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在吸附萃取后的进样衍生化。

In-port derivatization after sorptive extractions.

机构信息

Department of Analytical Chemistry, University of the Basque Country (UPV/EHU), PK 644, 48080 Bilbao, Spain.

出版信息

J Chromatogr A. 2013 Jun 28;1296:36-46. doi: 10.1016/j.chroma.2013.03.058. Epub 2013 Mar 28.

Abstract

Derivatization is necessary when analysis of polar compounds containing hydroxyl, carboxylic acid, amine or thiol functional groups is accomplished by gas chromatography (GC), in order to improve peak symmetry, peak separation and detector response. Derivatization can be performed off-line in a reaction vessel that is separated from the GC analysis hardware. However, on-line derivatization can eliminate time-consuming sample-processing steps, decrease the amount of valuable and/or toxic reagents and solvents that are used off-line, as well as increase the speed and efficiency of the analysis performed. The present work revises on-line in-port derivatizations where the derivatization reaction is simultaneously carried out with the analysis step by injecting the sample/reagent mixture directly into the hot GC inlet after a sorptive extraction step. Sorptive extractions revised range from the more classical solid-phase extraction (SPE) to the microextraction approaches, including solid-phase microextraction (SPME) and stir-bar sorptive extraction (SBSE) applications, as well as liquid-phase microextraction (LPME) or microextraction by packed sorbent (MEPS).

摘要

当通过气相色谱 (GC) 分析含有羟基、羧酸、胺或硫醇官能团的极性化合物时,需要进行衍生化,以改善峰形对称性、峰分离和检测器响应。衍生化可以在与 GC 分析硬件分离的反应容器中离线进行。然而,在线衍生化可以消除耗时的样品处理步骤,减少离线使用的有价值和/或有毒试剂和溶剂的用量,以及提高分析的速度和效率。本工作修订了在线进样口衍生化,其中在吸附萃取步骤之后,将样品/试剂混合物直接注入热 GC 进样口,同时进行衍生化反应。吸附萃取修订范围从更经典的固相萃取 (SPE) 到微萃取方法,包括固相微萃取 (SPME) 和搅拌棒吸附萃取 (SBSE) 应用,以及液相微萃取 (LPME) 或填充吸附剂的微萃取 (MEPS)。

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