期刊
ANALYTICA CHIMICA ACTA
卷 828, 期 -, 页码 53-60出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2014.04.031
关键词
In-syringe; Sequential injection analysis; Head-space; Single-drop micro-extraction; Spectrophotometric detection; Ethanol
资金
- Charles University in Prague - projects [GAUK 1316213, SVV 260063]
- Education for Competitiveness Operational Program (ECOP) [CZ.1.07/2.3.00/30.0022]
- European Social Fund
- state budget of the Czech Republic
A novel approach of head-space single-drop micro-extraction applied to the determination of ethanol in wine is presented. For the first time, the syringe of an automated syringe pump was used as an extraction chamber of adaptable size for a volatile analyte. This approach enabled to apply negative pressure during the enrichment step, which favored the evaporation of the analyte. Placing a slowly spinning magnetic stirring bar inside the syringe, effective syringe cleaning as well as mixing of the sample with buffer solution to suppress the interference of acetic acid was achieved. Ethanol determination was based on the reduction of a single drop of 3 mmol L-1 potassium dichromate dissolved in 8 mol L-1 sulfuric acid. The drop was positioned in the syringe inlet in the head-space above the sample with posterior spectrophotometric quantification. The entire procedure was carried out automatically using a simple sequential injection analyzer system. One analysis required less than 5 min including the washing step. A limit of detection of 0.025% (v/v) of ethanol and an average repeatability of less than 5.0% RSD were achieved. The consumption of dichromate reagent, buffer, and sample per analysis were only 20 mu L, 200 mu L, and 1 mL, respectively. The results of real samples analysis did not differ significantly from those obtained with the references gas chromatography method. (C) 2014 Elsevier B.V. All rights reserved.
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