Page 18 - 201812
P. 18
·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 1.410 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.