Soy glycinin microcapsules by simple coacervation method

Encapsulation of a dispersed oil phase (hexadecane) was realized by simple coacervation method using soy glycinin as the wall forming material. Suitable emulsification and coacervation conditions, that favor the formation of microcapsules wall, were identified and investigated. Mild acid (pH 2.0) and heat (55 degrees C) treatments of the reaction medium during the emulsification step enhanced significantly the deposition of coacervated glycinin around oil droplets. A pronounced correlation between glycinin concentration in the continuous phase, specific surface of the dispersed phase and the microencapsulation efficiency was also observed. Coacervation step study concerned the morphology and the stability of microcapsules. Controlled initiation of the coacervation, by slow readjustment of the pH, allowed a homogeneous precipitation of glycinin around oil droplets as well as the absence of aggregation phenomena. Since the morphology of microcapsules was considerably affected by a prolonged stirring of the reaction medium, the coacervation and reticulation time were optimized in order to preserve the homogeneity of the microcapsules size distribution and the microencapsulation efficiency.     

Study of Complex Coacervation of Gelatin A and Sodium Alginate for Microencapsulation of Olive Oil

Complex coacervation of gelatin A and sodium alginate was carried out to obtain the maximum coacervate yield. Turbidity and coacervate yield (%) measurements were carried out to support the ratio of the two polymers and pH that produced maximum coacervation. The optimum ratio between gelatin A-sodium alginate and pH to form the maximum coacervate complex was found to be 3.5:1 and 3.5–3.8, respectively. Olive oil microencapsulation was carried out at the optimized ratio and pH. Microcapsules were crosslinked by using glutaraldehyde. Scanning electron microscopy studies confirmed the formation of free flowing spherical microcapsules of different sizes. The size of microcapsules increased with the increase in the concentration of the polymer. The encapsulation efficiency and the release rates of olive oil were dependent on the amount of crosslinker, oil loading and polymer concentration. Thermogravimetric study revealed improvement of thermal stability with crosslinking. Fourier Transform Infrared Spectroscopy study showed that there was no significant interaction between olive oil and gelatin-alginate complex.     

Preparation and Characterization of Oil Containing Microcapsules Obtained by an Interaction Induced Coacervation

A novel method for microencapsulation of oil by coacervation is presented. The method employs segregative phase separation between sodium carboxymethyl cellulose (NaCMC) and a complex of hydroxypropylmethyl cellulose (HPMC) and sodium dodecylsulfate (SDS), which results in coacervate formation. Microstructural properties of the coacervate can be varied by tuning NaCMC-HPMC/SDS interaction, which is achieved by changing SDS concentration. Microcapsules preparation route is presented. Encapsulation efficiency and dispersion properties of microcapsules with coacervate shell of different properties and different oil content were tested. Microcapsules with smallest droplet size, the narrowest droplet size distribution, and with lowest extractability of encapsulated oil were obtained when NaCMC-HPMC/SDS interaction results in formation of the most compact coacervate shell, no matter of the encapsulated oil.     

Preparation of monodisperse crosslinked polymelamine microcapsules by phase separation method

Monodisperse polymelamine microcapsules were prepared by phase separation method. Control of microcapsule diameter was investigated using the uniform-sized oil-in-water emulsion droplets as the capsule core. The monodisperse emulsion droplets were prepared using the Shirasu porous glass (SPG) membrane emulsification technique. The effects of the diameter of the oil droplet and concentration of sodium dodecyl sulfate (SDS), which is a typical emulsifier in SPG membrane emulsification, on microencapsulation were investigated. The microcapsules were aggregated when oil droplets with small size were microencapsulated at high SDS concentration. To reduce the SDS concentration, the creamed emulsion was used. The monodisperse polymelamine microcapsules were successfully prepared by using the creamed emulsion. The microcapsule diameter was almost similar to the diameter of the encapsulated oil droplet. The coefficient of variation values was about 10% for all microcapsules prepared in this study. Control of microcapsule diameter was achieved in the range of 5–60 μm.     

