Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions

Head space (HS) solid phase microextraction (SPME) followed by gas chromatography with mass spectrometry detection (GC-MS) is the most widespread technique to study the volatile profile of honey samples. In this paper, the experimental SPME conditions were optimized by a multivariate strategy. Both...

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Main Authors: Elisa Robotti, Federica Campo, Marta Riviello, Marco Bobba, Marcello Manfredi, Eleonora Mazzucco, Fabio Gosetti, Giorgio Calabrese, Emanuele Sangiorgi, Emilio Marengo
Format: Article
Language:English
Published: Wiley 2017-01-01
Series:Journal of Chemistry
Online Access:http://dx.doi.org/10.1155/2017/6437857
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author Elisa Robotti
Federica Campo
Marta Riviello
Marco Bobba
Marcello Manfredi
Eleonora Mazzucco
Fabio Gosetti
Giorgio Calabrese
Emanuele Sangiorgi
Emilio Marengo
author_facet Elisa Robotti
Federica Campo
Marta Riviello
Marco Bobba
Marcello Manfredi
Eleonora Mazzucco
Fabio Gosetti
Giorgio Calabrese
Emanuele Sangiorgi
Emilio Marengo
author_sort Elisa Robotti
collection DOAJ
description Head space (HS) solid phase microextraction (SPME) followed by gas chromatography with mass spectrometry detection (GC-MS) is the most widespread technique to study the volatile profile of honey samples. In this paper, the experimental SPME conditions were optimized by a multivariate strategy. Both sensitivity and repeatability were optimized by experimental design techniques considering three factors: extraction temperature (from 50°C to 70°C), time of exposition of the fiber (from 20 min to 60 min), and amount of salt added (from 0 to 27.50%). Each experiment was evaluated by Principal Component Analysis (PCA) that allows to take into consideration all the analytes at the same time, preserving the information about their different characteristics. Optimal extraction conditions were identified independently for signal intensity (extraction temperature: 70°C; extraction time: 60 min; salt percentage: 27.50% w/w) and repeatability (extraction temperature: 50°C; extraction time: 60 min; salt percentage: 27.50% w/w) and a final global compromise (extraction temperature: 70°C; extraction time: 60 min; salt percentage: 27.50% w/w) was also reached. Considerations about the choice of the best internal standards were also drawn. The whole optimized procedure was than applied to the analysis of a multiflower honey sample and more than 100 compounds were identified.
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institution Kabale University
issn 2090-9063
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spelling doaj-art-372a0eba53a340c3a1dd1c0da5a540142025-08-20T03:55:02ZengWileyJournal of Chemistry2090-90632090-90712017-01-01201710.1155/2017/64378576437857Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target FunctionsElisa Robotti0Federica Campo1Marta Riviello2Marco Bobba3Marcello Manfredi4Eleonora Mazzucco5Fabio Gosetti6Giorgio Calabrese7Emanuele Sangiorgi8Emilio Marengo9Department of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyDepartment of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyDepartment of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyDepartment of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyDepartment of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyDepartment of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyDepartment of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyDepartment of Pharmacy, Università degli Studi di Napoli Federico II, Via Montesano 49, 80131 Napoli, ItalyIstituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna, Via Bianchi 9, 25124 Brescia, ItalyDepartment of Sciences and Technological Innovation, University of Piemonte Orientale, Viale Michel 11, 15121 Alessandria, ItalyHead space (HS) solid phase microextraction (SPME) followed by gas chromatography with mass spectrometry detection (GC-MS) is the most widespread technique to study the volatile profile of honey samples. In this paper, the experimental SPME conditions were optimized by a multivariate strategy. Both sensitivity and repeatability were optimized by experimental design techniques considering three factors: extraction temperature (from 50°C to 70°C), time of exposition of the fiber (from 20 min to 60 min), and amount of salt added (from 0 to 27.50%). Each experiment was evaluated by Principal Component Analysis (PCA) that allows to take into consideration all the analytes at the same time, preserving the information about their different characteristics. Optimal extraction conditions were identified independently for signal intensity (extraction temperature: 70°C; extraction time: 60 min; salt percentage: 27.50% w/w) and repeatability (extraction temperature: 50°C; extraction time: 60 min; salt percentage: 27.50% w/w) and a final global compromise (extraction temperature: 70°C; extraction time: 60 min; salt percentage: 27.50% w/w) was also reached. Considerations about the choice of the best internal standards were also drawn. The whole optimized procedure was than applied to the analysis of a multiflower honey sample and more than 100 compounds were identified.http://dx.doi.org/10.1155/2017/6437857
spellingShingle Elisa Robotti
Federica Campo
Marta Riviello
Marco Bobba
Marcello Manfredi
Eleonora Mazzucco
Fabio Gosetti
Giorgio Calabrese
Emanuele Sangiorgi
Emilio Marengo
Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions
Journal of Chemistry
title Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions
title_full Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions
title_fullStr Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions
title_full_unstemmed Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions
title_short Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions
title_sort optimization of the extraction of the volatile fraction from honey samples by spme gc ms experimental design and multivariate target functions
url http://dx.doi.org/10.1155/2017/6437857
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