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中国无机分析化学:2021,11(2):21-25
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联萘酚手性拆分方法及其用于实验室废水的检测
邱琬雅1, 冯航1, 许志刚1, 朱瑞芝2, 张凤梅2, 刘志华2, 司晓喜2
(1.昆明理工大学 理学院 化学分离与富集重点实验室;2.云南中烟工业有限责任公司技术中心)
Chiral separation method for binaphthol enantiomer and its application for laboratory wastewater analysis
QIU Wanya1, FENG Hang1, XU Zhigang1, ZHU Ruizhi2, ZHANG Fengmei2, LIU Zhihua2, SI Xiaoxi2
(1.Faculty of Science,Kunming University of Science and Technology;2.R D Center of China Tobacco Yunnan Industrial Co Ltd)
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投稿时间:2020-12-19    修订日期:2021-01-23
中文摘要: 联萘酚是具有手性的药物中间体,其对映体的拆分和检测具有重要意义。建立了一种反相色谱手性拆分方法,用于联萘酚对映体的拆分。考察了六种不同手性色谱柱的拆分效果,并进一步对流动相配比、柱温和流速等因素进行了优化。结果表明,CHIRALPAK? IA手性柱对联萘酚对映体有较好的拆分性能,在流动相为甲醇-1 %醋酸(90 : 10,v/v)、柱温25 ℃、流速0. 7 mL/min时,分离度最大、拆分效果最佳。该方法用于实验室排放水体中联萘酚对映体含量的测定,加标回收实验得到R-联萘酚的回收率在80.20% ~ 115.4%之间,RSD小于7.70%;S-联萘酚的回收率在82.17% ~ 117.83%之间,RSD在2.49% ~ 9.48%范围内。该方法简便、快速、低毒,可用于联萘酚对映体的拆分及在污水中其对映体含量检测。
Abstract:Binaphthol is a chiral pharmaceutical intermediate, and the separation of its enantiomers is of great significance to medicinal chemistry. A reverse phase liquid chromatography method was established for the chiral separation of binaphthol enantiomers. In this paper, six different chiral columns were used for the separation of binaphthol enantiomers. And the chromatography conditions were further optimized. The results showed that when the mobile phase was methanol-1% acetic acid (90: 10, v/v), the column temperature was 25 ℃, and the flow rate was 0.7 mL/min, the best chiral separation effect could be obtained. This method was also used for the determination of the enantiomeric content of binaphthol in three types of laboratory wastewater, but no binaphthol could be found in the above samples. The recovery of R-binaphthol was 80.20% – 115.4%, and the RSD was less than 7.70%. The recovery of S-binaphthol was 82.17% – 117.83%, and the RSD was 2.49% – 9.48%. The method is simple, rapid, and low-toxic. It can be used for the separation and determination of binaphthol enantiomers in wastewater.
文章编号:     中图分类号:O657.7    文献标志码:
基金项目:国家自然科学(21565018); 中国烟草总公司科技重大专项项目[No. 110201901002(XX-02)]; 云南中烟工业有限责任公司重点项目(No. 2018JC05); 昆明理工大学大学生课外学术科技创新基金(2020BA216).
引用文本:
邱琬雅,冯航,许志刚,朱瑞芝,张凤梅,刘志华,司晓喜.联萘酚手性拆分方法及其用于实验室废水的检测[J].中国无机分析化学,2021,11(2):21-25.
QIU Wanya,FENG Hang,XU Zhigang,ZHU Ruizhi,ZHANG Fengmei,LIU Zhihua,SI Xiaoxi.Chiral separation method for binaphthol enantiomer and its application for laboratory wastewater analysis[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(2):21-25.

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