含润滑油微胶囊复合镀铜机理和镀层性能

采用水相分离法制备了以润滑油为囊心、聚乙烯醇为囊壁的微胶囊，并考察了含这种微胶囊复合镀铜层的性能.通过对这种复合镀层微观形貌的观察及耐腐蚀性、耐磨性、动摩擦系数的测定，结果表明由于复合镀铜层中含有润滑油微胶囊，其耐腐蚀性和耐磨性能都得到很大提高，并分析了这种微胶囊复合电沉积的机理和镀层的润滑、修复作用.     

Microencapsulation of extract containing shikonin using gelatin-acacia coacervation method: a formaldehyde-free approach

The application of microcapsule for pharmaceutical dosage form for various drugs has received considerable attention in recent years due to its multiple advantages. The most frequently used crosslinking agent formaldehyde in the gelatin–acacia microencapsulation process was altered by glycerol in this study. The effect of various parameters such as the concentration of surfactant, concentration of gelatin and continuous phase pH condition on the microcapsule particle size distribution was experimentally investigated. It was shown that the optimum concentration for surfactant/oil ratio is 1/10 and gelatin/oil ratio is 1/5 in the pH condition of approximately 4–6 for the coacervation process. Results obtained from microscopy observation revealed that one core microcapsule prepared by 6% glycerol was no different from formaldehyde. Hence, glycerol was demonstrated to be a good potential non-toxic crosslinking material for the applications of encapsulated extract containing shikonin.     

Optimization of cross-linking parameters during production of transglutaminase-hardened spherical multinuclear microcapsules by complex coacervation

Gelatin-gum arabic spherical multinuclear microcapsules (SMMs) encapsulating peppermint oil were prepared by complex coacervation. Transglutaminase (TG) was used to harden the SMMs by complex coacervation instead of traditional reagents such as formaldehyde or glutaraldehyde. The effect of various cross-linking parameters on the hardening effectiveness of SMMs containing peppermint oil was investigated. The optimum parameters were as follows: hardening for 6h at 15 degrees C and pH 6.0 with a TG concentration of 15 U/g gelatin. Compared with formaldehyde, TG exhibits similar microcapsule hardening effectiveness.     

大豆分离蛋白-十二烷基硫酸钠微胶囊的制备与表征

以大豆分离蛋白(SPI)和十二烷基硫酸钠(SDS)为壁材, 以十六烷为芯材, 通过复凝聚法制备了微胶囊. 首先确定了SPI和SDS发生复凝聚的适宜pH、SPI/SDS配比、壁材浓度等. 在确定的实验条件下进行复凝聚, 凝聚物产率可达85%. 改变搅拌转速和芯壁比, 考察它们对微胶囊性能的影响. 用光学显微镜观察了微胶囊形貌. 用气相色谱测定了微胶囊的载药量和包覆率. 芯壁比为2、搅拌转速为400 r/min时所制备微胶囊的载药量可达61%. 随着芯壁比的增大, 微胶囊粒径及载药量都逐渐增大.     

