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大豆異黃酮納米粉體的反溶劑法制備及表征
發(fā)布時(shí)間:2019/11/4 15:57:25 瀏覽次數(shù):1164
大豆異黃酮納米粉體的反溶劑法制備及表征
Preparation and Characterization of Soy Isoflavone Nanoparticles by Antisolvent Precipitation Method
DOI:
中文關(guān)鍵詞: 大豆異黃酮 微細(xì)粉體 反溶劑 表征 粒徑
英文關(guān)鍵詞: soy isoflavone powder anti-solvent characterization particle size
以二甲基亞砜作為溶劑,丙酮為反溶劑制備大豆異黃酮納米粉體。通過正交試驗(yàn)設(shè)計(jì)法,以大豆異黃酮粒徑為指標(biāo),對(duì)各個(gè)影響因素和水平進(jìn)行研究,得到最佳的試驗(yàn)條件。結(jié)果:大豆異黃酮的納米粒徑與溶液體積比、勻漿器轉(zhuǎn)速、溶液濃度呈反比,與反應(yīng)時(shí)間呈正比。大豆異黃酮的最佳試驗(yàn)條件為:溶液質(zhì)量濃度300 mg/mL,轉(zhuǎn)速1 200 r/min,溶劑與反溶劑的體積比1∶6,反應(yīng)時(shí)間3 min。在該條件下得到的納米大豆異黃酮粒徑為98 nm。通過掃描電鏡(SEM)觀測粒子外觀,并用粉體堆密度方法統(tǒng)計(jì)。通過紅外光譜(FT-IR)、差熱掃描(DSC)等方法對(duì)制備的粉體進(jìn)行物理化學(xué)性質(zhì)表征。結(jié)果表明:制備前、后大豆異黃酮的粉體化學(xué)性質(zhì)沒有發(fā)生改變,納米大豆異黃酮顆粒分布均勻,粒徑顯著減小。
Taking dimethyl sulfoxide as solvent, soy isoflavone powder was prepared by acetone as the anti-solvent. Orthogonal experimental design method was used to in spect the major factors affecting the size and morphology of soy isoflavone powder. Results show that the particle size has a negative relationship with volume ratio, rotor speed and concentration, and has a positive relationship with reaction time. Experiment indicates that the measured powder particle size reaches 98 nm when the concentration is 300 mg/mL; rotor speed is 1 200 r/min; volume ratio is 1 ∶ 6 and reaction time is 3 min. Isoflavone and nano-isoflavone power were evaluated by using scanning electron microscope (SEM), infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and statistics of powder heap density. Results showed that the chemical properties of isoflavones did not change after preparation. Nano-isoflavone particles were distributed evenly and the particle size decreased significantly.