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Titre du document / Document title

Quantification of free and esterified sterols in portuguese olive oils by solid-phase extraction and gas chromatography-mass spectrometry

Auteur(s) / Author(s)

CUNHA Sara S. (1) ; FEMANDES José O. (1) ; OLIVEIRA M. Beatriz P. P. (1) ;

Affiliation(s) du ou des auteurs / Author(s) Affiliation(s)

(1) REQUIMTE/Serviço de Bromatologia, Faculdade de Farmàcia, Universidade do Porto, Rua Anibal Cunha 164, 4099-030 Porto, PORTUGAL

Résumé / Abstract

A simple and accurate method based on solid-phase extraction (SPE), transesterification and gas chromatography-mass spectrometry (GC-MS) was developed for the quantitative analysis of free and esterified sterols of olive oil. In order to achieve better separation of esterified and free sterols, silica and alumina SPE adsorbents were tested. Separations by silica provided more reproducible results. The transesterification of both sterol fractions was found to be more user friendly than saponification as a method to liberate the sterols from the respective esters. The free sterols were then silylated with N,O-bis-trimethylsilyltrifluoroacetamide (BSTFA) with 1% of trimethylchlorosilane (TMCS). The most favourable conditions for exploitation of this reagent were established. The optimized methodology was suitable for evaluation of free and esterified sterols in Protected Designation of Origin (PDO) olive oils and monovarietal olive oils with different maturation indices. The prevailing phytosterols in all olive oils were β-sitosterol and campesterol. The free sterols predominated, although they seemed to decrease with the maturation of the olive fruits.

Revue / Journal Title

Journal of chromatography    ISSN  0021-9673 

Source / Source

2006, vol. 1128, no1-2, pp. 220-227 [8 page(s) (article)] (39 ref.)

Langue / Language

Anglais

Editeur / Publisher

Elsevier, Amsterdam, PAYS-BAS  (1958) (Revue)

Mots-clés anglais / English Keywords

Europe

;

Chemical analysis

;

Trace analysis

;

Sample preparation

;

Chemical enrichment

;

Vegetable oil

;

Edible oil

;

Steroid

;

Validation

;

Silylation

;

Derivatization

;

Acylate

;

Mass spectrometry

;

Coupled method

;

Gas chromatography

;

Solid phase extraction

;

Olive oil

;

Portugal

;

Sterol

;

Quantitative analysis

;

Mots-clés français / French Keywords

Europe

;

GC MS

;

Analyse chimique

;

Analyse trace

;

Préparation échantillon

;

Enrichissement chimique

;

Huile végétale

;

Huile alimentaire

;

Stéroïde

;

Validation

;

Silylation

;

Dérivatisation

;

Acylate

;

Spectrométrie masse

;

Méthode couplée

;

Chromatographie phase gazeuse

;

Extraction SPE

;

Huile olive

;

Portugal

;

Stérol

;

Analyse quantitative

;

Mots-clés espagnols / Spanish Keywords

Europa

;

Análisis químico

;

Análisis huella

;

Preparación muestreo

;

Enriquecimiento químico

;

Aceite vegetal

;

Aceite alimentario

;

Esteroide

;

Validación

;

Sililación

;

Derivatisación

;

Acilato

;

Espectrometría masa

;

Método acoplado

;

Cromatografía fase gaseosa

;

Extracción SPE

;

Aceite oliva

;

Portugal

;

Esterol

;

Análisis cuantitativo

;

Mots-clés d'auteur / Author Keywords

Olive oils

;

Free sterols

;

Esterified sterols

;

Transesterification

;

Silica SPE

;

Localisation / Location

INIST-CNRS, Cote INIST : 8577 A, 35400014218623.0260

Nº notice refdoc (ud4) : 18082866



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