CN108272661B - 一种杜仲籽油微乳液的制备方法 - Google Patents
一种杜仲籽油微乳液的制备方法 Download PDFInfo
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
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Abstract
本发明公开了一种杜仲籽油微乳液的制备方法,该方法制备的杜仲籽油微乳液以生物表面活性剂、水酶法制备的杜仲籽油为主要原料,以助表面活性剂、乳化液、水为辅料,经转相乳化法制备而成。通过该方法制备的微乳液,不仅解决了杜仲籽油因不饱和脂肪酸含量高而不易贮藏的问题,而且减少了化学表面活性剂的应用,具有绿色安全的特性。同时,该杜仲籽油微乳液经干燥后的冻干粉,产品性质稳定,包封率较高,应用范围广。
Description
技术领域
本发明属于油脂加工技术领域,具体涉及一种杜仲籽油微乳液的制备方法。
背景技术
杜仲(Eucommia ulmoides Oliv.)为杜仲科(Eucommiaceae)植物,落叶乔木,是我国特有的单种科植物。研究发现:杜仲籽中的含油量为27%~33%,且富含不饱和脂肪酸,其中油酸为16%~18%,亚油酸为11%~13%,α-亚麻酸为61%~63%,这是目前所发现α-亚麻酸含量最高的天然植物油之一。α-亚麻酸是人体必需脂肪酸,属于ω-3系列脂肪酸,在人体内可代谢为EPA和DHA等多烯不饱和脂肪酸。药理实验证明,α-亚麻酸具有降血压,降低血脂和血小板凝固作用,抗肿瘤和增强人体免疫能力,促进神经系统、脑和视网膜的发育,延缓衰老等多种生理功能。此外,杜仲籽中还含有对人体有益的桃叶珊瑚甙等天然活性物质。由于杜仲籽油中的不饱和脂肪酸含量高,特别是α-亚麻酸的含量,因此其在加工、储存及应用过程中极易发生氧化反应,产生酸败味,这限制了杜仲籽油的应用范围。
微乳液是一种粒径在纳米级别的乳液体系,是一种水相、油相与大量表面活性剂和助表面活性剂混合后自发形成的透明或半透明体系,该体系是一种热力学稳定的分散体系,根据平衡状态的不同,微乳液可分为O/W型微乳液于与油相共存的多相体,W/O型微乳液与水共存的多相体系,油-水双连续微乳液共存的多相体系,单相微乳液四种不同的平衡体系,且一般均为球形,直径在10~100nm范围内。将不饱和脂肪酸含量高的易氧化油脂制备成微乳液,不仅有助于减缓油脂中不饱和脂肪酸的氧化速率,保护油脂的营养价值,而且微乳液本身具有良好的分散性和稳定性,这有助于拓宽油脂在药剂行业、农药行业及食品行业中的应用范围。
如中国专利(申请号201110099153.2)公开了一种核桃油微乳的制备方法,该方法分别以乳化剂和助乳化剂为原料,经乳化步骤后与水混合,制备了核桃油微乳。该制备方法具有增溶核桃油,降低核桃油腥味,减缓核桃油中不饱和脂肪酸的氧化,保护核桃油营养价值,改善产品品质,提高营养物质的生物利用率,拓展核桃油应用范围等优点。但是该发明中的乳化剂为聚氧乙烯氢化蓖麻油、吐温、苄泽、聚氧乙烯蓖麻油等化学合成的表面活性剂,这些物质具有一定的安全隐患,特别是用量较多时。
如中国专利(申请号201310230698.1)公开了一种山茶油微乳液及其制备方法,其中以重量百分比计,所述山茶油微乳液包括了5~70%的表面活性剂、2~30%的助表面活性剂、0.5~10%的液态脂肪酸、0.1~4%的山茶油和0~90%的水。该发明具有制备方法操作简单、组成配比设计合理,制备的山茶油微乳液具有产品外观澄清透明,稳定性好,液滴分散半径小的优点。但是该发明也采用了聚氧乙烯山梨醇酐单月桂酸酯、聚氧乙烯山梨醇酐单棕榈酸酯、聚氧乙烯山梨醇酐单硬脂酸酯、聚氧乙烯山梨醇酐单油酸酯和蔗糖脂肪酸酯等化学合成表面活性剂,产品存在有一定的安全隐患。同时该发明未具体指出所用山茶油的制备工艺,而制备工艺是影响油脂品质优劣及内含有效成分含量高低的一项重要因素。
