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作 者:唐晓丹[1] 王绍艳[2] 王智超[2] 张伟[1]
机构地区:[1]辽宁科技大学分离技术中心,辽宁鞍山114051 [2]辽宁科技大学化学工程学院,辽宁鞍山114051
出 处:《分析测试学报》2011年第1期34-37,42,共5页Journal of Instrumental Analysis
基 金:辽宁省教育厅创新团队项目(2008T093)
摘 要:在Chiralcel OJ手性柱上对苯磺酸氨氯地平对映体进行分离研究。考察了在正己烷流动相体系中,不同碳数、不同立体结构的醇类添加剂以及不同醇含量对分离结果的影响,同时还考察了流速及柱温对分离的影响。并通过色谱保留及热力学行为研究对药物手性识别机理进行了探讨。结果表明,在正己烷-异丙醇(90∶10,体积比)为流动相,流速0.4 mL/min,柱温20℃的条件下,苯磺酸氨氯地平对映体可获得基线分离,分离度Rs=3.228。在一定的温度范围内,用lnα对1/T作图,得到的Van′t Hoff曲线具有良好的线性,计算了苯磺酸氨氯地平对映体在色谱柱上分离的焓变和熵变差值、转折温度点Tiso等热力学参数。分离对映体满足‖ΔΔH0‖>‖ΔΔS0‖,说明手性拆分过程为焓驱动。Enantioseparation of amlodipine besylate on Chiralcel OJ chiral column was studied. The influences of different carbon number, alcohol modifier types with different three-dimensional structures and concentrations, flow rate and column temperature on the enantioseparation of amlodipine besylate were investigated. And the ehiral recognition mechanism for amlodipine was discussed by the chromatographic retention and thermodynamic parameters. A good baseline resolution was obtained for the separation of amlodipine besylate using hexaneisopropanol(90 : 10, by volume) as mobile phase with flow rate of 0. 4 mL/min and column temperature of 20℃. The resolution of amlodipine was up to 3. 228. In the experimental temperature range, Van't Hoff curve with a good linearity was acquired by ploting lnα to 1/T. The enthalpy change difference, entropy change difference and Tiso of the enantioseparation on chiral column were calculated. The enantioseparation meeting the requirements of ||△△H0||〉||△△S0|| showed that the process of chiral separation was an enthalpy-controlled process.
关 键 词:CHIRALCEL OJ柱 苯磺酸氨氯地平对映体 色谱保留 手性拆分
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