis (2,6-di-O-methyl)- and heptakis (2,3,6-tri-O-methyl)-beta-cyclodextrin was developed. Naphthyl-2-sulfonic acid (2-NSA), 3-iodobenzoic acid (3-IBA) and (1S)-1-phenylethylamine (PHEA) were tested as selective complex forming and UV absorbing background electrolyte additives. The composition of optimized background electrolyte for the separation of uncharged cyclodextrins and their derivatives was: 15 mM 3-iodobenzoic acid titrated with tris[hydroxymethyl]aminomethane to pH 8.0, 5% (v/v) of acetonitrile. A complete resolution of mono-2-O-, mono-3-O- and mono-6-O-carboxymethyl-beta-cyclodextrin regioisomers was achieved in the optimized background electrolyte system: 40 mM PHEA titrated with 2-[N-morpholino]ethanesulfonic acid to pH 5.6. In addition to indirect UV detection a contactless conductometric detector was successfully utilized.

摘要

开发了一种快速简便的毛细管电泳方法,适用于测定天然的α-、β-、γ-环糊精、它们的随机取代叔丁基衍生物(平均取代度3.8 - 4.4)、七(2,6-二-O-甲基)-和七(2,3,6-三-O-甲基)-β-环糊精。测试了萘基-2-磺酸(2-NSA)、3-碘苯甲酸(3-IBA)和(1S)-1-苯乙胺(PHEA)作为选择性络合形成和紫外吸收背景电解质添加剂。用于分离不带电荷的环糊精及其衍生物的优化背景电解质组成是:用三(羟甲基)氨基甲烷滴定至pH 8.0的15 mM 3-碘苯甲酸,5%(v/v)乙腈。在优化的背景电解质体系中:用2-[N-吗啉基]乙磺酸滴定至pH 5.6的40 mM PHEA,实现了单-2-O-、单-3-O-和单-6-O-羧甲基-β-环糊精区域异构体的完全分离。除了间接紫外检测外,还成功使用了非接触式电导检测器。

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