Determination of Stereoisomers in Landiolol Hydrochloride by Ultra Performance Convergence Chromatography / 分析化学

ABSTRACT

A new method for chiral separation and purity inspection of landiolol hydrochloride and its stereoisomers was developed by ultra-performance convergence chromatography ( UPC2 ) . The mobile phase was the mixture of supercritical CO2 and methanol/n-butyl alcohol/acetonitrile (111, V/V) plus 0. 5%NH3?H2O. The separation was carried out on the Daicel CHIRALPAK? IF column (150 mm × 4. 6 mm, 3 μm) with a flow rate of 2. 8 mL/min at 50℃ using 223 nm as detection wavelength. Under the optimized experimental conditions, for R,R-stereoisomer, R,S-stereoisomer and S,R-stereoisomer, the detection limits (LOD, S/N=3) were 0. 3, 0. 4 and 0. 3 mg/L, the linear ranges were 2-300 mg/L, 5-300 mg/L and 2-300 mg/L, the recoveries of spike samples were 103. 4%±2. 5%, 91. 8%±2. 5% and 101. 7%±1. 5%, and the injection repeatabilities were 0. 06%, 0. 09% and 0. 08% (n=6), respectively. The experimental results demonstrate that the UPC2-based method can be used for the analysis and determination of landiolol hydrochloride and its stereoisomers.