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目的:建立阿雷地平对映异构体高效液相色谱手性拆分方法,用于S构型阿雷地平光学纯度的分析测定。方法:采用硅胶表面涂敷有纤维素-三(4-甲基苯甲酸酯)填料(Chiralcel OJ-H)为固定相,以正己烷-乙醇(75∶25)为流动相,流速1.0 m L·min~(-1),检测波长238 nm,柱温35℃。结果:S-阿雷地平与R-阿雷地平之间的分离度为3.5;R-阿雷地平质量浓度在0.04~2.0μg·m L~(-1)范围内线性关系良好,线性方程为A=61 971C-0.321 4,r=0.999 9;R-阿雷地平的定量限和检测限分别为0.8 ng和0.3 ng;低、中、高3个浓度的R-阿雷地平回收率(n=3)分别为97.5%、98.5%、99.8%,RSD(n=9)为1.5%;供试品溶液在避光条件下室温放置12 h内稳定性良好。经检测,S-阿雷地平中R-阿雷地平的含量为0.08%。结论:所建立的方法经方法验证可用于分离和测定S-阿雷地平中的R-阿雷地平。
OBJECTIVE: To establish a chiral resolution method for the determination of isradipine enantiomers by high performance liquid chromatography (HPLC), and to determine the optical purity of isoform of S configuration. METHODS: Chiralcel OJ-H was used as the stationary phase on a silica gel surface and n-hexane-ethanol (75:25) was used as the mobile phase at a flow rate of 1.0 m L · min ~ (-1). The detection wavelength was 238 nm and the column temperature was 35 ℃. Results: The separation between S-isradipine and R-Areradipine was 3.5. The linear range of R-Areradipine was within the range of 0.04-2.0 μg · m L -1 with a linear equation of A = 61 971C-0.321 4, r = 0.999 9; The limits of quantitation and detection limits of R-Areradipine were 0.8 ng and 0.3 ng, respectively; The recoveries of R-Areradipine at low, middle and high concentrations = 3) were 97.5%, 98.5% and 99.8%, respectively, and the RSD (n = 9) was 1.5%. The stability of the test solution was good within 12 hours at room temperature in dark conditions. After testing, S-Areradipine R-Areradipine content of 0.08%. Conclusion: The established method was validated by the method and could be used for the isolation and determination of R-Areradipine in S-Areradipine.