棉酚旋光体的高效液相色谱分析

Analysis of Gossypol Enantiomers by High Performance Liquid Chromatography

使样品中的左旋（－）棉酚和右旋（＋）棉酚与Ｌ－苯基丙胺醇充分反应以后，对生成的两种衍生物进行高效液相色谱分析。该方法以Ｗａｔｅｒｓ μＢｏｎｄａｐａｋＣ１８色谱柱为固定相，甲醇－磷酸水溶液为流动相，获得了良好的分离效果。每次样品的分析时间在１０分钟以内。样品的制备过程简单，并排除了杂质干扰。实验结果指出，Ｌ－苯基丙胺醇与棉酚的充分反应时间应为１２０分钟以上，两者之间的摩尔比应大于４：１。在本文所述条件下，两种棉酚旋光体的进样量在１５ｎｇ～１．２μｇ之间与其峰面积呈良好的线性关系，相关系数均大于０．９９９。方法的精密度测验表明，两组分的标准方差与变异系数都分别在０．１５与３．０以下。（－）棉酚和（＋）棉酚的回收率依次为９８．０％和９８．７％。

After the fully reaction of levo)gossypol and dextro(+)gossypol with L-phenylaninol ,the two derivatives were analyzed by high performance liquid chromatography(HPLC).We employed Waters μBondapak C18 column as the stationary phase and methanol-phosphoric acid aqueous solution as the mobile phase ,and got very good analysis results.The separating time for one sample was within 10 minutes.Sample preparation is quite simpleand interferences from some impurities were eliminated.The results indicated that the reactiontime between gossypol and L-phenylalaninol should be above 120 minutes.The molecular pro-portion of the two substances must be over 4:1.Under the conditions stated in this paper,the linear relationship between the two enantiomers and their peak areas were very good as theinjections were from 15ng to 1.2μ g.The correlation coefficients of the regression lines wereboth more than 0.999.The precision determination of the method showed that the standarddeviation and variation coefficient were below 0.15 and 3.0 ,respectively.The recovery ratesfor(-)gossypol and(+) gossypol were 98.0%and 98.7%in tur.