单凝聚与复凝聚法制备昆虫激素十二醇微胶囊及其释放行为

通过向明胶溶液中加入硫酸钠溶液的单凝聚方法以及将明胶溶液加入到阿拉伯胶溶液的复凝聚方法,制备了聚合物包覆昆虫激素十二醇的水分散体系微胶囊.通过对凝聚过程中ζ电位与透光率跟踪测试确定了单凝聚中加入硫酸钠的最佳用量以及复凝聚中明胶与阿拉伯胶的相对量.在壁材浓度大于或等于3%条件下制备的复凝聚胶囊的尺寸大于单凝聚微胶囊,但后者的大小分布更均一.除非在2%壁材浓度下,其他条件下复凝聚制备的胶囊的十二醇包覆率明显高于单凝聚胶囊.对胶囊中十二醇在恒湿恒温条件下的释放研究表明,单凝聚胶囊中十二醇很快释放完毕,变化壁材浓度不明显改变其释放行为.相比之下复凝聚胶囊中十二醇的释放对壁材浓度有明显的依赖性.2%壁材浓度制备的胶囊其释放行为类似于单凝聚胶囊;但3%到5%壁材浓度制备的胶囊中十二醇的释放明显分为3个区间,即较快的初始释放、较长时间的恒速释放以及最后阶段释放速率的再次提高直至释放完毕.复凝聚胶囊中十二醇的释放表现出了明显的可控性.文中亦对该体系中昆虫激素十二醇的释放机理作了初步讨论.     

Preparation of PCM microcapsules by complex coacervation of silk fibroin and chitosan

Phase change material microcapsules were prepared by complex coacervation of silk fibroin (SF) and chitosan (CHI). n-Eicosane was used as the core material. The effects of SF/CHI ratio, and percentage of cross-linking agent and n-Eicosane content on the properties of microcapsules were studied. The size distribution and the surface morphology of microcapsules were characterized by optical and scanning electron microscopy. The encapsulation of core material was determined by energy dispersive spectrometer analysis. The results indicated that SF/CHI microcapsules were prepared successfully. Microcapsules had smooth outer surface when the ratio of SF to CHI was close to 5. On the other hand, at high SF/CHI ratios (≥14), microcapsules showed a two-layer structure, an inner compact layer, and an outer, more porous, sponge-like layer. The highest microencapsulation efficiency was obtained at a SF/CHI ratio of 20 in the presence of 0.9% cross-linking agent and of 1.5% n-Eicosane content.     

Chitosan–Alginate Microcapsules for Oral Delivery of Egg Yolk Immunoglobulin (IgY): Effects of Chitosan Concentration

In our previous study, chitosan–alginate microcapsules were developed to protect egg yolk immunoglobulin (IgY) from gastric inactivation. The present study was undertaken to determine the effect of chitosan concentration (0–0.8%; w/v) on various properties of the microcapsules in order to produce the optimum chitosan–alginate microcapsules for use in the oral delivery of IgY. The properties investigated included microcapsule morphology, loading capacity for IgY (expressed as the IgY loading percentage, w/w, of microcapsules), encapsulation efficiency (EE%), in vitro gastroresistance, and IgY release. IgY loading percentage and EE% were both highest at 0.2% (w/v) chitosan, and, above this level, further increases were not observed. The stability of IgY in simulated gastric fluid (pH 1.2) was significantly improved by encapsulation in alginate microcapsules (IgY retained 43.5% of its activity) and was further improved by including chitosan at any of the chitosan concentrations assessed (IgY retained an average of 69.4% activity) although there was no difference in protection of gastric inactivation among concentrations of chitosan varying from 0.05% to 0.8% (w/v). Higher chitosan concentrations (i.e., ≥0.2%; w/v) prolonged the release of IgY from the microcapsules during simulated intestinal fluid incubation (pH 6.8). However, above the 0.2% (w/v) level, no significant differences were observed. We conclude that the optimum chitosan concentration for microencapsulation is 0.2% (w/v).     

Preparation and release properties of flufiprole-loaded microcapsules with core status of solid particles,solution droplets and oil suspending agent

Our main goal was to evaluate release mechanism of microcapsules with different core status. First, flufiprole microcapsules were directly encapsulated with chitosan (CS) and sodium dodecyl sulfate (SDS) through layer-by-layer (LbL) self-assembly. The changes of process parameters on the microcapsules characteristics (zeta potential, and morphology) were investigated. Also the release trends of flufiprole were determined and fitted with mathematical models. It was revealed that releases of three types of microcapsules were all very similar, but microcapsule with solid particles and oil suspending agent reached their peak values at 36–42, 42–48?h respectively, microcapsule with solution droplets cannot reach a maximum value. In the stage of initial burst release, Higuchi model performed better with oil suspending agent and solid particles, which was in agreement with the Fick's law. Core status being solution, release curves of the pesticide corresponded to zero-order which was in agreement with dissolution mechanism. In the stage of slow release, the values of R² for solution and solid particles were all above 0.98, betokened the release phenomenon were in line with the first-order. On the other hand, release of oil suspending agent conformed to Higuchi model.     

