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直接进样和柱后衍生-电化学检测法测定尿香草扁桃酸

Determination of urinary vanillylmandelic acid by direct injection and coupled-column chromatography with electrochemical detection.

作者信息

Eriksson B M, Persson B A, Wikström M

机构信息

Bioanalytical Chemistry, AB Hässle, Mölndal, Sweden.

出版信息

J Chromatogr. 1990 Apr 27;527(1):11-9. doi: 10.1016/s0378-4347(00)82078-2.

DOI:10.1016/s0378-4347(00)82078-2
PMID:2365768
Abstract

An automated column-switching system for determination of vanillylmandelic acid in urine is described. The liquid chromatographic system was composed of two separation columns with different selectivity properties, an octadecyl column coated with tributyl phosphate as stationary liquid phase and a silica-based anion exchanger. Urine samples were injected directly onto the first column, where vanillylmandelic acid was separated from the main part of the sample matrix. The internal standard isovanillylmandelic acid was co-eluting with vanillylmandelic acid, and a fraction of the eluate containing both substances was switched to the second column, where separation was performed. To assess peak purity, detection was performed with dual working electrodes in parallel mode. A relative standard deviation of 3.5% was obtained for determination of human urine samples containing 3 microM vanillylmandelic acid, and less than 0.1 microM could be detected.

摘要

本文描述了一种用于测定尿中香草扁桃酸的自动柱切换系统。液相色谱系统由两根具有不同选择性的分离柱组成,一根涂有磷酸三丁酯作为固定液相的十八烷基柱和一根硅胶基阴离子交换柱。尿液样品直接注入第一根柱,在该柱上香草扁桃酸与样品基质的主要部分分离。内标异香草扁桃酸与香草扁桃酸共洗脱,含有这两种物质的一部分洗脱液切换至第二根柱进行分离。为评估峰纯度,采用双工作电极以平行模式进行检测。对于含3 microM香草扁桃酸的人尿样品测定,相对标准偏差为3.5%,检测限小于0.1 microM。

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