CN105662921B - 一种冷冻干燥油体的制备方法 - Google Patents
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Abstract
本发明公开了一种冷冻干燥油体的制备方法，它包括:用含有（重量）0.03‑0.05%尼泊金甲酯+0.03‑0.05%尼泊金丙酯，pH8.0‑8.5的PBS溶液，分别制备成油体PBS乳液和甘露醇PBS溶液，将上述的两种溶液等体积并流加入容器中，边加入边搅拌，得到油体甘露醇PBS乳液，油体的终浓度为0.05‑0.20克/ml，甘露醇的终浓度为油体的0.8‑3倍，预冷冻后，冷冻干燥机中干燥获得。室温放置6个月后，油体冻干粉的外观粒径均匀，颜色无明显变化，重新溶解水化容易。水后显微镜结构检测，无大油滴，质地均匀，细菌检测无菌落。本方法解决了油体不易保存的问题，方便保存及运输，降低了甘露醇的含量，为更好地利用油体生产食品、化妆品及药品奠定了基础。
Description
技术领域
本发明属食品深加工、化妆品及药品领域，具体地说是一种冷冻干燥油体的制备方法。
背景技术
油体是植物细胞中最小的细胞器。有时也被称为油滴、脂滴颗粒或圆球体的细胞器，油体为直径 0.5-2.5μm 的球体,油体的大小因植物种类和品种的不同而不同,且会受到营养和环境的影响。在同一粒种子的不同组织细胞中,油体的大小也会有所不同。在电镜下,油体的外部是一层致密的膜,内部为不透明的基质。从生理学的角度来说,若油体的直径小于 0.2μm,需要消耗大量的磷脂(PL)和油体蛋白(oleosin),相反如果油体的直径大于2.5μm,由于表面积过小,脂酶不能迅速水解脂类为植物生长提供所需的能量。油体主要组成为:中性脂类(92%-98%)、PL(1%-4%)和油体相关蛋白(1%-4%)。油体中也含有少量的细胞色素 C 还原酶,某些植物的油体中还含有脂酶和酰基甘油酶。植物种子经长期贮存,油体分子之间不会相互聚合,这是由于油体表面的电荷和oleosin 的存在。最近有研究表明，油体表面的蛋白主要为 oleosin,同时也镶嵌少量caleosin 等其他蛋白。
油体结合蛋白可以作为一种天然的乳化剂,而在油体表面,油体结合蛋白中带有电负性的残基使整个油体是带负电的,成熟种子的 pH 值是接近中性的,所以整个油体是较稳定的。在另一方面,油体蛋白的空间位阻作用,也可能阻止了油体的凝聚,使油体分散在水溶液中时可以形成稳定的乳液。
油体在化妆品和食品中都有广泛的应用，由于油体的特性，大多以乳剂的形式保存。而且保存时间很短，只有几天时间。为了延长保存时间、方便运输，人们偿试了很多方法对油体进行干燥。但是效果都不理想，大多出现油体聚集，聚集形成大的油滴；重新溶解，水化难，油体蛋白降解，失去了油体的原有特性。特别是在应用到化妆品时，不能达到原有的效果。
发明内容
本发明的目的是为解决干燥后的油体聚集形成大的油滴，水化难，油体蛋白降解，油体结构改变的问题，而提供甘露醇含量低的一种冷冻干燥油体的制备方法。
一种冷冻干燥油体的制备方法，它包括：
1）PBS溶液： pH8.0-8.5的PBS溶液；
2）油体PBS乳液：纯化的植物油体在上述的PBS溶液中重悬，制备成油体PBS乳液；
3）甘露醇PBS溶液：将甘露醇溶解至上述的PBS溶液中， 制备甘露醇PBS溶液，所述的甘露醇PBS溶液包括过饱和甘露醇PBS溶液；
4）油体甘露醇PBS乳液：将油体PBS乳液和甘露醇PBS溶液，并流加入容器中，边加入边搅拌，得到油体甘露醇PBS乳液，油体的终浓度为0.05 -0.20克/ml， 甘露醇的终浓度为油体的0.8-3倍。
5）将油体甘露醇PBS乳液预冷冻，置于冷冻干燥机中干燥得油体冻干粉；
所述的油体PBS乳液和甘露醇PBS溶液的体积比按4-6：4-6，并流加入；
所述的体积比1：1；
所述的油体终浓度为0.05-0.20克/ml，甘露醇的终浓度为油体的0.8-2倍；
所述的油体终浓度为0.05-0.10克/ml，甘露醇的终浓度为油体的0.8倍；
所述的预冷冻为-20℃冷冻1h，后转移至-80℃冷冻23小时；
所述的PBS溶液还含有（重量）0.03-0.05%尼泊金甲酯，0.03-0.05%尼泊金丙酯。
