科研之友
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摘要
A precise and sensitive LC method for the determination of roscovitine enantiomeric purity has been developed and validated. Baseline separation with a resolution higher than 5.8 was accomplished within 15 min using a CHIRALPAK AD column (250 x 4.6 mm; particle size 5 mu m) and n-hexane: 2-propanol (80:20 v/v) as mobile phase at a flow rate of 1 mL min(-1). Eluted analytes were monitored by UV detection at 260 nm. The effects of mobile phase components, temperature and flow rate on enantiomeric selectivity and resolution of enantiomers were investigated. Calibration curves were plotted within the concentration range between 0.003 and 1 mg mL(-1) (n = 12), and recoveries between 98.19 and 101.92 % were obtained, with relative standard deviation lower than 1.27 %. LOD and LOQ for roscovitine were 1.15 and 3.85 mu g mL(-1) and for its enantiomer were 1.07 and 3.42 mu g mL(-1), respectively. It was demonstrated that the developed method was accurate, robust and sensitive for the determination of the enantiomeric purity of roscovitine, especially for the analysis of bulk samples.
