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Molecularly imprinted polymer-sol-gel tablet toward micro-solid phase extraction: I. Determination of methadone in human plasma utilizing liquid chromatography-tandem mass spectrometry
Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Environmental Science and Analytical Chemistry.
Number of Authors: 2
2016 (English)In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 936, 116-122 p.Article in journal (Refereed) Published
Abstract [en]

In the present work molecularly imprinted sol-gel tablet (MIP-Tablet) was prepared. The MIP-sol-gel was prepared as a thin layer on polyethylene material in a tablet form. Methadone-d9 was selected as the template and 3-(propylmethacrylate)-trimethoxysilane was used as precursor. MIP-Tablet was applied for micro-solid phase extraction (μ-SPE). The MIP-Tablet was used for the determination of methadone in human plasma samples utilizing liquid chromatography-tandem mass spectrometry; and each tablet could be used twenty times. The extraction time was 10 min while desorption time was 6 min. Factors affecting the extraction efficiency such as desorption solvents, sample pH, salt addition, extraction time, desorption time and adsorption capacity were investigated. The calibration curves were obtained within the range of 5-5000 ng/mL using methadone in human plasma samples. The coefficients of determination (r(2)) values were >= 0.999 for all runs and the extraction recovery was >80%. The accuracy values for quality control samples varied from +3.6 to +9.7% and the inter-day precision (RSD %) values were ranged from 5.0 to 8.0%. The limit of detection was 1.0 ng/mL and the lower limit of quantification was 5 ng/mL utilizing methadone in human plasma samples.

Place, publisher, year, edition, pages
2016. Vol. 936, 116-122 p.
Keyword [en]
molecularly imprinted polymer, sol-gel, tablet, micro-solid phase extraction, methadone, human plasma
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-135000DOI: 10.1016/j.aca.2016.07.001OAI: oai:DiVA.org:su-135000DiVA: diva2:1040858
Available from: 2016-10-29 Created: 2016-10-29 Last updated: 2016-11-15Bibliographically approved
In thesis
1. Novel Microextraction Techniques for Bioanalysis of Neurotransmitters and Biomarkers in Biological Fluids
Open this publication in new window or tab >>Novel Microextraction Techniques for Bioanalysis of Neurotransmitters and Biomarkers in Biological Fluids
2016 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Sample preparation (sample pre-treatment) is the initial step and an essential part in bioanalysis procedure. The main role of sample preparation is to extract and transfer the analyte(s) of interest from a complex matrix to a purified media such as a pure solvent for analysis and quantification. Biological fluids are complex and contain, in addition to the target analyte(s), many different unwanted compounds from salts to proteins. Thus, the analysis of these samples requires an effective sample preparation method prior to the liquid chromatography-mass spectrometry (LC/MS) and gas chromatography-mass spectrometry (GC/MS) assays. The aim of the present work was to evaluate micro-extraction by packed sorbent (MEPS) and develop new sample preparation techniques for the extraction of neurotransmitters and biomarkers from biological samples. Moreover, two new sample preparation techniques were developed. The first developed technique is molecular imprinting on polysulfone membrane (MIPM), and the second one is molecularly imprinted polymer in tablet form (MIPT).

MEPS is a well-known sample preparation technique that can be used online with analytical instruments without any modifications. In this thesis, MEPS was used online with liquid chromatography-tandem mass spectrometry (LC/MS/MS) for the quantification of dopamine and serotonin in human urine samples (Study I) and with GC/MS for the analysis of methadone in humane urine (Study II). Polystyrene polymer and silica-C8 were used as sorbent in Study I and Study II, respectively. In both studies, small sample volumes (50 µL) were used and full method validation was performed. In both studies (I and II), MEPS enhanced the limit of detection (LOD) and reduced the extraction time compared to the previously published methods. In Study I, the mean accuracies of quality control (QC) samples of dopamine and serotonin were 99–101% while the precision values (RSD) were 6–11%. In Study II, the accuracy values of methadone were between 97 and 107% while the precisions (RSD) were between 11 and 15%.

MIP-sol-gel on polysulfone membrane (MIPM) was developed and used in combination with MEPS for the extraction of hippuric acid (HA) in plasma and urine samples (Study III). A good selectivity was obtained using plasma and urine samples. The precision of QC samples in plasma and urine samples were 2.2–4.8% and 1.1–6.7%, respectively. The method recovery was above 90%.

In Study IV, a new technique was developed using a tablet form of molecularly imprinted sol-gel (MIPT) for the extraction of methadone from human plasma samples. Methadone-d9 was selected as the template for accurate recovery, and 3-(propyl methacrylate) trimethoxysilane (3PMTMOS) was used as a precursor. The extraction recovery was higher than 80%. The LOD and LLOQ were 1.0 and 5.0 ng mL-1, respectively. The validation showed good selectivity, accuracy and precision.

In Study I, III and IV, LC/MS/MS system was used while GC/MS was used in Study II for the separation and detection of target analytes.

There will always be a high demand for rapid, selective, reliable and sensitive techniques for sample preparation. It is convenient to use molecular dynamics simulations as a theoretical tool for the optimization of molecularly imprinted system. Suitable monomers and cross-linkers are crucial to synthesize the new membrane and tablet molecular imprinted polymer platforms for all kinds of molecules.

Place, publisher, year, edition, pages
Stockholm: Department of Environmental Science and Analytical Chemistry, Stockholm University, 2016. 55 p.
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-135001 (URN)978-91-7649-581-0 (ISBN)978-91-7649-582-7 (ISBN)
Public defence
2016-12-15, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (English)
Opponent
Supervisors
Available from: 2016-11-22 Created: 2016-10-29 Last updated: 2016-11-17Bibliographically approved

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El-Beqqali, AzizaAbdel-Rehim, Mohamed
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