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Rapid on-line extraction and quantification of escitalopram from urine using sol-gel columns and mass spectrometric detection
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
2007 (English)In: Journal of Pharmaceutical and Biomedical Analysis, ISSN 0731-7085, E-ISSN 1873-264X, Vol. 43, no 3, 1045-1048 p.Article in journal (Refereed) Published
Abstract [en]

A fast and easy way to quantify escitalopram in urine has been developed. A capillary with a silica based monolithic bed inside is used to extract escitalopram from urine and the for mass spectrometry detrimental matrix is washed away by applied pressure. The analyte is eluted by a solution containing organic modifier and directly electrosprayed into a time-of-flight mass spectrometer, ESI-TOF-MS. This method makes it possible to load large volumes of sample onto the column and preconcentrate escitalopram on-line before detection. Standard addition of escitalopram to the urine sample gave a linear calibration curve (R2 = 0.988). The analyzed sample was found to contain an escitalopram concentration of 0.62 ng/ml, well in line with earlier publications. The calculated LOD was 10 pg/ml and LOQ was 34 pg/ml as compared to earlier reports with a LLOQ of 1 ng/ml. The intra day variation of the escitalopram peak area is less than 6.3%.

Place, publisher, year, edition, pages
2007. Vol. 43, no 3, 1045-1048 p.
Keyword [en]
Escitalopram, ESI-TOF-MS, On-line, Sample cleanup, Sol-gel, Urine
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:uu:diva-94822DOI: 10.1016/j.jpba.2006.09.008ISI: 000244623000035PubMedID: 17081717OAI: oai:DiVA.org:uu-94822DiVA: diva2:168813
Available from: 2006-09-15 Created: 2006-09-15 Last updated: 2011-03-29Bibliographically approved
In thesis
1. Column Development in Capillary Electrophoresis and Electrochromatography for Bioanalytical Applications
Open this publication in new window or tab >>Column Development in Capillary Electrophoresis and Electrochromatography for Bioanalytical Applications
2006 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Analysis of biological samples can be a difficult task. This thesis covers a broad aspect of the analytical areas of capillary electrophoresis (CE) and capillary electrochromatography (CEC) in combination with mass spectrometry (MS) that are of great importance for achieving fast, accurate and sensitive bioanalyses. A significantly time reduced and automated system for sample cleanup was developed to greatly simplify the pretreatment process of biological samples with a complex matrix. Desalting and preconcentration of species in urine was conducted and the limit of detection for the antidepressant escitalopram was lowered 10 times. This extraction devise was also successfully incorporated in a chip based platform for the possibility to be a part of multidimensional separation systems. The reduced risk of sample loss leads to improved detection limits, which are usually one the most challenging parts when working with bioanalyses.

In the area of separation, a monomer surface with tailored hydrophobicity was developed to achieve rapid, high efficient separations of complex mixtures. Within five minutes a tryptic digest of a protein could be separated and then identified by a Mascot search.

The applications addressed have been focused on medical conditions which are of highest interest for both physicians and patients. A high throughput analysis of the kynurenine metabolites with CE-MS offers a new method to rapidly examine samples from patients with neurological disorders.

A screening study of possible biomarkers for the two different types of appendicitis, gangraenous and phlegmonous was conducted. Indicative patterns were found for both pre and post surgery of the two types of inflammation as well as between them. The divergences were traced back to the MS peaks obtained in the CE- and CEC-MS setups as possible biomarkers for the two forms of appendicitis. A preliminary study of polycystic ovary syndrome also offered some valuable results for future biomarker identification.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2006. 54 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 216
Keyword
Analytical chemistry, Capillary electrophoresis (CE), Capillary electrochromatography (CEC), Mass spectrometry (MS), Bioanalysis, Sample pretreatment, Sol-gel, Analytisk kemi
National Category
Chemical Sciences
Identifiers
urn:nbn:se:uu:diva-7124 (URN)91-554-6644-3 (ISBN)
Public defence
2006-10-06, B22, BMC, Uppsala, 10:15 (English)
Opponent
Supervisors
Available from: 2006-09-15 Created: 2006-09-15 Last updated: 2012-02-08Bibliographically approved

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