Microencapsulation of cholesteryl alkanoate by polymerization‐induced phase separation and its association with drugs

A new microencapsulation technique is presented in which cholesteryl nonanoate (CN)/poly(methyl methacrylate) (PMMA) microcapsules are produced by the induction of phase separation between CN and PMMA within the droplets during the polymerization. The concentration of CN is the most important factor determining the final morphology of the microcapsules. For example, a polynuclear type is obtained at a low concentration (<20 wt %), a mononuclear type is obtained at a medium concentration (20–30 wt %), and an irregular phase is obtained at a high concentration (>40 wt %). To evaluate the effectiveness of the technique for stabilizing an unstable drug, we selected retinol (vitamin A) as a model drug and loaded it into the CN/PMMA microcapsules. We used a process called solute codiffusion, in which a fine solvent emulsion containing the retinol was diffused uniformly into the CN/PMMA microcapsules. The loading efficiency of retinol was predicted successfully with the aid of a thermodynamic equation. In the thermal stability test of retinol, we found that an effective association with the CN phase was the most important factor determining the limit of its molecular stability. The technique reported in this article has great potential for the microencapsulation of soft materials via a simple process and for the stabilization of unstable drugs. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 2202–2213, 2004     

Attachment of nickel oxide nanoparticles on the surface of palygorskite nanofibers

To study the relationship between emulsion stability and polymer emulsifier concentration, the preparation of paraffin oil emulsions by hydroxypropyl methylcellulose (HPMC) was carried out with HPMC concentrations below the overlapping concentration (C(*)) of HPMC. The stability of the emulsions incorporating HPMC was investigated by measuring the creaming velocity, volume fraction of emulsified paraffin oil, oil droplet size, and some rheological responses such as the stress-strain sweep curve and strain and frequency dependences of dynamic viscoelastic moduli. The paraffin oil was almost emulsified by HPMC above C(*)/20: the volume fraction of paraffin oil in the emulsion was higher than 0.72. Increasing in the HPMC concentration led to decreases in both the average oil droplet size and creaming velocity and an increase in the yield stress. All emulsions behaved as solid-like viscoelastic matter. Additionally, the measured dynamic storage moduli were compared with those calculated from a relationship based on functions of the volume fraction of oil in the emulsions and Laplace pressure; good agreement between the measured and calculated moduli was obtained. On the other hand, at HPMC concentrations below C(*)/50, the emulsified paraffin oil became unstable and the oil and the HPMC solution eventually separated.     

复凝聚法制备昆虫激素模拟物十二醇微胶囊及其释放性能

以明胶(GE)和阿拉伯胶(AG)为壁材, 通过复凝聚法将昆虫激素模拟物十二醇(C12OH)包覆在微胶囊中, 改变微胶囊壁材的浓度和交联度, 探讨了体系中C12OH的可控释放性能. 通过对壁材质量比为1及不同pH条件下的壁材凝聚率测试确定最佳复凝聚的pH为4.0; 考察了不同分散剂对微胶囊及其分散液性能的影响, 确定以Tween 20/Span 80(质量比1∶1)作为复凝聚法包覆C12OH体系的分散剂. 在壁材质量分数大于或等于3%条件下制备的微胶囊粒径大于壁材质量分数为2%的微胶囊, 胶囊的载药量和C12OH包覆率明显高于后者. 增加交联剂的用量, 壁材交联度、胶囊的载药量和C12OH包覆率都显著提高. 在相同用量的情况下, 用甲醛作交联剂时得到的微胶囊的交联度比用戊二醛作交联剂时的要低, 但其对C12OH的包覆率更高. 通过扫描电镜对微胶囊进行了分析, 认为GE与AG通过复凝聚能够将C12OH包覆在微胶囊内部. 对胶囊中C12OH在恒温恒湿条件下的释放研究结果表明, 3%与4%壁材含量下1%戊二醛交联的微胶囊和5%壁材含量下4%戊二醛交联的微胶囊中C12OH的释放行为有明显的可控性. 通过调节微胶囊的壁材含量和交联度可以达到昆虫激素可控释放的目的.     

