Enantioselective determination of R- and S-(alpha-bromoisovaleryl)urea in plasma using high-performance liquid chromatography after solid-phase extraction
| Autor: | Gerard J. Mulder, U.R. Tjaden, Vicki Venizelos, H. Irth, J. van der Greef, Douwe D. Breimer, T. M. T. Mulders |
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| Rok vydání: | 1992 |
| Předmět: |
Analyte
Chromatography Chemistry Extraction (chemistry) Reproducibility of Results Stereoisomerism General Chemistry Repeatability Amberlite Hydrogen-Ion Concentration High-performance liquid chromatography Matrix (chemical analysis) chemistry.chemical_compound Urea Humans Spectrophotometry Ultraviolet Solid phase extraction Bromisovalum Saliva Chromatography High Pressure Liquid |
| Zdroj: | Journal of chromatography. 573(2) |
| Popis: | A stereoselective method has been developed for the determination of R- and S-(alpha-bromoisovaleryl)urea in plasma and saliva after oral administration. The chiral separation was carried out on Chiralcel OJ or OD columns with hexane--2-propanol as the mobile phase. The poor detection properties of the analyte required the development of an effective sample pretreatment procedure to enable ultraviolet detection at 210 nm. Solid-phase extraction using hydrophobic Amberlite XAD-2 in combination with washing steps at alkaline and acidic pH completely removed interfering components of the biological matrix and allowed the detection of the optical isomers at concentrations down to 10 ng/ml (0.05 microM). The method was validated by determining the recovery, linearity, accuracy and within-day and between-day repeatability at 50, 200 and 2000 ng/ml. Application to the analysis of plasma and saliva samples is demonstrated. |
| Databáze: | OpenAIRE |
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