如中国专利(申请号201410197367.7)公开了一种食品级月见草油微乳冻的干粉及其制备方法,该冻干粉原料配比按重量百分比计包括了:月见草油5%~8%,乳化剂30%~50%,冻干保护剂40%~60%。通过将上述成分制备成微乳,利用真空冷冻技术低温下干燥制成一种稳定性高、毒副作用小的适用于食品及保健品中的月见草油微乳冻干粉。该粉剂能在室温下长期保存,且冻干后较好地保持微乳原来的性质,加水后迅速恢复,更好的保护了易氧化的物质,有利于储存、运输和销售,该制品具有制备工艺简单,易于操作的优点。但是该发明也采用了化学合成表面活性剂,存在有一定的安全隐患,且未指明月见草油的制备工艺。
发明内容
针对上述问题,本发明目的在于提供一种杜仲籽油微乳液的制备方法,该方法不仅要解决杜仲籽油不饱和脂肪酸含量高、不易贮藏的问题,而且要能在保证产品绿色安全的基础上,拓宽杜仲籽油的应用范围。
一种杜仲籽油微乳液的制备方法,该方法中包括了制备杜仲籽油、制备微乳液2个步骤。
其中,步骤1)制备杜仲籽油的操作为:取杜仲籽粉末,向其加入超纯水,搅拌后得到杜仲籽油提取液;将提取液加热至80~100℃进行灭酶;待降至常温后调节提取液pH值,并以杜仲籽粉末质量0.5~5%的量添加水解酶;将提取液置于振荡仪内进行酶解反应,酶解完成后超声处理;将经超声处理的提取液在转速为3000~5000r/min的条件下离心,离心后分别收集上层杜仲籽油,中间层乳化液备用。
其中,步骤2)制备微乳液的操作为:以质量计,将22~31份经步骤1)制备的杜仲籽油、3~8份经步骤1)制备的中间层乳化液、18~23份复合表面活性剂、5~11份助表面活性剂混合后搅拌,搅拌的同时滴加57~73份的超纯水,待溶液混匀后既得杜仲籽油微乳液;其中所述的复合表面活性剂为鼠李糖脂或槐糖脂任一与化学合成表面活性剂的混合物,所述助表面活性剂是已醇、丙醇、正丁醇中的一种或多种的等量混合物。值得注意的是,一边搅拌一边滴加超纯水时,体系最初清透,随着超纯水的加入,体系开始变浑浊,在此过程中会出现凝胶状态,此时应快速加水,适当加大转速,让体系迅速渡过凝胶相,重新变得清透,逐渐形成微乳液。
作为优选方案,所述步骤1)中的杜仲籽粉末粒度为30~50目。
作为优选方案,所述步骤1)中杜仲籽粉末与添加超纯水的料液质量比为1∶6~11。
作为优选方案,所述步骤1)中的水解酶为选自纤维素酶、蛋白酶、果胶酶中的任意一种或多种的混合酶。
水酶法是以机械破碎为基础,使用对脂蛋白、脂多糖等复合体和细胞壁有降解作用的酶,促进油料固体释放出油脂。同时,根据非油成分(蛋白和碳水化合物)对油和水的亲和力不同、油水比重有差异的原理而将油和非油成分分离。相较于目前常用的浸出法、压榨法等油脂制备工艺,水酶法具有产品品质高,简化精炼、无溶剂残留等优点。同时,水酶法制备过程条件温和,无蒸炒等高温工序,产品中以亚麻酸为主的多不饱和脂肪酸等热敏性成分保存较好。除了考虑上述优势外,本发明选择以水酶法制备的杜仲籽油为原料的另一原因是:在试验中发现,在制备杜仲籽油微乳液的过程中,如果添加3~8份经步骤1)制备的中间层乳化液则能显著提高微乳液产品的稳定性,且在微乳液产品中能检测到桃叶珊瑚甙,其具体机理尚未明确,推测与复杂的相变过程有关。
作为优选方案,所述步骤2)中的化学合成表面活性剂为吐温、司盘、聚氧乙烯氢化蓖麻油中的任意一种。
步骤2)中所用的鼠李糖脂或槐糖脂均为生物表面活性剂。生物表面活性剂指利用酶或微生物等通过生物催化和生物合成等生物技术制备的集亲水和疏水性基团于一体的天然表面活性剂。生物表面活性剂具有优良的乳化性和起泡性,对热、pH的稳定性,而且无毒、生物可降解,与常见的吐温、司盘、聚氧乙烯氢化蓖麻油等化学表面活性剂相比,具有良好的环境兼容性,不会对环境造成不利影响。即使生物表面活性剂有如此诸多优点,但是由于其目前的生产成本过高,因此在食品工业中的应用并不广泛。发明人在比较了鼠李糖脂、槐糖脂、海藻糖脂、脂蛋白等多种生物表面活性剂后发现:无论选择何种生物表面活性剂,当其单独使用时,所制备微乳液的稳定性均较差,甚至当体系的温度改变时,微乳液出现分层;而将生物表面活性剂与化学合成表面活性剂混用时,则微乳液的稳定性显著性提高,特别是鼠李糖脂的联用效果最佳。
