环氧虫啶多晶型的制备和表征

The preparation and characterization of polymorphs of cycloxaprid

[目的]制备环氧虫啶的多晶型,并对其进行表征。[方法]采用旋蒸法成功制备环氧虫啶晶型B,通过粉末X射线衍射、差示扫描量热、热重分析、红外光谱、单晶X射线衍射和扫描电镜等对其进行表征,并对其溶解度、粉末粒度和堆密度进行了测试。[结果]晶型B为环氧虫啶与硝基甲烷以1∶1摩尔比的硝基甲烷溶剂化物,在25℃水中溶解度为1616.19 mg/L,平均粒度D_(0.5)为10.650μm,堆积密度为0.289 g/cm^(3),均比原药晶型A有所提高。[结论]通过制备晶型B,可以提高环氧虫啶的溶解度、粉末粒度和堆积密度,方便其制剂加工。

[Aims]The study aims to prepare and characterize cycloxaprid polymorphs.[Methods]The cycloxaprid form B was successfully prepared by rotational evaporation method and characterized using powder X-ray diffraction,differential scanning calorimetry,thermogravimetric analysis,infrared spectroscopy,single-crystal X-ray diffraction and scanning electronmicroscope.In addition,the solubility,powder particle size,and bulk densitywere tested.[Results]The results showed that Form B was a nitromethane solvate with a 1:1 molar ratio of cycloxaprid and nitromethane.The solubility of Form B was 1616.19 mg/L in water at 25℃,an average particle size of D_(0.5) was 10.650μm,and a bulk density was 0.289 g/cm^(3).All of these results of Form B were higher than Form A.[Conclusions]The solubility,powder particle size,and bulk density of cycloxaprid were improved by being prepared to Form B,and the preparation process was more convenient.