Development of an Analytical Method for Antimony Speciation in Vegetables by HPLC-Hydride Generation-Atomic Fluorescence Spectrometry

David Olivares, Manuel Bravo, Jorg Feldmann, Andrea Raab, Alexander Neaman, Waldo Quiroz

Research output: Contribution to journalArticle

7 Citations (Scopus)

Abstract

A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 mu g/L and 5.0, 5.2, and 4.7%, respectively, for a 100 mu L sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts.

Original languageEnglish
Pages (from-to)1176-1182
Number of pages7
JournalJournal of Association of Analytical Communities International
Volume95
Issue number4
DOIs
Publication statusPublished - Jul 2012

Cite this

Development of an Analytical Method for Antimony Speciation in Vegetables by HPLC-Hydride Generation-Atomic Fluorescence Spectrometry. / Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea; Neaman, Alexander; Quiroz, Waldo.

In: Journal of Association of Analytical Communities International, Vol. 95, No. 4, 07.2012, p. 1176-1182.

Research output: Contribution to journalArticle

@article{2c604c9aa82e4042860aa8cfa6d00400,
title = "Development of an Analytical Method for Antimony Speciation in Vegetables by HPLC-Hydride Generation-Atomic Fluorescence Spectrometry",
abstract = "A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 mu g/L and 5.0, 5.2, and 4.7{\%}, respectively, for a 100 mu L sample volume. The application of this method to real samples allowed extraction of 50{\%} of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70{\%}, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70{\%} of the total antimony in the extracts.",
author = "David Olivares and Manuel Bravo and Jorg Feldmann and Andrea Raab and Alexander Neaman and Waldo Quiroz",
year = "2012",
month = "7",
doi = "10.5740/jaoacint.11-278",
language = "English",
volume = "95",
pages = "1176--1182",
journal = "Journal of Association of Analytical Communities International",
issn = "1060-3271",
publisher = "AOAC International",
number = "4",

}

TY - JOUR

T1 - Development of an Analytical Method for Antimony Speciation in Vegetables by HPLC-Hydride Generation-Atomic Fluorescence Spectrometry

AU - Olivares, David

AU - Bravo, Manuel

AU - Feldmann, Jorg

AU - Raab, Andrea

AU - Neaman, Alexander

AU - Quiroz, Waldo

PY - 2012/7

Y1 - 2012/7

N2 - A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 mu g/L and 5.0, 5.2, and 4.7%, respectively, for a 100 mu L sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts.

AB - A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 mu g/L and 5.0, 5.2, and 4.7%, respectively, for a 100 mu L sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts.

U2 - 10.5740/jaoacint.11-278

DO - 10.5740/jaoacint.11-278

M3 - Article

VL - 95

SP - 1176

EP - 1182

JO - Journal of Association of Analytical Communities International

JF - Journal of Association of Analytical Communities International

SN - 1060-3271

IS - 4

ER -