联萘酚手性拆分方法及其用于实验室废水的检测

Chiral Separation Method for Binaphtholenantiomer and Its Application for Laboratory Wastewater Analysis

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。建立一种反相液相色谱手性拆分方法,用于联萘酚对映体的拆分。考察了6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%乙酸(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。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-联萘酚的加标回收率在80.2%~115%,相对标准偏差(RSD)小于7.7%;S-联萘酚的加标回收率在82.2%~118%,RSD在2.5%~9.5%。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。

Binaphthol is a chiral pharmaceutical intermediate,and the separation of its enantiomers is of great significance to medicinal chemistry.A reversephase liquid chromatography method was established for the chiral separation of binaphtholenantiomers.In this paper,six different chiral columns were used for the separation of binaphtholenantiomers.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 bestchiral 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,butno binaphthol could be found in the above samples.The recovery of R-binaphthol was 80.2%-115%,and the RSD was less than 7.7%.The recovery of S-binaphthol was 82.2%-118%,and the RSD was 2.5%-9.5%.The method is simple,rapid,and low-toxic.It can be used for the separation and determination of binaphthol enantiomersin wastewater.