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Solid-Phase Microextraction for Qualitative and Quantitative Determination of Migrated Degradation Products of Antioxidants in an Organic Aqueous Solution
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
2005 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1080, no 2, 107-116 p.Article in journal (Refereed) Published
Abstract [en]

 Low molecular weight aromatic substances may migrate out from plastic packaging to their contents, especially if they consist of organic aqueous solutions or oils. It is, therefore, extremely important to be able to identify and quantify any migrated substances in such solutions, even at very low concentrations. We have in this work investigated and evaluated the use of solid-phase microextraction for the specific task of extraction from an organic aqueous solution such as a simulated pharmaceutical solution consisting of 10 vol.% ethanol in water. The goal was furthermore to investigate the possibility of simultaneously identifying and quantifying the substances in spite of differences in their chemical structures. Methods were developed and evaluated for extraction both with direct sampling and with headspace sampling. Difficulties appeared due to the ethanol in the solution and the minute amounts of substances present. We have shown that a simultaneous quantification of migrated low molecular weight degradation products of antioxidants using only one fibre is possible if the extraction method and temperature are adjusted in relation to the concentration levels of the analytes. Comparions were made with solid-phase extraction.

Place, publisher, year, edition, pages
2005. Vol. 1080, no 2, 107-116 p.
Keyword [en]
solid-phase microextraction, SPME, antioxidants, transformation products, migration
National Category
Chemical Engineering
Identifiers
URN: urn:nbn:se:kth:diva-5138DOI: 10.1016/j.chroma.2005.05.028ISI: 000230238600002Scopus ID: 2-s2.0-20444436365OAI: oai:DiVA.org:kth-5138DiVA: diva2:7933
Note
QC 20100929. Uppdaterad från Accepted till Published (20100929).Available from: 2005-05-25 Created: 2005-05-25 Last updated: 2017-12-04Bibliographically approved
In thesis
1. Chromatography and extraction techniques for new evaluation methods of polyolefins long-term performance
Open this publication in new window or tab >>Chromatography and extraction techniques for new evaluation methods of polyolefins long-term performance
2005 (English)Doctoral thesis, comprehensive summary (Other scientific)
Abstract [en]

Chromatography and extraction techniques, and also chemiluminescence have been utilized to develop new rapid and informative tools in the evaluation of long-term properties and environmental effects of polymeric materials.

Methods were developed for classification of materials and for early and rapid degradation detection. Degradable polyethylene films were classified on the basis of their incorporated prooxidant systems using chromatographic fingerprinting of carboxylic acids, the dominating type of degradation product. The fingerprints were also shown to be useful for prediction of the degradation states and evaluation of the degradation mechanisms. Classification and prediction models were obtained by Multivariate Data Analysis, where the diacids were grouped according to both their type of prooxidant system and their state of degradation. The use of total luminescence intensity (TLI) measurements was also investigated as a means of classifying films and for the early detection of degradation. Comparisons were carried out with common techniques, e.g. FTIR and DSC, after both thermal and UV oxidation. TLI gave an earlier detection of degradation and was more sensitive than carbonyl index and crystallinity measurements to relative differences in degradation between the materials. It furthermore offered complementary information regarding changes in activation energies during the course of the degradation. The results were compared with the chromatographic fingerprints.

A new way to evaluate the low temperature long-term stabilisation efficiency of antioxidants was investigated. A prooxidant was used to obtain catalytic oxidation, instead of using thermal acceleration, to evaluate the stabilisation efficiency of antioxidants at low temperatures but still during reasonably short aging times. Comparisons were made between polypropylene films stabilised with primary antioxidants (Irganox 1076, Irganox 1010 and α-tocopherol) with and without the prooxidant manganese stearate at different temperatures. The relative efficiencies of the antioxidants obtained under prooxidant acceleration test correlated better than thermal acceleration test with the results of a long-term low temperature test.

Additives in plastic packaging materials may affect the environment after migration from the packaging to e.g. their contents, especially if they consist of organic aqueous solutions or oils. The use of Solid-Phase Microextraction (SPME) for the specific task of extraction from an organic aqueous solution such as a simulated food or pharmaceutical solution consisting of 10 vol-% ethanol in water was investigated. Methods were developed and evaluated for extraction both with direct sampling and with headspace sampling. If the extraction method and temperature were selected to suit the concentration levels of the analytes, it was possible to quantify several degradation products simultaneously. Comparisons made with Solid Phase Extraction showed the advantage of SPME for this purpose.

Place, publisher, year, edition, pages
Stockholm: KTH, 2005. 86 p.
Series
Trita-FPT-Report, ISSN 1652-2443 ; 2005:20
Keyword
Chemical engineering, polymer, chromatographic fingerprinting, gas-chromatography – mass spectrometry, GC-MS, degradable polyethylene, prooxidant systems, chemiluminescence, oxidation, degradation mechanisms, accelerated ageing, antioxidants, transformation products, microwave assisted extraction, MAE, solid-phase microextraction, SPME, volatiles, solid phase extraction, SPE, Kemiteknik
National Category
Chemical Engineering
Identifiers
urn:nbn:se:kth:diva-219 (URN)91-7178-097-1 (ISBN)
Public defence
2005-06-16, K2, Teknikringen 28, Stockholm, 13:00
Opponent
Supervisors
Note
QC 20100929Available from: 2005-05-25 Created: 2005-05-25 Last updated: 2010-09-29Bibliographically approved

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