2-氧杂双环［3,3,0］辛-6-烯-3-酮对映异构体手性拆分及光学纯度的测定

吉林大学学报(理学版) ›› 2019, Vol. 57 ›› Issue (06): 1530-1534.

2-氧杂双环［3,3,0］辛-6-烯-3-酮对映异构体手性拆分及光学纯度的测定

曹宏^1,2, 王淑红³, 赵春影³, 胡川闽¹, 蔡建辉¹, 修志明¹

1. 吉林医药学院吉林省抗体工程科技协同创新中心, 吉林吉林 132013；2. 吉林大学中日联谊医院, 长春 130021； 3. 长春百纯和成医药科技有限公司, 长春 130012

收稿日期:2019-08-02 出版日期:2019-11-26 发布日期:2019-11-21
通讯作者: 修志明 E-mail:Xiuzm10@mails.jlu.edu.cn

Chiral Separation of Enantiomer of 2-Oxabicyclo［3,3,0］oct-6-en-3-oneand Determination of Optical Purity#br#

CAO Hong^1,2, WANG Shuhong³, ZHAO Chunying³, HU Chuanmin¹, CAI Jianhui¹, XIU Zhiming¹

1. Jilin Collaborative Innovation Center for Antibody Engineering, Jilin Medical University, Jilin 132013, Jilin Province, China; 2. The ChinaJapan Union Hospital of Jilin University, Changchun 130021, China;3. Changchun BC＆HC Pharmaceutical Technology Co., Ltd, Changchun 130012, China

Received:2019-08-02 Online:2019-11-26 Published:2019-11-21
Contact: XIU Zhiming E-mail:Xiuzm10@mails.jlu.edu.cn

摘要/Abstract

摘要： 以表面涂覆纤维素-三（3,5-二甲基苯基氨基甲酸酯）手性硅胶为固定相, 以V(正己烷)∶V(异丙醇)=95∶5[KG*8]的溶剂为流动相, 拆分对映异构体2-氧杂双环［3,3,0］辛-6-烯-3-酮. 流速为0.8 mL/min, 柱温25 ℃, 检测波长205 nm. 结果表明：该条件下对映异构体的分离度为30, 能有效拆分, 用面积归一化方法可确定光学纯度.

关键词: 2-氧杂双环［3,3,0］辛-6-烯-3-酮, 对映异构体, 拆分, 光学纯度

Abstract: The chiral silicon surface coated with cellulosethree (3,5dimethylphenyl carbamate) was used as stationary phase, the solvent of V(nhexane)∶V(isopropyl alcohol)=95∶5 was used as mobilephase to separate 2-oxabicyclo［3,3,0］oct-6-en-3-one. The flow rate was 08 mL/min, the column temperature was 25 ℃, and detection wavelength was 205 nm. The results show that the resolution is 3.0, the enantiomer can be effectively separated, and the optical purity can be determined by area normalization method.

Key words: 2-oxabicyclo［3,3,0］oct-6-en-3-one, enantiomer, separation, optical purity

中图分类号:

O641.6

曹宏, 王淑红, 赵春影, 胡川闽, 蔡建辉, 修志明. 2-氧杂双环［3,3,0］辛-6-烯-3-酮对映异构体手性拆分及光学纯度的测定[J]. 吉林大学学报(理学版), 2019, 57(06): 1530-1534.

CAO Hong, WANG Shuhong, ZHAO Chunying, HU Chuanmin, CAI Jianhui, XIU Zhiming. Chiral Separation of Enantiomer of 2-Oxabicyclo［3,3,0］oct-6-en-3-oneand Determination of Optical Purity#br#[J]. Journal of Jilin University Science Edition, 2019, 57(06): 1530-1534.

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