Physicochemical Properties and Storage Stability of Microencapsulated DHA-Rich Oil with Different Wall Materials

This study aimed to evaluate the physicochemical properties and storage stability of microencapsulated DHA-rich oil spray dried with different wall materials: model 1 (modified starch, gum arabic, and maltodextrin), model 2 (soy protein isolate, gum arabic, and maltodextrin), and model 3 (casein, glucose, and lactose). The results indicated that model 3 exhibited the highest microencapsulation efficiency (98.66 %) and emulsion stability (>99 %), with a moisture content and mean particle size of 1.663 % and 14.173 μm, respectively. Differential scanning calorimetry analysis indicated that the Tm of DHA-rich oil microcapsules was high, suggesting that the entire structure of the microcapsules remained stable during thermal processing. A thermogravimetric analysis curve showed that the product lost 5 % of its weight at 172 °C and the wall material started to degrade at 236 °C. The peroxide value of microencapsulated DHA-rich oil remained at one ninth after accelerated oxidation at 45 °C for 8 weeks to that of the unencapsulated DHA-rich oil, thus revealing the promising oxidation stability of DHA-rich oil in microcapsules.     

Process regulation for encapsulating pure polyamine via integrating microfluidic T-junction and interfacial polymerization

The quality of microcapsules directly determines the performance of microcapsule-based functional materials, such as self-healing materials. How to achieve high-quality microcapsules depends on not only the selected microencapsulation technique but also the process regulation. Herein, using tetraethylenepentamine (TEPA) as the core target to be encapsulated by a novel microencapsulation technique through integrating microfluidic T-junction and interfacial polymerization, this investigation studied how the process parameters influence the microencapsulation process and the quality of the synthesized microcapsules regarding the size, morphology, shell structure, and composition. The studied parameters include the solvent type and surfactant concentration in the co-flow solution, the fed volume of the co-flow solution, the types of the solvent, catalyst, and shell-forming monomer in the reaction solution for the shell-growth stage, and the reaction temperature at the shell-growth stage. The influence mechanisms were established based on the observations, and the optimized parameter combination for the process was achieved. Through the parametric study for the microencapsulation technique, this study also lays a solid foundation for the technique to fabricate microcapsules containing other functional substances with high quality.     

载细胞海藻酸钠/壳聚糖微胶囊的化学破囊方法研究

以海藻酸钠-壳聚糖-海藻酸钠微胶囊(简称ACA微胶囊)为研究体系,建立了一种生理条件下ACA微胶囊的化学破囊方法,破囊过程充分考虑了对囊内生物物质活性的保持.以微生物细胞PichiapastorisGS115和动物细胞L929为模型,以NaHCO₃和Na₃C₆H5O₇·2H₂O为破囊液基本组分,考察了破囊液对ACA微胶囊的破囊效果及破囊过程对囊内细胞活性的影响.结果表明,破囊操作可在30s内完成,破囊率为100%,微胶囊膜完全溶解,破囊后细胞存活率在85%以上.     