本发明提供了一种冷冻干燥油体的制备方法，它包括：用含有（重量）0.03-0.05%尼泊金甲酯+0.03-0.05%尼泊金丙酯，pH8.0-8.5的PBS溶液，分别制备成油体PBS乳液和甘露醇PBS溶液，将上述的两种溶液等体积并流加入容器中，边加入边搅拌，得到油体甘露醇PBS乳液，油体的终浓度为0.05 -0.20克/ml，甘露醇的终浓度为油体的0.8-3倍，预冷冻后，冷冻干燥机中干燥获得。室温放置6个月后，油体冻干粉的外观粒径均匀，颜色无明显变化，重新溶解水化容易。水后显微镜结构检测，无大油滴，质地均匀，细菌检测无菌落。本方法解决了油体不易保存的问题，方便保存及运输，降低了甘露醇的含量，为更好地利用油体生产食品、化妆品及药品奠定了基础。
附图说明
图1 含油体10%的油体PBS乳液中添加0%甘露醇制备的油体冻干粉照片；
图2 含油体10%的油体PBS乳液中添加1%甘露醇制备的油体冻干粉照片；
图3 含油体10%的油体PBS乳液中添加2%甘露醇制备的油体冻干粉照片；
图4 含油体10%的油体PBS乳液中添加3%甘露醇制备的油体冻干粉照片；
图5 含油体10%的油体PBS乳液中添加4%甘露醇制备的油体冻干粉照片；
图6 含油体10%的油体PBS乳液中添加5%甘露醇制备的油体冻干粉照片；
图7 含油体10%的油体PBS乳液中添加6%甘露醇制备的油体冻干粉照片；
图8 含油体10%的油体PBS乳液中添加7%甘露醇制备的油体冻干粉照片；
图9 含油体10%的油体PBS乳液中添加8%甘露醇制备的油体冻干粉照片；
图10 含油体10%的油体PBS乳液中添加9%甘露醇制备的油体冻干粉照片；
图11 含油体10%的油体PBS乳液中添加10%甘露醇制备的油体冻干粉照片；
图12 含油体10%的油体PBS乳液中添加30%甘露醇制备的油体冻干粉照片；
图13 含油体10%的油体PBS乳液中添加50%甘露醇制备的油体冻干粉照片；
图14 含油体10%的油体PBS乳液中添加70%甘露醇制备的油体冻干粉照片；
图15 含油体10%的油体PBS乳液中添加90%甘露醇制备的油体冻干粉照片；
图16 含油体10%的油体PBS乳液中添加0%甘露醇制备的油体冻干粉显微照片；
图17 含油体10%的油体PBS乳液中添加1%甘露醇制备的油体冻干粉显微照片；
图18 含油体10%的油体PBS乳液中添加2%甘露醇制备的油体冻干粉显微照片；
图19 含油体10%的油体PBS乳液中添加3%甘露醇制备的油体冻干粉显微照片；
图20 含油体10%的油体PBS乳液中添加4%甘露醇制备的油体冻干粉显微照片；
图21 含油体10%的油体PBS乳液中添加5%甘露醇制备的油体冻干粉显微照片；
图22 含油体10%的油体PBS乳液中添加6%甘露醇制备的油体冻干粉显微照片；
图23 含油体10%的油体PBS乳液中添加7%甘露醇制备的油体冻干粉显微照片；
图24 含油体10%的油体PBS乳液中添加8%甘露醇制备的油体冻干粉显微照片；
图25 含油体10%的油体PBS乳液中添加9%甘露醇制备的油体冻干粉显微照片；
图26 含油体10%的油体PBS乳液中添加10%甘露醇制备的油体冻干粉显微照片；
图27 含油体10%的油体PBS乳液中添加30%甘露醇制备的油体冻干粉显微照片；
图28 含油体10%的油体PBS乳液中添加50%甘露醇制备的油体冻干粉显微照片；
图29 含油体10%的油体PBS乳液中添加70%甘露醇制备的油体冻干粉显微照片；
图30 含油体10%的油体PBS乳液中添加90%甘露醇制备的油体冻干粉显微照片；
图31 含油体10%的油体PBS乳液中添加8%甘露醇制备的油体冻干粉重新溶解水化显微照片。
具体实施方式
实施例1 红花油体纯化
将红花种子浸泡在蒸馏水中(1:5，W/V)放置于 4-6℃ 冰箱中 20 h，然后将浸泡后的植物种子置于含有氯化钠和蔗糖的 Tris-HCl 缓冲溶液(1:5，W/V，50 mmol/LTris-HCl, pH 7.5, 0.4 mol/L 蔗糖，0.5 mol/L 氯化钠)中，用榨汁搅拌机搅拌 180s得到植物种子的匀浆液。用三层滤布过滤除去渣滓，滤出液在 4℃，9600 rpm/min 的条件下离心30min，收集最上层乳状的物质。上层的乳状物质均匀分散在上述的含有氯化钠和蔗糖的Tris-HCl 缓冲溶液(1:1，W/V)中，在 4℃，9600 rpm/min 的条件下离心 30 min，收集最上层乳状的物质。得到的上层乳状物质均匀分散在 Tris-HCl 缓冲溶液(1:5，W/V，50mmol/LTris-HCl, pH 7.5)中，4℃，9600 rpm/min，重复分散在缓冲溶液中和离心分离 3次，将得到的上层乳状物质(即植物油体)放置于 4℃冰箱中备用，用前最多放置 2 d。
