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Dynamic hollow-fibre liquid phase microextraction of dinitrophenols from human plasma: Optimization of an extraction flow system using experimental design methodology
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.
2009 (English)In: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 79, no 3, 633-638 p.Article in journal (Refereed) Published
Abstract [en]

The utility of a dynamic hollow-fibre liquid phase microextraction method (optimized using a four-variable experimental design and response surface modelling) for extracting dinitrophenolic compounds from human plasma samples was evaluated. The investigated variables were donor phase salt concentration (10–400 mM), donor phase pH (2–6), acceptor phase pH (7–12), and donor/acceptor phase flow rates (30/7.5 to 70/17.5 μL min−1). Four dinitrophenol pesticides were used as model substances at concentrations of 0.1 μg mL−1 in spiked human plasma samples. Extraction efficiencies ranging from 42 to 77% with RSDs below 9 were achieved with the optimized method. The flow rate and acceptor pH were shown to strongly affect the extraction efficiency for all compounds, while the donor phase pH and salt concentration had minor effects. With a well-defined acceptor phase pH and flow rate the system exhibited high robustness. The limits of quantification for the investigated compounds, using the presented extraction method followed by liquid chromatography/electrospray ionization mass spectrometry in selected ion monitoring mode, ranged from 0.05 to 0.1 μg mL−1 plasma.

Place, publisher, year, edition, pages
Elsevier , 2009. Vol. 79, no 3, 633-638 p.
Keyword [en]
Supported liquid membrane; Hollow-fibre liquid phase microextraction; Nitrophenols; Human blood plasma; Optimization
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-34670DOI: 10.1016/j.talanta.2009.04.051ISI: 000268346800012OAI: oai:DiVA.org:su-34670DiVA: diva2:285262
Available from: 2010-01-11 Created: 2010-01-11 Last updated: 2017-12-12Bibliographically 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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