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用于分析水样中挥发性脂肪酸的衍生化单滴微萃取方法的开发。

Development of a Single-Drop Microextraction with Derivatization Procedure for Analysis of Volatile Fatty Acids in Water Samples.

作者信息

Wejnerowska Grażyna

机构信息

Department of Food Analytics and Environmental Protection, Faculty of Chemical Technology and Engineering, University of Science and Technology in Bydgoszcz, Seminaryjna 3 St., 85-326 Bydgoszcz, Poland.

出版信息

Chromatographia. 2017;80(7):1115-1120. doi: 10.1007/s10337-017-3316-0. Epub 2017 May 25.

DOI:10.1007/s10337-017-3316-0
PMID:28725084
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5486468/
Abstract

A single-drop microextraction (SDME) was developed for the analysis of volatile fatty acids (VFAs) (C-C) in water by gas chromatography (GC) with flame ionization detection. The significant parameters affecting the SDME performance such as selection of microextraction solvent, extraction time, stirring rate, sample pH and temperature, and ionic strength were studied and optimized. To lower limits of detection, derivatization of VFAs by -methyl--(-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) was performed. The method developed requires very short time of extraction and derivatization (13 min) and it is characterized by a good precision (max RSD = 11.4%), linearity and relatively low limits of detection (from 8.3 mg L for acetic acid to 0.008 mg L for heptanoic acid). The results of the SDME in combination with GC show promising potential for the analysis of VFAs in water samples.

摘要

开发了一种单滴微萃取(SDME)方法,用于通过气相色谱(GC)和火焰离子化检测分析水中的挥发性脂肪酸(VFA,C - C)。研究并优化了影响SDME性能的重要参数,如微萃取溶剂的选择、萃取时间、搅拌速率、样品pH值、温度和离子强度。为了降低检测限,用α - 甲基 - N - (叔丁基二甲基硅烷基)三氟乙酰胺(MTBSTFA)对VFA进行衍生化。所开发的方法所需的萃取和衍生化时间非常短(13分钟),具有良好的精密度(最大相对标准偏差 = 11.4%)、线性和相对较低的检测限(从乙酸的8.3毫克/升到庚酸的0.008毫克/升)。SDME与GC相结合的结果表明,该方法在分析水样中的VFA方面具有广阔的应用前景。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d45c/5486468/0d7d093e7e97/10337_2017_3316_Fig3_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d45c/5486468/cc5887938f73/10337_2017_3316_Fig1_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d45c/5486468/a62b4cca22a1/10337_2017_3316_Fig2_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d45c/5486468/0d7d093e7e97/10337_2017_3316_Fig3_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d45c/5486468/cc5887938f73/10337_2017_3316_Fig1_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d45c/5486468/a62b4cca22a1/10337_2017_3316_Fig2_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d45c/5486468/0d7d093e7e97/10337_2017_3316_Fig3_HTML.jpg

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Trace analysis of chlorobenzenes in water samples using headspace solvent microextraction and gas chromatography/electron capture detection.采用顶空溶剂微萃取和气相色谱/电子捕获检测法对水样中的氯苯进行痕量分析。
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