苹果籽油CO2超临界流体萃取及微胶囊化研究

1、苹果籽油CO2超临界流体萃取及微胶囊化研究摘 要本研究以苹果籽为原料，利用CO2超临界萃取技术，采用单因素试验的方法，对CO2超临界流体萃取苹果籽精油的影响因素进行了考察；采用正交试验对萃取工艺条件进行了优化，并与溶剂法浸提的苹果籽精油进行了品质的比较；气相色谱分析表明苹果籽精油富含不饱和脂肪酸（91.81，其中亚油酸含量59.54），具有较好的开发利用价值。采用“气流式锐孔凝固浴法”实现了苹果籽精油的微胶囊化，为苹果深加工开拓了新的途径。研究结果表明：CO2超临界萃取苹果籽油的工艺是可行的。萃取压力、萃取温度、CO2流量、原料粉碎度以及萃取时间对苹果籽油萃取率的影响较大，影响程度大小依次为萃

2、取压力萃取温度原料粉碎度CO2流量萃取时间，其中萃取压力和萃取温度对苹果籽油萃取率的影响显著。最佳工艺条件为：原料破碎度50目、一次投料量300g、萃取压力3035MPa、萃取温度3035、CO2流量25kg/h、萃取时间、分离压力8MPa、分离温度45。在此条件下苹果籽油萃取率可达苹果籽油/100g苹果籽。苹果籽油的超临界CO2萃取优于溶剂法萃取。超临界萃取所得的苹果籽精油萃取率高于溶剂法萃取，且油品质优良，无溶剂残留，适于微胶囊包埋。试验采用“气流式锐孔凝固浴法”实现了苹果籽油的微胶囊化。以对微胶囊外形及颗粒均匀度等产品效果为衡量指标，确定了以海藻酸钠作为壁材，浓度为2.5%，氯化钙为固化

3、剂，浓度为2.0%；乳化剂为单干酯和吐温-80的复合物，配比为0.2% 单干酯0.1% 吐温-80；壁材与芯材的比例为1：1。在气流式锐孔凝固浴法喷雾造粒过程中，物料流速、物料粘度、喷雾造粒液面距、喷雾气体压力对微胶囊产品状态质量有较大影响。试验结果表明，喷雾造粒工艺参数对微胶囊产品状态质量的影响主次为：物料粘度喷雾气体压力物料流速喷雾造粒液面距。最优工艺参数为mL/s，物料粘度2360mPa·s，喷雾造粒液面距300400mm，喷雾气体压力0.10MPa。干燥方式对微胶囊的包埋率及产品状态质量影响明显。试验结果表明：从干燥时间、温度、产品外观等综合考虑，流化床干燥为苹果籽精油微胶囊

4、产品的首选干燥方式；恒温干燥次之，真空冷冻干燥效果较差，自然干燥对产品影响最大，干燥效果最差。苹果籽精油微胶囊产品收得率67.35%，包埋率88.37%；颜色乳白，气味纯正；电镜观察结果表明，微胶囊产品具有较好的包埋效果，且颗粒均匀，大多呈球状，表面较光滑；产品干燥不结块，流动性好。关键词：苹果籽油；CO2超临界流体；萃取；脂肪酸；微胶囊STUDIES ON SUPERCRITICAL CARBON DIOXIDE FLUID EXTRACTION AND MICRO-ENCAPSULATION TECHNOLOGY OF APPLE SEEDS OILABSTRACTSupercritica

5、l CO2 fluid extraction was applied to apple seeds extraction. The effect factories on the supercritical extraction were worked out via single factor experiments, and the operative parameters were optimized by use orthogonal experiment. The oil with SCFE-CO2 under optimal conditions was compared to c

6、rude oil extracted by petroleum ether. GC analysis showed that apple seeds oil contained plenty of unsaturated acid (the unsaturated fatty acids are 91.81%，the content of linoleic acid are 59.54%), so apple seeds oil is available for further studying and exploiting. At same time, this study achieves

7、 apple seed oil micro-encapsulation with method of “tiny hole and solidifying bath”, find a new road for apple process.Results of the study indicate:The Technology of extracting apple seeds oil by Supercritical CO2 fluid extraction is feasible. The results indicated that the extraction rate of apple

8、 seeds oil was affected by extraction pressure，extraction temperature, carbon dioxide flow rate, particle size of material and extracting time. And extraction pressureextraction temperatureparticle size of materialcarbon dioxide flow rateextracting time. Extraction pressure and extraction temperatur

9、e is the most important factor. The optimum technological condition of extraction: particle size 50 meshes, material weights 300g,working pressure 3035MPa, temperature 3035, carbon dioxide flow rate 25kg/h, extracting time , separate pressure 8MPa, separate temperature 45. In this condition, the ext

10、raction yield of apple seeds oil is in 100g apple seed.Through the comparing test，the results showed that extraction of SCFE is excelled than petroleum ether, and extraction rate of apple seeds oil is higher than organic solvent. The product quality is unparalleled by SCFE, without remainder solvent

11、, so it is adapted to be embedded with micro-encapsulation.Study on apple seed oil micro-encapsulation with method of “tiny hole and solidifying bath”, weigh the figure and structure of microcapsule, The results showed that the wall-material was 2.5% sodium alginate, and microcapsule by spray with t

12、he solidifying bath of solution of % CaCl2, the mixture of 0.2% Glycerin Monostearate and 0.1% Tween-80 as emulsifiable solution, the scale of wall material and center material is 1:1.Materiel velocity, materiel viscidity, distance between the nozzle and the solidifying bath, and pressure of sprayin

13、g gas are the main factors when producing microcapsule by spray with tiny hole and solidifying bath. The results indicated that the embedded rate and quality of the microcapsule product was affected ordinal by materiel viscidity, pressure of spraying gas, materiel velocity, distance between the nozz

14、le and the solidifying bath. The optimal micro-encapsulation condition showed that materiel velocity is mL/s, materiel viscidity is 2360mPa·s, the distance between the nozzle and the solidifying bath is 300400mm, and pressure of spraying gas is 0.10MPa。The drying means obviously affect the embe

15、dded rate and quality of the microcapsule product. The results indicated that, consider as a whole of drying-time, temperature, shape and so on, continuous fluid-bed dryer is preferred means of dryness for microcapsule, natural desiccation has unfavorable effect on the product, the others drying mot

16、hers for the microcapsule product was affected ordinal by constant temperature desiccation, vacuum and freezing desiccation, natural desiccation。The gain ratio of apple seeds oil microcapsule product is 67.35%, the embedded rate is 88.37%. The product is milky, and the smell is pure. The observation of structure of apple seeds oil microcapsule under the SEM indicates that the p