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·1986·                            精细化工   FINE CHEMICALS                                  第 35 卷

            变化并不大;而且 Tween 80 质量浓度远高于其临界                       围内,PCL 质量浓度通过改变乳液黏度对微胶囊粒
                           2
            胶束浓度 1.410  g/L 时,界面张力不再随 Tween 80                径产生影响。(4)经扫描电镜、FTIR 光谱图、Zeta
            浓度发生变化。均质乳化转速方面,当输入的能量                             电位表征,制备所得微胶囊成功包覆槲皮素,且粒
            超过基本能量时,粒径分布相差不大                  [15] 。由于本文       径均匀,分散度好,在水中具有较好的稳定性。研
            采用的均质机为间歇式高剪切,一档(5000 r/min)                       究结果对 SFEE 法在载药微胶囊的制备上提供了一
            便能提供较大能量,因此,以上两种因素对粒径分                             定的理论依据,为下一步将 SFEE 法应用在聚合物
            布影响不大。                                             纳米微胶囊的制备上奠定基础。
            2.3   微胶囊水中稳定性及包埋效果表征
            2.3.1   槲皮素微胶囊 Zeta 电位                             参考文献:
                                                               [1]   Heo D J, Shon M S, Kim G N, et al. Effect of UV irradiation on the
                 微胶囊在水中的长期稳定性与每个微粒的表面                              antioxidant and anti-adipogenic activities  of quercetin[J]. Food
            电荷密切相关。文献[16]指出,当体系的 Zeta 电位                           Science & Biotechnology, 2015, 24(1): 341-345.
            绝对值大于 30 mV 时,才能实现微粒间的稳定状态,                        [2]   Kiekow C J, Figueiró F, Dietrich F,  et al. Quercetin derivative
                                                                   induces cell death in glioma  cells by  modulating NF-κB nuclear
            反之当体系 Zeta 电位过小,微粒之间则倾向于团聚                             translocation and  caspase-3 activation[J]. European Journal  of
            状态。经检测,本文制备的载槲皮素微胶囊 Zeta 电                             Pharmaceutical Sciences Official Journal of the European Federation
                                                                   for Pharmaceutical Sciences, 2016, 84: 116-122.
            位值为34.80 mV,因而槲皮素微胶囊处于稳定状态。                       [3]   Guazelli C F, Fattori V, Colombo B B,  et al. Quercetin-loaded
            2.3.2   槲皮素微胶囊红外图谱分析                                   microcapsules ameliorate experimental colitis in mice  by anti-
                                                                   inflammatory and antioxidant mechanisms[J]. Journal  of Natural
                 PCL、槲皮素、微胶囊的红外谱图见图 8。                             Products, 2013, 76(2): 200-208.
                                                               [4]   Khaled K A,  El-Sayed  Y M,  Al-Hadiya  B M. Disposition of the
                                                                   flavonoid quercetin in rats after single intravenous and oral doses[J].
                                                                   Drug Development & Industrial Pharmacy, 2003, 29(4): 397-403.
                                                               [5]   Gugler R, Leschik M, Dengler H J. Disposition of quercetin in man
                                                                   after single oral and intravenous doses[J]. European Journal of
                                                                   Clinical Pharmacology, 1975, 9(2/3): 229-234.
                                                               [6]   Lévai G, Ángel Martín, Paz E D, et al. Production of stabilized quercetin
                                                                   aqueous suspensions by supercritical fluid extraction of emulsions[J].
                                                                   Journal of Supercritical Fluids, 2015, 100: 34-45.
                                                               [7]   Porta G, Reverchon E. Nanostructured microspheres produced by
                                                                   supercritical fluid extraction  of emulsions[J]. Biotechnology &
                                                                   Bioengineering, 2008, 100(5): 1020-1033.
                                                               [8]   Paz E  D,  Rodríguez S, Kluge J,  et al. Solubility of  β-carotene in
                                                                   poly-(-caprolactone) particles produced in colloidal  state by

                   图 8  PCL、槲皮素、微胶囊 FTIR 谱图                        Supercritical Fluid Extraction of Emulsions (SFEE)[J]. Journal of
                                                                   Supercritical Fluids, 2013, 84(84): 105-112.
             Fig. 8    FTIR spectra of PCL, quercetin, and microcapsules   [9]   Porta G D,  Castaldo  F. Bacteria  microencapsulation  in PLGA
                                                                   microdevices by supercritical emulsion extraction[J]. Journal of
                 文献[6]指出槲皮素的特征峰为 1600~1100 cm            1        Supercritical Fluids, 2012, 63(2): 1-7.
                                                    1
            之间。由图 8 可知,槲皮素在 1600~1100 cm 之间                    [10]  Falco N, Reverchon E, Della P G. Injectable PLGA/hydrocortisone
                                                                   formulation  produced by continuous supercritical emulsion
            的特征峰并未出现在微胶囊的波谱图上,而 PCL 的                              extraction[J]. International Journal of Pharmaceutics, 2013, 441(1/2):
            波谱图与微胶囊的波谱图在整个波数范围内非常相                                 589-597.
                                                               [11]  Vignes A. Diffusion in Binary Solutions. Variation of diffusion
            似,因而证明槲皮素被壁材 PCL 所包覆,而不是以                              coefficient with composition[J]. Industrial & Engineering Chemistry
            槲皮素晶体形式存在。                                             Fundamentals, 1966, 5(2): 189-199.
                                                               [12]  Byun H S, Choi M Y,  Lim J S. High-pressure phase behavior and
                                                                   modeling of binary mixtures for alkyl acetate in supercritical carbon
            3   结论                                                 dioxide[J]. Journal of Supercritical Fluids, 2006, 37(3): 323-332.
                                                               [13]  Mattea F, Ángel Martín, Matías-Gago A,  et al. Supercritical
                 本研究以槲皮素为芯材,PCL 为壁材,采用                             antisolvent precipitation from an emulsion: β-Carotene nanoparticle
                                                                   formation[J]. Journal of Supercritical Fluids, 2009, 51(2): 238-247.
            SFFE 法制备出粒径在 1~5 μm 的载槲皮素微胶囊。
                                                               [14]  Chattopadhyay P, Shekunov B Y, Yim D, et al. Production of solid
            通过对过程参数研究表明:(1)升高萃取温度、加快                               lipid nanoparticle suspensions using supercritical fluid extraction of
                                                                   emulsions (SFEE) for pulmonary delivery using the AERx system[J].
            CO 2 流速都能提高萃取效率,一定温度下,溶剂残
                                                                   Advanced Drug Delivery Reviews, 2007, 59(6): 444-453.
            留量随萃取压力的升高先减少后增加。当萃取压力                             [15]  Li Ji Cheng (李继成), Dong Li Feng (董立峰), Liu Zhen Bang (刘振
            达到该温度下 EA/CO 2 二元体系临界点压力时,即可                           邦),  et al. The Impactof Shearing  Speed, Time and Content  of
                                                                   Emulsifier on the Particle Size Distribution of EW[J]. World Pesticides
            取得较好的萃取效果。(2)与溶剂蒸发法相比,SFEE                             (世界农药), 2011, 33(3): 53-57.
            法在 40 min 内使溶剂残留降至 59 mg/L。(3)乳液                   [16] Lu Yi (吕怡). Preparation of jasmine essence micro/nano-capsule via
                                                                   complex coacervation and its mechanism research[D]. Wuxi:
            配比是控制微胶囊粒径的重要手段,本实验研究范                                 Jiangnan University (江南大学), 2012.
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