Determination of Fat-Soluble Vitamins in Foods Based on Supercritical Fluid Extraction

Research output: ThesisDoctoral Thesis (compilation)


Sample clean-up methodologies based on supercritical fluid extraction (SFE) have been developed for determination of fat-soluble vitamins in foods. This thesis focuses on method development, stressing important issues concerning sample pre-treatment, extraction conditions and collection parameters. It was demonstrated that by using SFE followed by saponification and determination using RP-HPLC with UV and fluorescence detection, quantitative recoveries of vitamins A, E and b-carotene could be obtained in milk, milk powder, minced meat, liver paste, infant formula and canned baby food. The importance of modifying the sample matrix by adding an ethanolic entrainer prior to extraction was stressed. It was also shown that careful optimisation of the collection parameters is essential to accurately determine the vitamins. When solvent collection was employed, the type of solvent had an especially significant impact on the collection efficiency.

In the work reported in this thesis, the possibility of replacing the rather harsh saponification step with on-line enzymatic hydrolysis using lipases was also investigated. Important parameters such as water content, temperature and extraction pressure were examined using several lipases and one esterase. It was shown that immobilised lipase from Candida antarctica type B was superior in terms of activity and operational stability. This on-line extraction/reaction methodology resulted in 100% conversion of retinyl palmitate to retinol (vitamin A), samples sufficiently clean for direct vitamin determination, and quantitative recoveries of vitamins A and E. Moreover, the methodology was fully automated and consumed much smaller amounts of organic solvents than conventional extraction methodologies.

Instead of trying to obtain all the selectivity in the extraction step, work has also been done on using a solid phase trap in the collection step for selectivity enhancement. With a longer trap than is normally used in this type of equipment, it was found that the collection capacity of condensed modifier and coextracted fat was increased, thereby allowing the use of a lower trap temperature without risking analyte breakthrough losses. It was also shown that fat-soluble vitamins A, D and E could be fully fractionated from triacylglycerols in rapeseed oil during the elution step. This methodology was employed for the determination of tocopherols in rapeseed and fish liver oil.
Original languageEnglish
Awarding Institution
  • Centre for Analysis and Synthesis
  • [unknown], [unknown], Supervisor, External person
Award date2001 Jan 26
ISBN (Print)91-7874-107-6
Publication statusPublished - 2000

Bibliographical note

Defence details

Date: 2001-01-26
Time: 10:15
Place: Lecture Hall B at the Chemical Center

External reviewer(s)

Name: Clifford, Anthony A.
Title: Prof
Affiliation: School of Chemistry, University of Leeds, Leeds LS2 9JT, UK


Article: Paper I:Determination of vitamins A and E in milk powder using supercritical fluid extraction for sample clean-upC. Turner and L. MathiassonJournal of Chromatography A, 2000, 874, 275-283

Article: Paper II:Determination of food constituents based on SFE: applications to vitamins A and E in meat and milk.H. Berg, C. Turner, L. Dahlberg and L. MathiassonJournal of Biochemical and Biophysical Methods, 2000, 43, 391-401

Article: Paper III:Development of methods for the determination of vitamin A, E and b-carotene in food formulae based on supercritical fluid extraction (SFE) for sample work-upL. Mathiasson, C. Turner, H. Berg, L. Dahlberg, E. Anklam, A. Theobald, M. Sharman, R. Ginn, F. Ulberth and R. GabernigThe Analyst, 2000, submitted

Article: Paper IV:On-line SFE/enzymatic hydrolysis of vitamin A esters -A new simplified approach for the determination of vitamin A and E in foodC. Turner, J. W. King and L. MathiassonJournal of Agricultural and Food Chemistry, 2000, accepted

Article: Paper V:Lipase-catalyzed reactions in organic and supercritical solvents: application to fat-soluble vitamin determination in milk powder and infant formulaC. Turner, M. Persson, L. Mathiasson, P. Adlercreutz and J. W. KingEnzyme and Microbial Technology, 2000, submitted

Article: Paper VI:Inherent possibilities of improving recovery and selectivity using a long solid phase trap in analytical supercritical fluid extractionC. Sparr Eskilsson, C. Turner, A. Esbjörnsson and L. MathiassonJournal of Separation Science, 2000, submitted

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), Department of Chemistry (011001220)

Subject classification (UKÄ)

  • Analytical Chemistry

Free keywords

  • Supercritical fluid extraction
  • Solvent collection
  • Solid phase trapping
  • SFE
  • Selectivity
  • Retinol
  • Milk powder
  • Lipase
  • Food
  • Enzymatic hydrolysis
  • Alcoholysis
  • Candida antarctica
  • Tocopherol
  • Vitamins
  • Analytical chemistry
  • Analytisk kemi


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