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应用于气相色谱法测定脂肪胺的血浆样品的液膜后处理

Liquid membrane work-up of blood plasma samples applied to gas chromatographic determination of aliphatic amines.

作者信息

Lindegård B, Jönsson J A, Mathiasson L

机构信息

Analytical Chemistry, University of Lund, Sweden.

出版信息

J Chromatogr. 1992 Jan 17;573(2):191-200. doi: 10.1016/0378-4347(92)80119-b.

DOI:10.1016/0378-4347(92)80119-b
PMID:1601951
Abstract

A technique for sample work-up and enrichment using a supported liquid membrane in an automated flow system, connected to a gas chromatograph, was used for the determination of aliphatic amines in human blood plasma. The amines studied were N,N-dimethylethylamine, triethylamine, N-methylmorpholine, cyclohexylamine and N,N-dimethylcyclohexylamine. An efficient clean-up of the complex plasma matrix was achieved, resulting in identical blank chromatograms for plasma samples and aqueous solutions. Different parameters influencing the efficiency and selectivity of the extraction procedure were experimentally studied and theoretically explained. The detection limit depends on the extraction flow-rate and the available sample volume. With 1 ml of sample and a flow-rate giving an extraction time of 16 min, the detection limit was ca. 5 ppb (5 micrograms/l); with 4 ml of sample and a lower flow-rate, sub-ppb detection limits could be reached in ca. 3 h. Linear calibration curves up to 500 ppb were obtained. Blood plasma samples from volunteers exposed to N,N-dimethylethylamine in air were analysed, and the results compared favourably with independent measurements by another method.

摘要

一种在与气相色谱仪相连的自动化流动系统中使用支撑液膜进行样品处理和富集的技术,被用于测定人血浆中的脂肪胺。所研究的胺类包括N,N-二甲基乙胺、三乙胺、N-甲基吗啉、环己胺和N,N-二甲基环己胺。实现了对复杂血浆基质的有效净化,使得血浆样品和水溶液的空白色谱图相同。通过实验研究并从理论上解释了影响萃取过程效率和选择性的不同参数。检测限取决于萃取流速和可用样品体积。使用1 ml样品且流速使得萃取时间为16分钟时,检测限约为5 ppb(5微克/升);使用4 ml样品且流速较低时,在约3小时内可达到亚ppb的检测限。获得了高达500 ppb的线性校准曲线。对暴露于空气中N,N-二甲基乙胺的志愿者的血浆样品进行了分析,结果与另一种方法的独立测量结果相比具有优势。

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