On-line coupling of cyclodextrin mediated nonaqueous capillary electrophoresis to mass spectrometry for the determination of salbutamol enantiomers in urine.
The usefulness of the on-line coupling of nonaqueous capillary electrophoresis (NACE) with electrospray ionization (ESI) mass spectrometry (MS) using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD) was demonstrated for the enantioselective determination of low concentrations of salbutamol in human urine. After optimization of several parameters, such as sheath-liquid composition and flow rate, nebulizing gas pressure, CE counter-pressure and position of the CE capillary outlet, a limit of quantification of 18 and 20 ng/ml was obtained for salbutamol enantiomers. Moreover, the relative standard deviation values for repeatability at a concentration of 30 ng/ml were below 7% for both enantiomers. Typical regression lines obtained after application of a simple linear regression model revealed a good relationship between peak area and analyte concentration (with 0.9988 and 0.9966 as coefficients of determination). This paper proposes an easy to use and sensitive NACE-MS method to determine enantiomers of a basic chiral drug in biological fluids preceded by solid-phase extraction as sample cleanup.
Servais
Anne-Catherine
AC
Department of Analytical Pharmaceutical Chemistry, Institute of Pharmacy, University of Liège, CHU, B36, B-4000 Liège 1, Belgium.
Fillet
Marianne
M
Mol
Roelof
R
Somsen
Govert W
GW
Chiap
P
P
de Jong
Gerhardus J
GJ
Crommen
Jacques
J
D000318:Adrenergic beta-Agonists / Q000652:urine*; D000420:Albuterol / Q000652:urine*; D003505:Cyclodextrins / Q000737:chemistry*; D019075:Electrophoresis, Capillary; D006801:Humans; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D009862:Online Systems; D012015:Reference Standards; D015203:Reproducibility of Results; D012984:Software; D012996:Solutions; D013056:Spectrophotometry, Ultraviolet; D013237:Stereoisomerism
D000318:Adrenergic beta-Agonists; D003505:Cyclodextrins; D007202:Indicators and Reagents; D012996:Solutions; D000420:Albuterol