实施例2 含红花油体PBS乳液（pH8.0）加入不同浓度甘露醇制成油体冻干粉对比结果；
0.20克/ml的油体PBS乳液（pH8.0），分别与甘露醇含量为0.02克/ml、0.04克/ml、0.06克/ml、0.08克/ml、0.10克/ml、0.12克/ml、0.14克/ml、0.16克/ml、0.18克/ml、0.20克/ml、0.60克/ml、1.00克/ml、1.40克/ml、1.80克/ml的甘露醇PBS溶液，所述的甘露醇PBS溶液包括过饱和甘露醇PBS溶液，等体积并流缓慢加入容器中，边加入边搅拌，混匀后，-80℃预冷24h后，置于冷冻干燥机中干燥成油体冻干粉。
在含油体10%的油体PBS乳液中添加1%、2%、3%、4%、5%、6%、7%、8%、9%、10%、30%、50%、70%、90%甘露醇，并将该乳液混匀分装后冷冻干燥制备干燥油体（表1）。结果见图1-31。
从图中可以看出，终浓度为含油体10%、甘露醇1-7%油体甘露醇PBS乳液制成的冻干粉，有团聚现象，有大油滴出现，说明油体结构被破坏。甘露醇50-90%油体甘露醇PBS乳液制成的冻干粉，颜色发黄。
实施例3 油体再悬浮、制备油体乳液、油体冷冻干燥
1）PBS溶液：含有（重量）0.03-0.05%尼泊金甲酯+0.03-0.05%尼泊金丙酯，pH8.0-8.5的PBS溶液；
2）油体PBS乳液：纯化的植物油体在上述的PBS溶液中重悬，制备成油体PBS乳液；
3）甘露醇PBS溶液：将甘露醇溶解至上述的PBS溶液中， 制备甘露醇PBS溶液；
4）油体甘露醇PBS乳液：将油体PBS乳液和甘露醇PBS溶液并流缓慢加入容器中，边加入边搅拌；得到油体甘露醇PBS乳液，油体的终浓度为0.05-0.20克/ml， 甘露醇的终浓度为油体的0.8-3倍。
5）将油体甘露醇PBS乳液预冷冻，置于冷冻干燥机中干燥得油体冻干粉。
实施例4 油体冻干粉稳定性分析0.20克/ml的红花油体PBS乳液（pH8.0）（油体终浓度为10%），与甘露醇含量为0.16克/ml甘露醇PBS溶液（甘露醇终浓度8%），等量并流加入，边加入边搅，不同预冻条件对油体固体化的影响。
粒径均一，无明显聚集。
室温放置6个月后，油体冻干粉的外观粒径均匀，颜色无明显变化，重新溶解水化容易。水后显微镜结构检测，无大油滴，质地均匀（见图31），细菌检测无菌落。
Claims (7)
1.一种冷冻干燥油体的制备方法，它包括：
1）PBS溶液： pH8.0-8.5的PBS溶液；
2）油体PBS乳液：纯化的植物油体在上述的PBS溶液中重悬，制备成油体PBS乳液；
3）甘露醇PBS溶液：将甘露醇溶解至上述的PBS溶液中， 制备甘露醇PBS溶液，所述的甘露醇PBS溶液包括过饱和甘露醇PBS溶液；
4）油体甘露醇PBS乳液：将油体PBS乳液和甘露醇PBS溶液，并流加入容器中，边加入边搅拌，得到油体甘露醇PBS乳液，油体的终浓度为0.05 -0.20克/ml， 甘露醇的终浓度为油体的0.8-3倍；
5）将油体甘露醇PBS乳液预冷冻，置于冷冻干燥机中干燥得油体冻干粉。
2.根据权利要求1所述的一种冷冻干燥油体的制备方法，其特征在于：所述的油体PBS乳液和甘露醇PBS溶液的体积比按4-6：4-6，并流加入。
3.根据权利要求2所述的一种冷冻干燥油体的制备方法，其特征在于：所述的体积比1：1。
4.根据权利要求1、2或3所述的一种冷冻干燥油体的制备方法，其特征在于：所述的油体终浓度为0.05-0.20克/ml，甘露醇的终浓度为油体的0.8-2倍。
5.根据权利要求3所述的一种冷冻干燥油体的制备方法，其特征在于：所述的油体终浓度为0.05-0.10克/ml，甘露醇的终浓度为油体的0.8倍。
6.根据权利要求5所述的一种冷冻干燥油体的制备方法，其特征在于：所述的预冷冻为-20℃冷冻1h，后转移至-80℃冷冻23小时。
7.根据权利要求1或 6所述的一种冷冻干燥油体的制备方法，其特征在于：所述的PBS溶液还含有重量百分比为0.03-0.05%尼泊金甲酯，0.03-0.05%尼泊金丙酯。
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