RT info:eu-repo/semantics/article
T1 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
A1 Urban, Pawel L.
A1 García Ruiz, Carmen
A1 García González, María Ángeles
A1 Marina Alegre, María Luisa
K1 Anabolic steroids
K1 Capillary electrokinetic chromatography
K1 Online multistep stacking
K1 Ciencia
K1 Química analítica e industrial
K1 Science
K1 Chemistry, analytic and technical
AB 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.
PB John Wiley & Sons
SN 1615-9314
YR 2005
FD 2005
LK http://hdl.handle.net/10017/1364
UL http://hdl.handle.net/10017/1364
LA eng
NO Ministerio de Ciencia y Tecnología
DS MINDS@UW
RD 24-abr-2024