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通过毛细管电泳采用高碘酸盐氧化法测定环糊精含量。

Determination of cyclodextrin content using periodate oxidation by capillary electrophoresis.

作者信息

Pumera M, Jelínek I, Jindrich J, Coufal P, Horský J

机构信息

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

出版信息

J Chromatogr A. 2000 Sep 1;891(1):201-6. doi: 10.1016/s0021-9673(00)00628-2.

Abstract

A simple and general method suitable for the determination of cyclodextrin content in various matrices is described. The proposed method involves selective cleavage of C-C bonds with vicinal hydroxyl groups by means of periodate (Malaprade's reaction). The amount of produced iodate is monitored by capillary electrophoresis. Optimized electrophoretic conditions (20 mM disodium tetraborate with 1 mM tetradecyltrimethylammonium bromide, direct UV detection lambda = 200 nm) ensure complete separation of periodate and iodate ions and sufficient sensitivity towards iodate. Under optimized reaction conditions (2-fold excess of periodate, temperature 70 degrees C) reproducible quantitative results were obtained for alpha-, beta- and gamma-cyclodextrins as model samples. The proposed method was tested on a real sample of acrylamide--2'-O-allyl-beta-CD copolymer. The values of beta-cyclodextrin content were compared with those obtained by reference NMR measurement and were found to be identical.

摘要

本文描述了一种适用于测定各种基质中 cyclodextrin 含量的简单通用方法。所提出的方法涉及通过高碘酸盐(马拉普雷德反应)选择性裂解具有邻位羟基的 C-C 键。通过毛细管电泳监测生成的碘酸盐的量。优化的电泳条件(20 mM 四硼酸钠与 1 mM 十四烷基三甲基溴化铵,直接紫外检测波长λ = 200 nm)确保高碘酸盐和碘酸盐离子的完全分离以及对碘酸盐有足够的灵敏度。在优化的反应条件(高碘酸盐过量 2 倍,温度 70 摄氏度)下,以α-、β-和γ-环糊精作为模型样品获得了可重复的定量结果。该方法在丙烯酰胺 - 2'-O-烯丙基-β-CD 共聚物的实际样品上进行了测试。将β-环糊精含量的值与通过参考 NMR 测量获得的值进行比较,发现两者相同。

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