摘要
建立一种使用多糖衍生物类手性色谱柱拆分N-叔丁氧羰基-3-羟基-1-金刚烷甘氨酸对映体的正相高效液相色谱方法,为实现通过拆分方法制备该化合物单一对映体的过程控制提供依据.采用手性色谱柱Chiralpak ID在正相液相色谱条件下拆分该对映体,通过考察流动相比例、柱温、流速对对映体分离效果的影响,得到最佳拆分条件为:以V(正己烷)∶V(乙醇)=85∶15为流动相,流速0.8mL/min,检测波长220nm,柱温30℃.可使N-叔丁氧羰基-3-羟基-1-金刚烷甘氨酸对映体达到基线分离,分离度达3.72.该方法准确可靠,灵敏度高,重现性好,可用于该对映体的手性拆分.
An immobilized chiral column was used to establish a normal phase HPLC method for the enantiometric separation of racemic N-boc-3-hydroxyadamantylglycine. It provides a basis for the process control of the preparation of monoenantiotropic N-boc-3-hydroxyadamantylglycine by chiral resolution. The chiral separation of enantionmer was achieved by using a Chiralpak ID immobilized chiral column. The mobile phase was consisted of V（n-hexane） ： V（ethanol）= 85 ： 15 at a flow rate of 0.8 mL/min, the column temperature was kept at 30 ℃, and the wavelength was set at 220 nm. The enantionmer resolution was successfully conducted with a resolution value of 3. 72. This method is accurate, reliable, sensitive and available for the enantiometric separation of racemic N-boc-3-hydroxyadamantylglycine.
出处
《浙江工业大学学报》
CAS
北大核心
2015年第3期298-301,共4页
Journal of Zhejiang University of Technology
基金
浙江省省级公益性技术应用研究计划项目(2014C33274)
