手性HPLC法分析双乙酰科立内酯对映异构体  

Determination of Diacetylation Corey Lactone Enantiomers by Chiral HPLC

作　　者：赵春影 王淑红 崔佰吉[1] 杨威龙 孟繁伟 蔡建辉[1] 修志明 ZHAO Chun-ying;WANG Shu-hong;CUI Bai-ji;YANG Wei-long;MENG Fan-wei;CAI Jian-hui;XIU Zhiming(Jilin Medical University,Jilin 132013,China;Changchun BC&HC Pharmaceutical Technology Co.,Ltd.,Changchun 130012,China)

机构地区：[1]吉林医药学院,吉林吉林132013 [2]长春百纯和成医药科技有限公司,吉林长春130012

出　　处：《精细化工中间体》2023年第3期62-67,共6页Fine Chemical Intermediates

基　　金：吉林省科技厅项目(20200708090YY)。

摘　　要：建立了前列腺素中间体双乙酰科立内酯对映异构体的手性高效液相色谱测定方法。采用硅胶表面涂覆有纤维素-三(3,5-二甲基苯基氨基甲酸酯)的手性色谱柱(OD-H,4.6 mm×250 mm,5μm),以正己烷-异丙醇(V∶V=80∶20)为流动相,流速1.0 mL/min,柱温40℃,检测波长205 nm,外标法测定对映异构体超量值。结果双乙酰科立内酯对映异构体分离度为3.5,(+)-双乙酰科立内酯在0.199~3.980 mg/mL(R^(2)=0.9994)、(-)-双乙酰科立内酯在0.198~3.960 mg/mL(R^(2)=0.9994)浓度范围线性关系良好。(+)-双乙酰科立内酯低、中、高浓度平均加样回收率(RSD)分别为99.38%(0.43%)、99.30%(0.88%)、100.10%(0.51%),(-)-双乙酰科立内酯低、中、高浓度平均加样回收率(RSD)为99.76%(0.86%)、100.07%(0.26%)、99.27%(0.20%)。3批样品平均对映异构体超量值为4.75%、70.10%、-75.33%。方法简便、快速,能准确测定双乙酰科立内酯对映异构体超量值,为前列腺素药物手性中间体提供新的分离和检测方法。A method for determination of the prostaglandin intermediates diacetylation corey lactone enantiomers by chiral HPLC were established.The optimal chromatographic conditions were as follows:chiral column(OD-H,4.6 mmx250 mm,5μm)coated with Cellulose-tri(3,5-dimethylphenylcarbamate),mobile phase:n-hexane-iso-propyl alcohol(V:V=80:20),flow rate 1.0 mL/min,column temperature 40 C,detection wavelength 205 nm,the enantiomeric excess value was calculated by external standard method.The results showed that the resolution be-tween the corey lactone diol enantiomers was 3.5,and(+)-diacetylation corey lactone had a good linear relation-ship(R^(2)=0.9994)in the concentration range of 0.199~3.980 mg/mL as well as(-)-diacetylation corey lactone in the concentration range of 0.198~3.960 mg/mL(R^(2)=0.9994).The average recoveries(RSD)of(+)-diacetylation corey lactone at low,medium and high concentrations were 99.38%(0.43%),99.30%(0.88%),100.10%(0.51%).The average recoveries(RSD)of(-)-diacetylation corey lactone at low,medium and high concentrations were 99.76%(0.86%),100.07%(0.26%),99.27%(0.20%).The average enantiomeric excess values of three samples were 4.75%,70.10%,-75.33%.The established method is simple,rapid and accurate,and can accurately determine the enantiomeric excess value of diacetylation corey lactone enantiomers.It provides a new method for the separation and detection of chiral intermediates of prostaglandin drugs.

关 键 词：HPLC 手性 双乙酰科立内酯 对映异构体超量 

分 类 号：R917[医药卫生—药物分析学]