Issue 16, 2012
From the journal:

Analyst

Determination of Se using a solid-phase micro-extraction device coupled to a graphite furnace and detection by gas chromatography-mass spectrometry

Elidiane Gomes da Silva,a   Fabio Augustob  and  Marco Aurélio Zezzi Arruda*a  

* Corresponding authors

a National Institute of Science and Technology for Bioanalytics and Spectrometry, Sample Preparation and Mechanization Group (GEPAM), Institute of Chemistry – University of Campinas (UNICAMP), P.O. Box 6154, 13083-970 Campinas, SP, Brazil
E-mail: zezzi@iqm.unicamp.br

b Laboratory of Gas Chromatography, Institute of Chemistry – University of Campinas (UNICAMP), P.O. Box 6154, 13083-970 Campinas, SP, Brazil

Abstract

A solid-phase micro-extraction (SPME) method using an SPME fiber device and graphite furnace (GF) for extracting Se compounds was proposed. Various factors affecting the derivatization and extraction of Se(IV) by SPME-GF were evaluated, including the effect of acid (type and concentration), the concentration of the derivatizing agent, the derivatization temperature, the extraction and derivatization times and the extraction temperature. After optimizing these conditions, the quantification of Se(IV) was performed by Gas Chromatography-Mass Spectrometry (GC-MS). The limit of detection was 0.37 μg L−1 for Se(IV). The method was successfully applied to the total Se determination in certified reference materials (BCR-414 and SRM 1643e). A recovery of 97% was obtained for water (SRM 1643e). After microwave oven decomposition and the reduction of selenium using a mixture of 2 mol L−1 HCl and 1% (w/v) KBr, a recovery of 101% and a relative standard deviation of 3.5% were attained for plankton (BCR-414). The SPME-GF method combined with GC-MS was also applied to the determination of the total selenium in a drug sample (selenium chelate).

Graphical abstract: Determination of Se using a solid-phase micro-extraction device coupled to a graphite furnace and detection by gas chromatography-mass spectrometry

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Article information

DOI
https://doi.org/10.1039/C2AN35598A
Article type
Paper
Submitted
08 Feb 2012
Accepted
11 Jun 2012
First published
12 Jun 2012

Analyst, 2012,137, 3841-3846

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Determination of Se using a solid-phase micro-extraction device coupled to a graphite furnace and detection by gas chromatography-mass spectrometry

E. Gomes da Silva, F. Augusto and M. A. Z. Arruda, Analyst, 2012, 137, 3841 DOI: 10.1039/C2AN35598A

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