氯仿重结晶棉酚的质量研究

报道了氯仿重结晶的棉酚的化学性质,样品在不同温度下干燥恒重后,经熔点、薄层层析、紫外光谱、红外光谱、X-射线衍射、热重量分析、元素(C,H,Cl)分析及棉酚合量测定等一系列的分析,确证了在60℃以下棉酚与氯仿成溶剂化物(solvate)。随着干燥温度的升高或在室温长时间的贮存,此现象逐渐消失,100℃真空干燥恒重后成为纯棉酚。

STUDY ON QUALITY OF GOSSYPOL RECRYSTALIZED FROM CHLOROFORM

In this paper, the chemical properties of gossypol recrystallized from chloroform are described. Samples were dried at different temperatures at reduced pressure, and stored under room temperature for different times. They were identified and determined by melting point, thin layer chromatography, UV spectrophotometry, IR spectrophotometry, thermo-gravimetric analysis, X-ray diffraction, elementary analysis and also for the content of gossypol. The results of these tests proved gossypol to be solvated with chloroform at low temperature. This phenomenon decreased gradually with increase of drying temprature or storage time, and the content of gossypol increased accordingly. The presence of chloroform in the crystal interferes with the purity of gossypol.Thus,it is necessary to identify the presence of chloroform with oxygen flask ombustion-mercurimetry beforehand.