山葡萄籽油的提取及微胶囊化研究
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摘要
本研究以山葡萄籽为原料,利用超临界CO_2萃取技术,对影响山葡萄籽油萃取的工艺条件进行了系统研究,并对不同方法提取的山葡萄籽油的理化指标和营养成分进行了分析对比;同时对喷雾干燥法制备微胶囊化山葡萄籽油粉末油脂的工艺进行了研究,对微胶囊产品的质量进行了评定,并预测了其保质期。研究结果表明:
1.超临界CO_2萃取山葡萄籽油的最佳生产工艺参数为:原料粉碎度60目、萃取温度35℃、萃取压力30Mpa、萃取时间160min。在此条件下,山葡萄籽油的提取率可达18.31%。
2.溶剂法提取山葡萄籽油的最佳工艺参数为:石油醚(60-90)为浸提剂、葡萄籽粉碎粒度为60目、温度95℃、浸提时间3h、料液比1g:7mL。在此条件下,山葡萄籽油的粗油提取率可达21.6%。对提取得到的粗油制品进行精炼加工,其收率为87.3%。
3.对超临界CO_2萃取得到的山葡萄籽油和溶剂法提取且经过精炼的山葡萄籽油的理化和卫生指标测定分析发现,超临界CO_2萃取出的山葡萄籽油的主要指标均优于溶剂法浸提后精炼得到的山葡萄籽油,具有很高的营养价值。说明超临界流体萃取技术在天然油脂提取方面具有无可比拟的优势。
4.微胶囊化山葡萄籽油的最佳乳化条件为:阿拉伯树胶为壁材,麦芽糊精为壁材填充物;复合乳化剂配比(单甘酯:蔗糖酯)为1:9;乳化温度为80℃;乳化剂用量0.75%;壁材用量20%;壁材比(阿拉伯树胶:麦芽糊精)为1:5;油/壁材为0.5。喷雾干燥法制备山葡萄籽油微胶囊的最佳工艺参数为:进料温度50℃～60℃、均质压力40MPa、进风温度180℃、出风温度80℃、喷雾压力180 KPa。在此工艺条件下微胶囊化效率可达77.36%。
5.喷雾干燥法制取的微胶囊化山葡萄籽油粉末油脂为乳白色粉末,密度0.7312g/cm~3,水分含量2.76%,溶解度94.0%。通过扫描电镜观察,微胶囊颗粒较圆整,基本接近球形,平均颗粒直径3.6±0.75μm。
6.贮藏稳定性实验表明,经微胶囊化的山葡萄籽油,其贮藏稳定性要明显优于未微胶囊化的山葡萄籽油以及添加了抗氧化剂V_E的山葡萄籽油制品。三种产品的货架期分别为:在室温条件下,微胶囊化山葡萄籽油粉末油脂可以保存140天,添加抗氧化剂V_E的山葡萄籽油可以保存102天,而没有经过微胶囊化处理的山葡萄籽油只能保存46天。
This research takes the Amur grape seed as raw material. The various factors that had effects on the extraction efficiency of the grape seed oil were systematically studied with supercritical carbon dioxide fluid extraction (SCF-CO2) technology. Oil from Amur grape seeds with two methods of SCF-CO2 and refining after organic solvent extraction was extracted. The physical and chemical index and the nourishment composition of Amur grape seeds oil were mensurated. The method of preparing Amur grape seed oil microcapsule by spray-drying was confirmed. The characters of microcapsuled Amur grape seed oil prepared by spray drying technique was valued, and its period of validity was predicted. The results showed that:
1. Extraction of oil from Amur grape seeds with supercritical CO_2 was studied. The results showed that the optimal comminution granularity, pressure, temperature and extraction time were 60, 30 Mpa, 35℃and 160min. On this condition, the production rate of the oil from Amur grape seeds can reach 18.31%.
2. Extraction of oil from Amur grape seeds with organic solvent was studied. Through experiment, the optimal solvent, comminution granularity, temperature, extraction time and the proportionment of raw material and solvent were petroleum aether, 60 mu. 95℃. 3 h and 1 : 7. On this condition, the production rate of the raw oil from Amur grape seeds can reach 21.6%. The rate of refined oil was 87.3%.
3. Oil from Amur grape seeds with two methods of SCF-CO_2 and refining after organic solvent extraction was extracted. The physical and chemical index and the nourishment composition of Amur grape seeds oil were mensurated. The results showed that oil by SCF-CO_2 extraction excelled the refined oil in main index. The Amur grape seed oil is a kind edible oil of high quality.
4. The optimum condition of the emulsifying technique were obtained in the preparation of Amur grape seeds oil microcapsules by spray-drying. The result was as follows: the ratio of glycerol monoester to sucrose fatty acid ester was 1 : 9, the temperature of emulsifying was 80℃, the content of emulsifier was 0.75%. the concentration of emulsion was 20%. the ratio of arabin to maltodextrane was 1: 5, the ratio of oil to wall was 0.5.
The optimum spray dehydration technological parameters were confirmed. The result of the orthogenesis test indicates that the optimum parameters about microencapsulated Amur grape seeds oil techniques were as follows: the feed temperature was about 50℃～~60℃, the homogenizing pressure was 40 MPa, the temperatures of inlet wind and outlet wind were 180℃and 80℃respectively, the spray pressure was 180 KPa. The microencapsulating efficiency of Amur grape seeds oil was about 77.36% on the condition above.
5. The characters of microcapsuled Amur grape seeds oil prepared by spray drying technique was valued. The preparation of Amur grape oil showed milkiness in colour. The density, the content of moisture and solubility were about 0.7312 g/cm~3, 2.76% and 94.0%. It provided with certain dispersion and admixture.
