A robust method for quantification of volatile compounds within and between vintages using headspace-solid-phase micro-extraction coupled with GC'MS

Application on Semillon wines

Research output: Contribution to journalArticle

39 Citations (Scopus)

Abstract

A headspace-solid-phase micro-extraction'gas chromatography'mass spectrometry (HS-SPME'GC'MS) method has been developed to quantify a range of volatile compounds in Hunter Valley Semillon wines. The fibre selected for the method was a 50/30 'm divinylbenzene/carboxen/polydimethylsiloxane fibre, a three-phase fibre that allows extraction and desorption of a wide range of volatile compounds of different chemical functionalities and polarities. Four internal standards, methyl isobutyl ketone, n-dodecane, 4-methyl-2-pentanol and ethyl nonanoate were used to monitor the SPME fibre extraction efficiency and integrity. Fibre integrity was monitored by plotting the ratio of the peak area for each internal standard divided by the sum of the peak area for all internal standards as a function of analysis number. The advantage of using four internal standards for better quality control of the fibre integrity is described. The identity of twenty-one volatile compounds was ascertained by comparison of their chemical characteristics (retention indices, mass spectra) with reference compounds using two columns of different polarities. Quantification was achieved using calibration curves constructed for each compound with linear regression equations having correlation coefficients (R2) ranging from 0.9717 to 0.9999. The method was applied to two Semillon wines (recent vintage and aged) representative of the Hunter Valley styles. As is typical of white wines, 3-methyl-1-butanol was quantified as the most concentrated volatile compound (83 and 66 mg L'1 for the 2006 and the 1996 wines, respectively). The study highlights the use of well-defined procedures to ensure integrity of quantitative data where several fibres may be required during an extended study over one or more vintages.
Original languageEnglish
Pages (from-to)149-157
Number of pages9
JournalAnalytica Chimica Acta
Volume660
Issue number1-2
DOIs
Publication statusPublished - Feb 2010

Fingerprint

Wine
Solid Phase Extraction
Fibers
divinyl benzene
Quality Control
Gas Chromatography-Mass Spectrometry
Calibration
Linear Models
valley
ketone
fibre
method
wine
Linear regression
Gas chromatography
quality control
Quality control
Mass spectrometry
Desorption
desorption

Cite this

@article{cc471055976d4f5cac327a8c439ea076,
title = "A robust method for quantification of volatile compounds within and between vintages using headspace-solid-phase micro-extraction coupled with GC'MS: Application on Semillon wines",
abstract = "A headspace-solid-phase micro-extraction'gas chromatography'mass spectrometry (HS-SPME'GC'MS) method has been developed to quantify a range of volatile compounds in Hunter Valley Semillon wines. The fibre selected for the method was a 50/30 'm divinylbenzene/carboxen/polydimethylsiloxane fibre, a three-phase fibre that allows extraction and desorption of a wide range of volatile compounds of different chemical functionalities and polarities. Four internal standards, methyl isobutyl ketone, n-dodecane, 4-methyl-2-pentanol and ethyl nonanoate were used to monitor the SPME fibre extraction efficiency and integrity. Fibre integrity was monitored by plotting the ratio of the peak area for each internal standard divided by the sum of the peak area for all internal standards as a function of analysis number. The advantage of using four internal standards for better quality control of the fibre integrity is described. The identity of twenty-one volatile compounds was ascertained by comparison of their chemical characteristics (retention indices, mass spectra) with reference compounds using two columns of different polarities. Quantification was achieved using calibration curves constructed for each compound with linear regression equations having correlation coefficients (R2) ranging from 0.9717 to 0.9999. The method was applied to two Semillon wines (recent vintage and aged) representative of the Hunter Valley styles. As is typical of white wines, 3-methyl-1-butanol was quantified as the most concentrated volatile compound (83 and 66 mg L'1 for the 2006 and the 1996 wines, respectively). The study highlights the use of well-defined procedures to ensure integrity of quantitative data where several fibres may be required during an extended study over one or more vintages.",
keywords = "Gas chromatography'mass spectrometry, Internal standard, Semillon, Solid-phase micro-extraction, Volatile compounds, White wine",
author = "Laure Rebiere and Andrew Clark and Leigh Schmidtke and Paul Prenzler and Geoffrey Scollary",
note = "Imported on 12 Apr 2017 - DigiTool details were: month (773h) = Feb 2010; Journal title (773t) = Analytica Chimica Acta. ISSNs: 0003-2670;",
year = "2010",
month = "2",
doi = "10.1016/j.aca.2009.10.029",
language = "English",
volume = "660",
pages = "149--157",
journal = "Analytica Chimica Acta",
issn = "0003-2670",
publisher = "Elsevier",
number = "1-2",

