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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 sufficient reaction of L-(? -) gossypol and dextrorpol (+) gossypol in the sample with L-phenylpropanolamine, both of the resulting derivatives were subjected to high performance liquid chromatography. The method uses Waters μ Bondapak C18 column as the stationary phase and methanol-phosphoric acid aqueous solution as the mobile phase to obtain a good separation effect. Analysis time for each sample is within 10 minutes. Sample preparation is simple and excludes impurity interference. The experimental results show that L-phenylpropanolamine and gossypol sufficient reaction time should be 120 minutes or more, the molar ratio between the two should be greater than 4: 1. Under the conditions described in this paper, the injection volume of two kinds of gossypol photon has a good linear relationship with the peak area of 15ng ~ 1.2μg, the correlation coefficient is greater than 0.999. The method of precision test showed that the two components of the standard deviation and coefficient of variation were 0.15 and 3.0, respectively. The recoveries of (-) gossypol and (+) gossypol were 98.0% and 98.7%, respectively.