RESUMEN
A fully automated sugaring-out assisted liquid-liquid extraction procedure was suggested. The procedure was based on the separation of the acetonitrile phase, containing a target analyte from the homogeneous sample solution after injection of sugaring-out reagent (glucose) into a mixing chamber of the flow system. Air bubbling was used to promote the extraction process and phase separation. After the fast phase separation in the mixing chamber, the acetonitrile phase containing the target analyte was transferred to an HPLC-UV system. Under the optimal conditions, the detector response of procainamide was linear in the concentration range of 6×10-7-4×10-5molL-1. The limit of detection, calculated from a blank test based on 3σ, was 2×10-7molL-1. The proposed method was successfully applied for the determination of procainamide in human urine samples and the analytical results agreed fairly well with the results obtained by reference CE method.
Asunto(s)
Acetonitrilos/química , Automatización , Cromatografía Líquida de Alta Presión/métodos , Glucosa/química , Extracción Líquido-Líquido/métodos , Procainamida/orina , Adolescente , Adulto , Femenino , Voluntarios Sanos , Humanos , Límite de Detección , Masculino , Rayos Ultravioleta , Adulto JovenRESUMEN
Fast isotopic separation of 10 B and 11 B boric acid by CZE was demonstrated. The BGE contained 25 mM phenylalanine and 5 mM putrescine (ÑÐ 8.95). The running conditions were +25 kV at 20°C with indirect photometric detection at 210 nm. Baseline separation was achieved in less than 9 min. RSD of migration times and corrected peak areas were less than 0.5 and 3%, respectively (n = 5). Linearity was demonstrated in the range 0.2-2 mM for 11 B and 0.2-0.5 mM for 10 B.
Asunto(s)
Ácidos Bóricos/química , Ácidos Bóricos/aislamiento & purificación , Electroforesis Capilar/métodos , Ácidos Bóricos/análisis , Concentración de Iones de Hidrógeno , Isótopos/análisis , Isótopos/química , Isótopos/aislamiento & purificación , Límite de Detección , Modelos Lineales , Reproducibilidad de los ResultadosRESUMEN
Separation of (6)Li and (7)Li isotopes by CZE was demonstrated. The BGE contained 5 mM 4-aminopyridine, 0.9 mM oxalic acid, 0.25 mM CTAB, and 0.25% w/v Tween 20 (ÑÐ = 9.2). The running conditions were +25 kV at 30°C with indirect photometric detection at 261 nm. Under optimal experimental conditions, the analysis time was less than 21 min. Separation of Li preparations with mole fraction of (6)Li ranging from 3.44 up to 90.38% was demonstrated.