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作 者:沈报春[1,2] 袁建勇[3] 王恒春[1] 徐贝佳[2] 徐秀珠[2]
机构地区:[1]昆明医学院药学院,昆明650031 [2]浙江大学化学系,杭州310027 [3]浙江医药股份有限公司新昌制药厂,新昌312500
出 处:《理化检验(化学分册)》2008年第11期1017-1020,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:云南省自然科学基金(2007B220M)资助项目
摘 要:在直链淀粉手性固定相(Chiralpak AD)上分离了二茂铁衍生物3-(1-N,N-二甲基)乙基二茂铁的对映体。考察了醇类添加剂种类和浓度、碱的浓度对对映体分离的影响,同时探讨了手性识别机理。结果发现:乙醇是最佳醇类添加剂,并且在流动相中加入少量碱有助于改善峰形,增加分离度。通过改变温度求出相应的拆分过程中热力学参数,这些参数表明在所研究温度范围内,Chiralpak AD对该溶质的分离过程为焓控过程,高温对分离不利。Enantiomers of a ferrocenyl derivative, i.e. 3-(1-N, N-dimethyl) ethyl ferrocene, were separated on the Chiralpak AD column (250 mm×4 mm, 5 μm). Factors influential to the separation, including kinds and concentration of alcohol as denaturant added to the mobile phase and concentration of base in the mobile phase, were studied, and the mechanism of recognition of chirality was discussed. It was found that ethanol was the best additive, and that addition of small amount of triethylamine was profitable to improve the peak shape and rate of separation. By changing the temperature during the separation process, relative thermodynamic parameters were found, which indicated that within the range of temperatures studied, an enthalpy control process of Chiralpak AD against the separation of the solute was observed. Too high a temperature was unfavourable.
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