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Separation and online preconcentration by multistep stacking with large-volume injection of anabolic steroids by capillary electrokinetic chromatography using charged cyclodextrins and UV-absorption detection

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Authors
Urban, Pawel L.; García Ruiz, CarmenUniversity of Alcalá Author; García González, María ÁngelesUniversity of Alcalá Author; Marina Alegre, María LuisaUniversity of Alcalá Author
Identifiers
Permanent link (URI): http://hdl.handle.net/10017/1364
DOI: 10.1002/jssc.200500113
ISSN: 1615-9314
Publisher
John Wiley & Sons
Date
2005
Affiliation
Universidad de Alcalá. Departamento de Química Analítica e Ingeniería Química
Bibliographic citation
Journal of Separation Science, 2005, v. 28, p. 2200-2209
Keywords
Anabolic steroids
Capillary electrokinetic chromatography
Online multistep stacking
Project
BQU2003-03638 (Ministerio de Ciencia y Tecnología)
RYC-2003-001 (Ministerio de Ciencia y Tecnología)
Document type
info:eu-repo/semantics/article
Version
info:eu-repo/semantics/publishedVersion
Publisher's version
http://dx.doi.org/10.1002/jssc.200500113
Rights
© Wiley, 2005
Access rights
info:eu-repo/semantics/openAccess
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Abstract
The separation of three common anabolic steroids (methyltestosterone, methandrostenolone and testosterone) was performed for the first time by capillary EKC. Different charged CD derivatives and bile salts were tested as dispersed phases in order to achieve the separation. A mixture of 10 mmol/L succinylated-b-CD with 1 mmol/L bCD in a 50 mmol/L borate buffer (pH 9) enabled the separation of the three anabolic steroids in less than 9 min. Concentration LODs, obtained for these compounds with low absorption of UV light, were ~5610–5 mol/L. The use of online reverse migrating sample stacking with large-volume injection (the effective length of the capillary) enabled to improve the detection sensitivity. Sensitivity enhancement factors (SEFs) ranging from 95 (for testosterone) to 149 (for methyltestosterone) were achieved by single stacking preconcentration. Then, the possibilities of multistep stacking to improve the sensitivity for these analytes were investigated. SEFs obtained by double stacking preconcentration ranged from 138 to 185, enabling concentration LODs of 2.79610–7 mol/L (for methyltestosterone), 3.47610–7 mol/L (for testosterone) and 3.56610–7 mol/L (for methandrostenolone). Although online triple stacking preconcentration was achieved, its repeatability was very poor and SEFs for the studied analytes were not calculated.
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