摘要
使用Chiralpak IC(纤维素-三(3,5-二氯苯基氨基甲酸酯)共价键合硅胶)手性柱,建立了采用手性固定相高效液相色谱拆分6种α-芳基萘满酮类衍生物对映体的方法。考察了流动相中有机改性剂的种类和比例、柱温和流速对对映体分离的影响。结果显示6种化合物在异丙醇为改性剂的条件下均可获得较高的对映体分离度。热力学研究表明6种化合物对映体的手性拆分过程均受焓驱动影响,且低温有利于对映体分离。最终推荐分离化合物Ⅰ对映体的流动相是正己烷-异丙醇(90∶10,v/v);分离化合物Ⅱ、Ⅲ、Ⅳ对映体的流动相是正己烷-异丙醇(99∶1,v/v);分离化合物Ⅴ对映体的流动相是正己烷-异丙醇(85∶15,v/v);分离化合物Ⅵ对映体的流动相是正己烷-异丙醇(80∶20,v/v)。柱温为25℃,流速为1.0 mL/min。6种化合物对映体均可在Chiralpak IC手性固定相上得到完全分离,证明该色谱柱对6种化合物具有较高的对映体选择性。
A high performance liquid chromatographic method（ HPLC）was developed for the chiral separation of six α-aryl tetralone derivatives using a Chiralpak IC column. The factors influencing the chiral separation including the type and concentration of organic modifier,col-umn temperature and flow rate were investigated. The results showed that high enantiomeric separation can be obtained with isopropanol as modifier for the six compounds. The thermody-namic study indicated that the enantioseparation was enthalpically driven and showed that low column temperature was beneficial to separation. Complete separation of compound Ⅰ was achieved with a binary solvent mixture of n-hexane-isopropanol（90 ： 10,v / v）as the recom-mended mobile phase. The compounds Ⅱ,Ⅲ and Ⅳ were separated with the mobile phase of the mixture of n-hexane-isopropanol（99 ：1,v / v）and the compound Ⅴ was separated with the mixture of n-hexane-isopropanol（85 ：15,v / v）. The compound Ⅵ was separated with the mix-ture of n-hexane-isopropanol（80 ：20,v / v）. The column temperature was 25 ℃ ,and the flow rate was 1. 0 mL / min. The six tetralone derivative enantiomers were separated on a chiral sta-tionary phase of Chiralpak IC by HPLC. The column has high enantiomeric selectivity to the six tetralone derivative enantiomers.
出处
《色谱》
CAS
CSCD
北大核心
2014年第8期832-836,共5页
Chinese Journal of Chromatography
关键词
纤维素-三(3
5-二氯苯基氨基甲酸酯)
手性固定相
正相高效液相色谱法
萘满酮衍生物
对映体分离
cellulose-tris （ 3,5-dichlorobenzene carbamate）
chiral stationary phase
normalphase-high performance liquid chromatography （NP-HPLC）
tetralone derivatives
enantiomer-ic separation
