Preparation and Characterization of Microcapsules by Heat Treated Myofibrillar Protein Coacervation
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摘要: 探索罗非鱼（Oreochromis niloticus）中提取肌原纤维蛋白（MP）在热处理后（HMP）作为一种新型微胶囊的壳材料，在海藻酸钠（SA）和壳聚糖（CS）共存下，采用超声复凝聚法对玉米油进行微胶囊化，并对其性能进行表征。结果表明：当海藻酸钠含量2.5%，HMP含量3.0%，玉米油含量30%时，乳液粒径小而均匀，乳化稳定性高。壳聚糖含量为1.2%、海藻酸钠和壳聚糖质量比1:1、氯化钙浓度为5.0%时，通过超声复凝聚法得到的微胶囊平均粒径为88.74±2.60 μm，包封率为82.59%±1.44%；微胶囊具有不规则形状和起伏的表面；红外光谱和X射线衍射结果表明，海藻酸钠与壳聚糖因静电结合作用，与HMP共同构成了微胶囊致密的外壳；DSC结果显示HMP微胶囊具有一定的热稳定性；HMP微胶囊显著降低了贮存过程中油脂的POV值与TBA值，有效延缓了玉米油的氧化速度；HMP微胶囊在整个模拟消化阶段的游离脂肪酸（FFA）释放量为92.67%，且在肠消化阶段释放更多的FFA，表明微胶囊化对芯材的释放起到了缓释作用。这项研究显示，HMP与海藻酸钠和壳聚糖复合后，是可以用于微胶囊制备及保护生物活性物质，为HMP的乳化应用扩展途径。
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关键词:
- 热处理肌原纤维蛋白（HMP） /
- 海藻酸钠 /
- 玉米油 /
- 微胶囊 /
- 性能表征
Abstract: Myogenic fibrin (MP) extracted from Tilapia (Oreochromis niloticus) after heat treatment (HMP) was explored as a novel encapsulant for microencapsulation of corn oil together with sodium alginate (SA) and chitosan (CS), and its performance was characterized using ultrasonic coalescence. The results showed that at 2.5% sodium alginate, 3.0% HMP content and 30% corn oil, the emulsion had small and uniform particle size with high emulsification stability. The average particle size of microcapsules after ultrasonic recondensation was 88.74±2.60 μm while the encapsulation rate was 82.59%±1.44% under the following conditions: 1.2% CS, SA:CS mass ratio of 1:1, and 5.0% calcium chloride. The microcapsules had irregular shapes and undulating surfaces, and the results of infrared spectroscopy and X-ray diffraction indicated that CS and SA formed the dense shell of microcapsules together with HMP due to electrostatic binding. Results from DSC showed that HMP microcapsules had a degree of thermal stability, and the microencapsulation significantly reduced the POV and TBA values of oil during storage, which effectively slowed down the oxidation process. The release of free fatty acids (FFA) from HMP microcapsules was 92.67% during the whole simulated digestion phase with a greater amount released during the intestinal digestion phase, indicating that microencapsulation had a retarding effect on the release of core material. This study shows that HMP compounded with sodium alginate and chitosan is feasible for microencapsulation and protection of bioactive substances, and hence expanding the applications of HMP microgel particles. -
图 3 HMP含量对HMP乳液微观结构的影响
Figure 3. Effect of HMP addition on the microstructure of HMP emulsion
图 4 HMP含量对SA-HMP乳液乳化稳定性和平均粒径的影响
Figure 4. Effect of HMP content on emulsification stability and average particle size of SA-HMP emulsion
图 5 玉米油含量对HMP乳液微观结构的影响
Figure 5. Effect of corn oil addition on the microstructure of HMP emulsion
图 6 玉米油含量对SA-HMP乳液乳化稳定性和平均粒径的影响
Figure 6. Effect of corn oil content on emulsification stability and average particle size of SA-HMP emulsion
图 7 不同壳聚糖含量对HMP微胶囊平均粒径及包封率的影响
Figure 7. Effect of different chitosan content on average particle size and encapsulation efficiency of HMP microcapsules
图 8 不同海藻酸钠/壳聚糖质量比对HMP微胶囊平均粒径及包封率的影响
Figure 8. Effect of different sodium alginate/chitosan mass ratio on the average particle size and encapsulation efficiency of HMP microcapsules
图 9 不同CaCl2浓度对HMP微胶囊平均粒径及包封率的影响
Figure 9. Effect of different CaCl2 potency on average particle size and encapsulation efficiency of HMP microcapsules
图 10 微胶囊水溶液（冻干前）超景深显微图像（A）、微胶囊超景深显微图像（B）、微胶囊宏观图像（C）
Figure 10. Microcapsule aqueous solution (before lyophilization) super-depth of field microscopic image (A), microcapsule super-depth of field microscopic image (B), microcapsule macroscopic image (C)
注：放大倍数：A：300×；B：600×。
图 11 微胶囊壁材、微胶囊和玉米油的红外光谱图
Figure 11. Infrared spectra of microcapsule wall materials, microcapsules and corn oil
注：a：HMP；b：海藻酸钠；c：壳聚糖；d：HMP微胶囊；e：玉米油。
图 12 微胶囊壁材和微胶囊的X射线衍射图
Figure 12. X-ray diffraction of microcapsule wall materials and microcapsules
图 13 玉米油、微胶囊壁材和微胶囊的差示扫描量热曲线
Figure 13. Differential scanning calorimetric curves of corn oil, microcapsule wall materials and microcapsules
注：a：玉米油；b：海藻酸钠；c：壳聚糖；d：HMP；e：HMP微胶囊。
图 14 储存期间玉米油和微胶囊POV值变化
Figure 14. POV trend of corn oil and microcapsules during storage
注：不同小写字母表示不同样品差异显著（P<0.05），图15同。
图 15 储存期间玉米油和微胶囊TBA值变化
Figure 15. TBA value trend of corn oil and microcapsules during storage
图 16 体外模拟胃肠消化过程中HMP微胶囊的FFA释放量
Figure 16. FFA release from HMP microcapsule during simulated gastrointestinal digestion in vitro
注：不同字母表示同一样品差异显著（P<0.05）。
表 1 微胶囊的理化性质
Table 1. Physicochemical properties of microcapsules
样品 水分含量
（%）水分活度 包封率
（%）粒径
（μm）润湿时间
（s）溶解度
（%）HMP
微胶囊2.82±0.76 0.19±0.01 82.59±1.44 88.74±2.60 37.00±4.00 6.17±1.76 
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