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On-line clean-up and determination of tramadol in human plasma and urine samples using molecularly imprinted monolithic column coupling with HPLC
Amirkabir University of Technology, Tehran, Iran.
Amirkabir University of Technology, Tehran, Iran.
Ministry of Health and Medical Education, Tehran, Iran.
2012 (English)In: Journal of chromatography. B, ISSN 1570-0232, E-ISSN 1873-376X, Vol. 911, no 12, 49-54 p.Article in journal (Refereed) Published
Abstract [en]

The applicability of an on-line solid phase extraction method using molecularly imprinted monolithic column was developed for the assay of tramadol (TRD) in urine and plasma samples. The monolithic column was prepared by using TRD as the template, methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker and chloroform as the porogen with in situ molecular imprinting polymerization technique. Various parameters affecting the extraction efficiency of the monolithic column were evaluated. Chromatographic analysis of TRD after on-line clean-up of samples was performed by reversed-phase HPLC on an ACE column with ultraviolet detection at 218 nm. The present work was successfully applied for automated simple analysis of TRD in urine and plasma samples with high recoveries between 90.5–93.1% and 93.3–96.0%, respectively. The results revealed that in concentration up to 500 ng/mL of dextromethorphan (DEX), timolol (TMO) and O-desmethyltramadol (M1), the recoveries were not reduced more than 4.3% and 4.0% for plasma and urine samples, respectively. The limit of detection (S/N = 3) and limit of quantification (S/N = 10) for TRD in urine samples were 0.03 ng/mL and 0.10 ng/mL, and in plasma samples were 0.3 and 1.0 ng/mL, respectively. Inter-column precision of the assays (n = 3) for urine and plasma samples at the 100 ng/mL TRD level were 4.0% and 4.2%, respectively.

Place, publisher, year, edition, pages
2012. Vol. 911, no 12, 49-54 p.
Keyword [en]
Molecularly imprinted polymer, Tramadol, Human Plasma, Monolithic column, Sample clean-up
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-103356DOI: 10.1016/j.jchromb.2012.10.019OAI: oai:DiVA.org:su-103356DiVA: diva2:716773
Available from: 2014-05-12 Created: 2014-05-12 Last updated: 2017-12-05Bibliographically approved
In thesis
1. Towards more selective sorbents for extraction of drugs and biomarkers from biological fluids using molecularly imprinted polymers
Open this publication in new window or tab >>Towards more selective sorbents for extraction of drugs and biomarkers from biological fluids using molecularly imprinted polymers
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Sample preparation has a critical role as a first step in analytical processes, especially in bioanalysis and environmental analysis. A good sample preparation technique should be robust and stable, regardless of the sample matrix.

The aim of this thesis is to design and synthesize molecularly imprinted polymers that can be used in various sample preparation techniques, such as on-line MEPS, on-line SPE and on-line monolithic pre-columns used for the extraction of drugs, hormones, and cancer biomarkers from human plasma and urine samples. Additional aim was to provide full automation, on-line coupling, short sample preparation time and high-throughput.

In this thesis MIP in MEPS was used on-line with liquid chromatography-tandem mass spectrometry (LC/MS/MS) for the determination of sarcosine in human urine and plasma samples. The method was fully automated and the packed sorbent could be used for about hundred extractions. In additional work a coated needle with MIP-Sol-Gel as thin layer was prepared and used for the microextraction of bilirubin from human plasma and urine. Small sample volumes could be handled and the validation of the method showed that the method was robust and selective.

In a further work MIP-SPE on-line with HPLC was used for the extraction and determination of dextromethorphan in human plasma samples. MIP-SPE showed a good selectivity and high recovery (87% - 92%). On-line MIP monolithic pre-column was prepared and used in a coupled system for the extraction of tramadol in human plasma and urine samples. The MIP monolithic pre-column showed good selectivity and high extraction recovery was obtained (91-96%). The extraction and analysis of human insulin in plasma and pharmaceutical formulation solutions were carried out using MIP-SPE on-line with HPLC. The validation of the method showed that the method was accurate and robust.

Place, publisher, year, edition, pages
Stockholm: Department of Analytical Chemistry, Stockholm University, 2014. 77 p.
Keyword
molecularly imprinted polymer, sol-gel, solid phase extraction, microextraction by packed sorbent, monolithic column
National Category
Chemical Sciences
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-103379 (URN)978-91-7447-904-1 (ISBN)
Public defence
2014-06-12, G-salen, Arrheniuslaboratorierna, Svante Arrhenius väg 20 C, Stockholm, 13:00 (English)
Opponent
Supervisors
Note

At the time of the doctoral defense, the following paper was unpublished and had a status as follows: Paper 5: Submitted.

Available from: 2014-05-22 Created: 2014-05-13 Last updated: 2014-05-20Bibliographically approved

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