}

TY - JOUR

T1 - A robust method for quantification of volatile compounds within and between vintages using headspace-solid-phase micro-extraction coupled with GC'MS

T2 - Application on Semillon wines

AU - Rebiere, Laure

AU - Clark, Andrew

AU - Schmidtke, Leigh

AU - Prenzler, Paul

AU - Scollary, Geoffrey

N1 - Imported on 12 Apr 2017 - DigiTool details were: month (773h) = Feb 2010; Journal title (773t) = Analytica Chimica Acta. ISSNs: 0003-2670;

PY - 2010/2

Y1 - 2010/2

N2 - A headspace-solid-phase micro-extraction'gas chromatography'mass spectrometry (HS-SPME'GC'MS) method has been developed to quantify a range of volatile compounds in Hunter Valley Semillon wines. The fibre selected for the method was a 50/30 'm divinylbenzene/carboxen/polydimethylsiloxane fibre, a three-phase fibre that allows extraction and desorption of a wide range of volatile compounds of different chemical functionalities and polarities. Four internal standards, methyl isobutyl ketone, n-dodecane, 4-methyl-2-pentanol and ethyl nonanoate were used to monitor the SPME fibre extraction efficiency and integrity. Fibre integrity was monitored by plotting the ratio of the peak area for each internal standard divided by the sum of the peak area for all internal standards as a function of analysis number. The advantage of using four internal standards for better quality control of the fibre integrity is described. The identity of twenty-one volatile compounds was ascertained by comparison of their chemical characteristics (retention indices, mass spectra) with reference compounds using two columns of different polarities. Quantification was achieved using calibration curves constructed for each compound with linear regression equations having correlation coefficients (R2) ranging from 0.9717 to 0.9999. The method was applied to two Semillon wines (recent vintage and aged) representative of the Hunter Valley styles. As is typical of white wines, 3-methyl-1-butanol was quantified as the most concentrated volatile compound (83 and 66 mg L'1 for the 2006 and the 1996 wines, respectively). The study highlights the use of well-defined procedures to ensure integrity of quantitative data where several fibres may be required during an extended study over one or more vintages.

AB - A headspace-solid-phase micro-extraction'gas chromatography'mass spectrometry (HS-SPME'GC'MS) method has been developed to quantify a range of volatile compounds in Hunter Valley Semillon wines. The fibre selected for the method was a 50/30 'm divinylbenzene/carboxen/polydimethylsiloxane fibre, a three-phase fibre that allows extraction and desorption of a wide range of volatile compounds of different chemical functionalities and polarities. Four internal standards, methyl isobutyl ketone, n-dodecane, 4-methyl-2-pentanol and ethyl nonanoate were used to monitor the SPME fibre extraction efficiency and integrity. Fibre integrity was monitored by plotting the ratio of the peak area for each internal standard divided by the sum of the peak area for all internal standards as a function of analysis number. The advantage of using four internal standards for better quality control of the fibre integrity is described. The identity of twenty-one volatile compounds was ascertained by comparison of their chemical characteristics (retention indices, mass spectra) with reference compounds using two columns of different polarities. Quantification was achieved using calibration curves constructed for each compound with linear regression equations having correlation coefficients (R2) ranging from 0.9717 to 0.9999. The method was applied to two Semillon wines (recent vintage and aged) representative of the Hunter Valley styles. As is typical of white wines, 3-methyl-1-butanol was quantified as the most concentrated volatile compound (83 and 66 mg L'1 for the 2006 and the 1996 wines, respectively). The study highlights the use of well-defined procedures to ensure integrity of quantitative data where several fibres may be required during an extended study over one or more vintages.

KW - Gas chromatography'mass spectrometry

KW - Internal standard

KW - Semillon

KW - Solid-phase micro-extraction

KW - Volatile compounds

KW - White wine

U2 - 10.1016/j.aca.2009.10.029

DO - 10.1016/j.aca.2009.10.029

M3 - Article

VL - 660

SP - 149

EP - 157

JO - Analytica Chimica Acta

JF - Analytica Chimica Acta

SN - 0003-2670

IS - 1-2

ER -