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Dynamic hollow-fibre liquid phase microextraction for human plasma samples automated by sequential injection analysis
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
(English)Manuscript (preprint) (Other academic)
Abstract [en]

This paper presents an easily handled, hollow-fibre liquid phase microextraction (HF-LPME) sample clean-up method, automated by the use of a programmable sequential injection analysis (SIA) system. Use of a SIA system significantly reduces the need for manual sample handling. This new type of clean-up system was assessed and compared with manual HF-LPME for the extraction of acidic compounds (dinitrophenols) from human plasma, in terms of human intervention requirements, efficiency, repeatability and carry-over. Its application to a SIA system for basic compounds (b-blockers) is also presented. The sample aliquots collected off-line from the SIA system were subsequently subjected to separation with LC and the various analytes were detected with ESI-MS.

Extraction efficiency values between 28 and 56% (RSD 5-10%, n = 7) were achieved for the dinitrophenol compounds after an extraction cycle of 58 min including a 30 min washing step. According to the MS analysis the SIA/HF-LPME method yielded clean chromatograms with no detectable interfering peaks. Ion suppression in positive ESI-MS was between 4 and 21% when tested on extracts with b-blockers.

National Category
Other Basic Medicine
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-40984OAI: oai:DiVA.org:su-40984DiVA: diva2:327651
Available from: 2010-06-30 Created: 2010-06-30 Last updated: 2010-08-10Bibliographically approved
In thesis
1. A Novel Miniaturised Dynamic Hollow-Fibre Liquid-Phase Micro-Extraction Method for Xenobiotics in Human Plasma Samples
Open this publication in new window or tab >>A Novel Miniaturised Dynamic Hollow-Fibre Liquid-Phase Micro-Extraction Method for Xenobiotics in Human Plasma Samples
2010 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Bioanalytical chemistry is a challenging field, often involving complex samples, such as blood, plasma, serum or urine. In many applications, sample cleanup is the most demanding and time-consuming step.

In the work underlying this thesis a novel dynamic miniature extractor, known as a hollow-fibre liquid-phase microextractor (HF-LPME), was designed, evaluated and studied closely when used to clean plasma samples. Aqueous-organic-aqueous liquid extraction, in which the organic liquid is immobilised in a porous polypropylene membrane, was the principle upon which the extractor was based, and this is discussed in all the papers associated with this thesis. This type of extraction is known as supported-liquid membrane extraction (SLM). The aim of this work was the development of a dynamic system for SLM. It was essential that the system could handle small sample volumes and had the potential for hyphenations and on-line connections to, for instance, LC/electrospray-MS. The design of a miniaturised HF-LPME device is presented in Paper I. The extraction method was developed for some weakly acidic pesticides and these were also used for evaluation. In the work described in Paper II, the method was optimised on the basis of an experimental design using spiked human plasma samples. Paper III presents a detailed study of the mass-transfer over the liquid membrane. The diffusion through the membrane pores was illustrated by a computer-simulation. Not surprisingly, the more lipophilic, the greater the retention of the compounds, as a result of dispersive forces. The main focus of the work described in Paper IV was to make the HF/LPME system more versatile and user-friendly; therefore, the extractor was automated by hyphenation to a SIA system.

Place, publisher, year, edition, pages
Stockholm: Department of Analytical Chemistry, Stockholm University, 2010. 97 p.
Keyword
sample clean-up, human blood plasma, hollow-fibre liquid phase microextraction, supported liquid membrane extraction, SLM, HF-LPME, sample preparation, bioanalysis, liquid-liquid extraction
National Category
Other Basic Medicine
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-41742 (URN)978-91-7447-128-1 (ISBN)
Public defence
2010-09-29, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (Swedish)
Opponent
Supervisors
Note
At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 4: Manuscript. Available from: 2010-09-07 Created: 2010-08-05 Last updated: 2011-05-02Bibliographically approved

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