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Determination of 2,4,6-trichloroanisole and 2,4,6-tribromoanisole on ng L-1 to pg L-1 levels in wine by soild-phase microextraction and gas chromatography-high-resolution mass spectrometry
Örebro University, Department of Natural Sciences.
Örebro University, Department of Natural Sciences.ORCID iD: 0000-0001-6217-8857
Örebro University, Department of Restaurant & Culinary Arts.
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2006 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1111, no 1, p. 71-75Article in journal (Refereed) Published
Abstract [en]

A gas chromatography-high-resolution mass spectrometry (GC-HRMS) method using solid-phase microextraction (SPME) for the determination of 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA) in wine at low ng L−1 levels was developed. A robust SPME method was developed by optimizing several different parameters, including type of fiber, salt addition, sample volume, extraction and desorption time. The quantification limit for TCA and TBA in wine was lowered substantially using GC-HRMS in combination with the optimized SPME method and allowed the detection of low analyte concentrations (ng L−1) with good accuracy. Limits of quantification for red wine of 0.3 ng L−1 for TCA and 0.2 ng L−1 for TBA with gas chromatography-negative chemical ionization mass spectrometry and 0.03 ng L−1 for TCA and TBA were achieved using GC-HRMS. The method was applied to 30 wines of which 4 wines were sensorically qualified as cork defected. TCA was found in three of these wines with concentrations in the range 2–25 ng L−1. TBA was not detected in any of the samples.

Place, publisher, year, edition, pages
2006. Vol. 1111, no 1, p. 71-75
National Category
Chemical Sciences
Research subject
Chemistry
Identifiers
URN: urn:nbn:se:oru:diva-2906DOI: 10.1016/j.chroma.2006.01.096OAI: oai:DiVA.org:oru-2906DiVA, id: diva2:135473
Available from: 2008-02-15 Created: 2008-02-15 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Microextraction for usage in environmental monitoring and modelling of nitroaromatic compounds and haloanisoles
Open this publication in new window or tab >>Microextraction for usage in environmental monitoring and modelling of nitroaromatic compounds and haloanisoles
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Processes in the environment are often complex and the description and prediction of the behaviour of environmental pollutants requires sophisticated methodology including multidimensional technology. Multivariate statistical methods including principal component analysis (PCA) and partial least squares projection to latent structures (PLS) were used to characterise several nitroaromatic compounds according to a large number of chemical and physical properties. These descriptors were derived from databases and semi-empirical, empirical and quantum-chemical calculations. A model was calculated and used for prediction of experimentally determined relevant environmental parameters, including volatility through gas chromatographic retention times and the distribution between air and water phase using solid-phase microextraction measurements. Analytical microextraction techniques are very well suited for both monitoring and measuring relevant environmental properties. Two such methods, solid-phase microextraction (SPME) and microextraction by packed syringe (MEPS), which are both faster and less resource demanding than traditional methodology, were used to improve the analysis of nitroaromatic compound and haloanisoles. Both techniques showed few interfering compounds and good reproducibility in combination with GC-MS detection. The reproducibility for SPME and MEPS was further enhanced by the usage of isotopically labelled internal standards (nitroaromatic compounds) or internal standards with similar chemical properties as the analytes (haloanisoles).

The SPME method for nitroaromatic compounds was tested using industrial wastewater from a wastewater treatment facility receiving input from several nitrogen based industries. Using gas chromatography-negative chemical ionisation-mass spectrometry(GC-NCI-MS) as the final detection, limits of detection (LODs) in the range 0.02–38 ng L−1 were achieved. Results for the 2,4,6-TCA (TCA) and 2,4,6-TBA (TBA) using high resolution GC-MS were even more impressive obtaining LODs in the range 0.02-0.03 ng L-1, which are currently the lowest reported in the international literature. Although the newly developed MEPS technology is generally faster than SPME, similar LODs as for SPME could not yet be achieved. Both methods were found to be so sensitive that TCA and TBA could be detected in wine before it could be sensorically noticed as cork tainted.

Place, publisher, year, edition, pages
Örebro: Örebro universitet, 2008. p. 58
Series
Örebro Studies in Chemistry, ISSN 1651-4270 ; 9
Keyword
PCA, PLS, QSPR, SPME, MEPS, nitroaromatic compounds, TCA, TBA
National Category
Chemical Sciences
Research subject
Chemistry
Identifiers
urn:nbn:se:oru:diva-1786 (URN)978-91-7668-582-2 (ISBN)
Public defence
2008-03-07, Bion, Forumhuset, Örebro universitet, Örebro, 10:00
Opponent
Supervisors
Available from: 2008-02-15 Created: 2008-02-15 Last updated: 2017-10-18Bibliographically approved

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Jönsson, Sofievan Bavel, BertGustafsson, Inga-BrittLindström, Gunilla

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