6. Through experiment, the preserved stability of microcapsuled Amur grape seeds oil excelled other production. The storage life of three kind of production were 140, 102, 46 days, respectively.
1.超临界CO_2萃取山葡萄籽油的最佳生产工艺参数为:原料粉碎度60目、萃取温度35℃、萃取压力30Mpa、萃取时间160min。在此条件下,山葡萄籽油的提取率可达18.31%。
2.溶剂法提取山葡萄籽油的最佳工艺参数为:石油醚(60-90)为浸提剂、葡萄籽粉碎粒度为60目、温度95℃、浸提时间3h、料液比1g:7mL。在此条件下,山葡萄籽油的粗油提取率可达21.6%。对提取得到的粗油制品进行精炼加工,其收率为87.3%。
3.对超临界CO_2萃取得到的山葡萄籽油和溶剂法提取且经过精炼的山葡萄籽油的理化和卫生指标测定分析发现,超临界CO_2萃取出的山葡萄籽油的主要指标均优于溶剂法浸提后精炼得到的山葡萄籽油,具有很高的营养价值。说明超临界流体萃取技术在天然油脂提取方面具有无可比拟的优势。
4.微胶囊化山葡萄籽油的最佳乳化条件为:阿拉伯树胶为壁材,麦芽糊精为壁材填充物;复合乳化剂配比(单甘酯:蔗糖酯)为1:9;乳化温度为80℃;乳化剂用量0.75%;壁材用量20%;壁材比(阿拉伯树胶:麦芽糊精)为1:5;油/壁材为0.5。喷雾干燥法制备山葡萄籽油微胶囊的最佳工艺参数为:进料温度50℃～60℃、均质压力40MPa、进风温度180℃、出风温度80℃、喷雾压力180 KPa。在此工艺条件下微胶囊化效率可达77.36%。
5.喷雾干燥法制取的微胶囊化山葡萄籽油粉末油脂为乳白色粉末,密度0.7312g/cm~3,水分含量2.76%,溶解度94.0%。通过扫描电镜观察,微胶囊颗粒较圆整,基本接近球形,平均颗粒直径3.6±0.75μm。
6.贮藏稳定性实验表明,经微胶囊化的山葡萄籽油,其贮藏稳定性要明显优于未微胶囊化的山葡萄籽油以及添加了抗氧化剂V_E的山葡萄籽油制品。三种产品的货架期分别为:在室温条件下,微胶囊化山葡萄籽油粉末油脂可以保存140天,添加抗氧化剂V_E的山葡萄籽油可以保存102天,而没有经过微胶囊化处理的山葡萄籽油只能保存46天。
This research takes the Amur grape seed as raw material. The various factors that had effects on the extraction efficiency of the grape seed oil were systematically studied with supercritical carbon dioxide fluid extraction (SCF-CO2) technology. Oil from Amur grape seeds with two methods of SCF-CO2 and refining after organic solvent extraction was extracted. The physical and chemical index and the nourishment composition of Amur grape seeds oil were mensurated. The method of preparing Amur grape seed oil microcapsule by spray-drying was confirmed. The characters of microcapsuled Amur grape seed oil prepared by spray drying technique was valued, and its period of validity was predicted. The results showed that:
1. Extraction of oil from Amur grape seeds with supercritical CO_2 was studied. The results showed that the optimal comminution granularity, pressure, temperature and extraction time were 60, 30 Mpa, 35℃and 160min. On this condition, the production rate of the oil from Amur grape seeds can reach 18.31%.
2. Extraction of oil from Amur grape seeds with organic solvent was studied. Through experiment, the optimal solvent, comminution granularity, temperature, extraction time and the proportionment of raw material and solvent were petroleum aether, 60 mu. 95℃. 3 h and 1 : 7. On this condition, the production rate of the raw oil from Amur grape seeds can reach 21.6%. The rate of refined oil was 87.3%.
3. Oil from Amur grape seeds with two methods of SCF-CO_2 and refining after organic solvent extraction was extracted. The physical and chemical index and the nourishment composition of Amur grape seeds oil were mensurated. The results showed that oil by SCF-CO_2 extraction excelled the refined oil in main index. The Amur grape seed oil is a kind edible oil of high quality.
4. The optimum condition of the emulsifying technique were obtained in the preparation of Amur grape seeds oil microcapsules by spray-drying. The result was as follows: the ratio of glycerol monoester to sucrose fatty acid ester was 1 : 9, the temperature of emulsifying was 80℃, the content of emulsifier was 0.75%. the concentration of emulsion was 20%. the ratio of arabin to maltodextrane was 1: 5, the ratio of oil to wall was 0.5.
The optimum spray dehydration technological parameters were confirmed. The result of the orthogenesis test indicates that the optimum parameters about microencapsulated Amur grape seeds oil techniques were as follows: the feed temperature was about 50℃～~60℃, the homogenizing pressure was 40 MPa, the temperatures of inlet wind and outlet wind were 180℃and 80℃respectively, the spray pressure was 180 KPa. The microencapsulating efficiency of Amur grape seeds oil was about 77.36% on the condition above.
5. The characters of microcapsuled Amur grape seeds oil prepared by spray drying technique was valued. The preparation of Amur grape oil showed milkiness in colour. The density, the content of moisture and solubility were about 0.7312 g/cm~3, 2.76% and 94.0%. It provided with certain dispersion and admixture.
6. Through experiment, the preserved stability of microcapsuled Amur grape seeds oil excelled other production. The storage life of three kind of production were 140, 102, 46 days, respectively.
引文
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