超声辅助-反溶剂法制备大豆素超微粉及性质

Preparation and properties of daidzein microparticles by an ultrasonic assisted anti-solvent method

针对天然大豆素的水溶性差,生物利用度低和实际应用受限的问题,以天然大豆素为原料,N,N-二甲基甲酰胺为溶剂,去离子水为反溶剂,通过超声辅助-反溶剂法制备大豆素超微粉,采用单因素对大豆素生成的粒径进行考察,并结合响应面优化单因素结果,利用扫描电子显微镜(SEM)、傅里叶变换红外光谱(FTIR)、差示扫描量热仪(DSC)、气相色谱观测和分析粉体外观形貌、粒径、性质和大豆素超微粉溶剂残留浓度。结果表明,大豆素超微粉的最佳制备条件分别为:溶液质量浓度为15.83 mg×mL^(-1),喷嘴孔径为300μm,均质转速为3000 r×min^(-1),反溶剂-溶剂的体积比(液液比)为9,超声功率为144W,制得的最小大豆素超微粉粒径为188 nm;与原粉相比,大豆素超微粉的粒径显著减小,化学结构无改变,且抗氧化活性显著提高。

In order to solve the problems of poor water solubility,low bioavailability and limited practical application of natural daidzein,daidzein ultrafine powders were prepared by an ultrasonic assisted anti-solvent method which used natural daidzein as raw material,N,N-dimethylformamide as solvent,and deionized water as antisolvent.Daidzein particle size was studied by single factor experiments,and the results were optimized by Box-Behnken design combined with response surface methodology.The appearance and particle size of the powder was observed by scanning electron microscopy,the properties were analyzed by Fourier Transform infrared spectroscopy and differential calorimetry and the residual solvent concentration of daidzein ultrafine powder was analyzed by gas chromatography.The results show that the best preparation conditions were:solution concentration=15.83 mg×mL^(-1),nozzle diameter=300μm,homogenization rate=3000 r×min^(-1),volume ratio of inverse solvent to solvent(liquid to liquid)=9 and ultrasonic power=144 W.The minimum particle size of daidzein ultrafine powder was 188 nm.Compared with raw powder,the size of ultrafine powder is greatly reduced,the chemical structure is not changed before and after preparation,and the antioxidant activity is significantly increased.