Multicore-shell PNIPAm-co-PEGMa microcapsules for cell encapsulation

The overall goal of this study was to fabricate multifunctional core-shell microcapsules with biological cells encapsulated within the polymer shell. Biocompatible temperature responsive microcapsules comprised of silicone oil droplets (multicores) and yeast cells embedded in a polymer matrix (shell) were prepared using a novel microarray approach. The cross-linked polymer shell and silicone multicores were formed in situ via photopolymerization of either poly(N-isopropylacryamide)(PNIPAm) or PNIPAm, copolymerized with poly(ethylene glycol monomethyl ether monomethacrylate) (PEGMa) within the droplets of an oil-in-water-in-oil double emulsion. An optimized recipe yielded a multicore-shell morphology, which was characterized by optical and laser scanning confocal microscopy (LSCM) and theoretically confirmed by spreading coefficient calculations. Spreading coefficients were calculated from interfacial tension and contact angle measurements as well as from the determination of the Hamaker constants and the pair potential energies. The effects of the presence of PEGMa, its molecular weight (M(n) 300 and 1100 g/mol), and concentration (10, 20, and 30 wt %) were also investigated, and they were found not to significantly alter the morphology of the microcapsules. They were found, however, to significantly improve the viability of the yeast cells, which were encapsulated within PNIPAm-based microcapsules by direct incorporation into the monomer solutions, prior to polymerization. Under LSCM, the fluorescence staining for live and dead cells showed a 30% viability of yeast cells entrapped within the PNIPAm matrix after 45 min of photopolymerization, but an improvement to 60% viability in the presence of PEGMa. The thermoresponsive behavior of the microcapsules allows the silicone oil cores to be irreversibly ejected, and so the role of the silicone oil is 2-fold. It facilitates multifunctionality in the microcapsule by first being used as a template to obtain the desired core-shell morphology, and second it can act as an encapsulant for oil-soluble drugs. It was shown that the encapsulated oil droplets were expelled above the volume phase transition temperature of the polymer, while the collapsed microcapsule remained intact. When these microcapsules were reswollen with an aqueous solution, it was observed that the hollow compartments refilled. In principle, these hollow-core microcapsules could then be filled with water-soluble drugs that could be delivered in vivo in response to temperature.     

The Effect of Wall Material Type on the Encapsulation Efficiency and Oxidative Stability of Fish Oils

Fish oil is the primary source of long-chain omega-3 fatty acids, which are important nutrients that assist in the prevention and treatment of heart disease and have many health benefits. It also contains vitamins that are lipid-soluble, such as vitamins A and D. This work aimed to determine how the wall material composition influenced the encapsulation efficiency and oxidative stability of omega fish oils in spray-dried microcapsules. In this study, mackerel, sardine waste oil, and sand smelt fish oil were encapsulated in three different wall materials (whey protein, gum Arabic (AG), and maltodextrin) by conventional spray-drying. The effect of the different wall materials on the encapsulation efficiency (EE), flowability, and oxidative stability of encapsulated oils during storage at 4 °C was investigated. All three encapsulating agents provided a highly protective effect against the oxidative deterioration of the encapsulated oils. Whey protein was found to be the most effective encapsulated agent comparing to gum Arabic and maltodextrin. The results indicated that whey protein recorded the highest encapsulation efficiency compared to the gum Arabic and maltodextrin in all encapsulated samples with EE of 71.71%, 68.61%, and 64.71% for sand smelt, mackerel, and sardine oil, respectively. Unencapsulated fish oil samples (control) recorded peroxide values (PV) of 33.19, 40.64, and 47.76 meq/kg oil for sand smelt, mackerel, and sardine oils after 35 days of storage, while all the encapsulated samples showed PV less than 10 in the same storage period. It could be concluded that all the encapsulating agents provided a protective effect to the encapsulated fish oil and elongated the shelf life of it comparing to the untreated oil sample (control). The results suggest that encapsulation of fish oil is beneficial for its oxidative stability and its uses in the production of functional foods.