Recent Extraction Techniques with Emphasis on Supercritical Fluid Extraction and Microwave-assisted Extraction

Cecilia Sparr Eskilsson

Research output: ThesisDoctoral Thesis (compilation)

Abstract

Today’s requirements of fast, reliable and selective analytical methods with minimal usage of organic solvents have accelerated the development of new, automated extraction techniques. In this thesis recent extraction techniques with emphasis on supercritical fluid extraction (SFE) and microwave-assisted extraction (MAE) were investigated. Different environmental and industrial applications such as extraction of pesticides from process dust, active compounds in pharmaceutical tablets, mycotoxins in cereals and aromatic amines released from azo dyes in leather have been studied to outline advantages and limitations of the techniques. In all cases the extraction efficiencies were similar or better, solvent usage reduced and extraction times shortened compared to traditional extraction techniques such as sonication and liquid-solid extraction (shaking) procedures. Even though recent extraction techniques in most cases are superior to the conventional techniques, they differ in terms of selectivity, simplicity and sample throughput as discussed in this thesis. By utilizing an elongated trap in SFE further selectivity in the collection step was achieved for extractions of aromatic amines and for separation of fat-soluble vitamins from lipids. Devices to perform direct SFE of liquid samples were tested, resulting in a selective extraction of alkylphenols from real waste water samples. Furthermore, a fractionated MAE procedure including a reaction/extraction step was developed for the determination of amines after reductive cleavage of azo dyes in leather. A variant of pressurized liquid extraction (PLE) that utilizes water as extracting media is pressurized hot water extraction (PHWE). This technique was investigated for extraction of pesticides from process dust and obtained results were compared with results obtained using SFE. With better understanding of the characteristics of the recent techniques, conventional techniques can in most cases be replaced. In the future it is anticipated that combinations of different extraction techniques will appear in a single analytical method, where the inherent advantages of each technique are utilized. This was here demonstrated , where leather samples were degreased using SFE and further treated using MAE.
Original languageEnglish
QualificationDoctor
Awarding Institution
  • Centre for Analysis and Synthesis
Supervisors/Advisors
  • [unknown], [unknown], Supervisor, External person
Award date2003 May 3
Publisher
ISBN (Print)91-628-5626-X
Publication statusPublished - 2003

Bibliographical note

Defence details

Date: 2003-05-03
Time: 10:15
Place: Hall B at Center for Chemistry and Chemical Engineering, Lund

External reviewer(s)

Name: Chester, Thomas L.
Title: Dr
Affiliation: The Procter & Gamble Company, Miami Valley Laboratories, Cincinnati, USA

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Article: 1. Supercritical fluid extraction of the pesticides carbosulfan and imidacloprid from process dust wasteC. Sparr Eskilsson, L. MathiassonJournal of Agricultural and Food Chemistry 2000, 48, 5159-5164.

Article: 2. Inherent possibilities of improving recovery and selectivity using a long solid phase trap in analytical supercritical fluid extractionC. Sparr Eskilsson, C. Turner, A. Esbjörnsson, L. MathiassonJournal of Separation Science 2001, 24, 297-303.

Article: 3. Direct supercritical fluid extraction of alkylphenols from spiked and waste water samples using extraction cells equipped with hydrophobic membrane-assembliesC. Sparr Eskilsson, A. Ågren, E. Björklund, L. Mathiassonmanuscript

Article: 4. Microwave-assisted extraction of felodipine tabletsC. Sparr Eskilsson, E. Björklund, L. Mathiasson, L. Karlsson, A. TorstenssonJournal of Chromatography A 1999, 840, 59-70.

Article: 5. Microwave-assisted extraction of zearalenone from wheat and cornL. Pallaroni, C. von Holst, C. Sparr Eskilsson, E. BjörklundAnalytical and Bioanalytical Chemistry 2002, 374, 161-166.

Article: 6. Harmful azo colorants in leather. Determination based on their cleavage and extraction of corresponding carcinogenic aromatic amines using modern extraction techniquesC. Sparr Eskilsson, R. Davidsson, L. MathiassonJournal of Chromatography A 2002, 955, 215-227.

Article: 7. Pressurized hot water extraction of insecticides from process dust. Comparison with supercritical fluid extractionC. Sparr Eskilsson, K. Hartonen, L. Mathiasson, M.-L. Riekkolasubmitted to Journal of Separation Science in February 2003.

Article: Appendix:

Article: 8. Collection in analytical-scale supercritical fluid extractionC. Turner, C. Sparr Eskilsson, E. BjörklundJournal of Chromatography A 2002, 947, 1-22.

Article: 9. Analytical scale microwave-assisted extractionC. Sparr Eskilsson, E. BjörklundJournal of Chromatography A 2000, 902, 227-250.


The information about affiliations in this record was updated in December 2015.
The record was previously connected to the following departments: Analytical Chemistry (S/LTH) (011001004)

Subject classification (UKÄ)

  • Analytical Chemistry

Free keywords

  • Analytisk kemi
  • Analytical chemistry
  • Pressurized hot water extraction
  • Pressurized liquid extraction
  • Microwave-assisted extraction
  • Recent extraction techniques
  • Supercritical fluid extraction

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