作为优选方案,所述步骤2)中搅拌转速为280~400转/分。
作为优选方案,所述制备过程中所用超纯水的含盐量在0.1mg/L以下,电导率小于0.1μs/cm。
作为改进方案,所述制备的杜仲籽油微乳液经干燥后以粉末态应用于食品、化妆品、日化等行业。杜仲籽油微乳液干燥成粉末态有助于保护其原有的活性物质,特别是不饱和脂肪酸等易氧化成分,同时粉末态产品便于储存、运输和销售。
具体实施方式
下面结合具体实施方式对本发明做进一步的说明,需要指出的是以下实施方式仅是以例举的形式对本发明所做的解释性说明,但本发明的保护范围并不仅限于此,所有本领域的技术人员以本发明的精神对本发明所做的等效的替换均落入本发明的保护范围。
实施例1
水酶法制备杜仲籽油
将清理、洗净后的杜仲籽干燥(55℃,12h),冷却至室温后粉碎过筛(40目),收集粉末以备用。取500g杜仲籽籽粉末于锥形瓶内,按1∶11g/mL的料液比加入超纯水,旋涡混匀2min,放置于水浴锅中灭酶(90℃,10min),冷却至室温后调pH至8,向其添加2.5g的碱性内切蛋白酶,并置于恒温振荡器(25转/分)内,控制酶解温度为53~55℃,反应完成后于水浴锅中再次灭酶(90℃,3min),并采用超声波处理酶解液10min。将酶解液进行离心(4000转/分,30min),并用移液管收集上层游离油和中间层乳化液备用。
实施例2
水酶法制备杜仲籽油
将清理、洗净后的杜仲籽干燥(55℃,12h),冷却至室温后粉碎过筛(50目),收集粉末以备用。取500g杜仲籽籽粉末于锥形瓶内,按1∶6g/mL的料液比加入超纯水,旋涡混匀2min,放置于水浴锅中灭酶(90℃,10min),冷却至室温后调pH至7.5,向其分别添加1.5g的果胶酶、1.5g的纤维素酶,并置于恒温振荡器(30转/分)内,控制酶解温度为45~58℃,反应完成后于水浴锅中再次灭酶(90℃,3min),并采用超声波处理酶解液10min。将酶解液进行离心(4000转/分,30min),并用移液管收集上层游离油和中间层乳化液备用。
实施例3
杜仲籽油微乳液的制备
以质量计,将22份实施例1~2制备的杜仲籽油、3份实施例1~2制备的中间层乳化液、18份复合表面活性剂(其中8份鼠李糖脂,10份吐温)、5份乙醇助表面活性剂混合,将上述混合液通过磁力搅拌器混匀,一边搅拌一边滴加去离子水,初始搅拌器的转速为280转/分,体系最初清透,随着去离子水的加入,开始变浑浊,在此过程中会出现凝胶状态,此时应快速加水,加大转速至400转/分,让体系迅速渡过凝胶相,重新变得清透,加入57份超纯水后即得杜仲籽油微乳液。
实施例4
杜仲籽油微乳液的制备
以质量计,将31份实施例1~2制备的杜仲籽油、8份实施例1~2制备的中间层乳化液、23份复合表面活性剂(其中15份鼠李糖脂,8份吐温)、11份乙醇助表面活性剂混合,将上述混合液通过磁力搅拌器混匀,一边搅拌一边滴加去离子水,初始搅拌器的转速为300转/分,体系最初清透,随着去离子水的加入,开始变浑浊,在此过程中会出现凝胶状态,此时应快速加水,加大转速至400转/分,让体系迅速渡过凝胶相,重新变得清透,加入73份超纯水后即得杜仲籽油微乳液。
实施例5
杜仲籽油微乳液的制备
以质量计,将27份实施例1~2制备的杜仲籽油、6份实施例1~2制备的中间层乳化液、20份复合表面活性剂(其中14份鼠李糖脂,6份司盘)、4份丙醇和4份正丁醇助表面活性剂混合,将上述混合液通过磁力搅拌器混匀,一边搅拌一边滴加去离子水,初始搅拌器的转速为290转/分,体系最初清透,随着去离子水的加入,开始变浑浊,在此过程中会出现凝胶状态,此时应快速加水,加大转速至390转/分,让体系迅速渡过凝胶相,重新变得清透,加入63份超纯水后即得杜仲籽油微乳液。
实施例6
杜仲籽油微乳液的制备
以质量计,将27份实施例1~2制备的杜仲籽油、6份实施例1~2制备的中间层乳化液、20份复合表面活性剂(其中16份槐糖脂,4份聚氧乙烯氢化蓖麻油)、4份丙醇和4份正丁醇助表面活性剂混合,将上述混合液通过磁力搅拌器混匀,一边搅拌一边滴加去离子水,初始搅拌器的转速为280转/分,体系最初清透,随着去离子水的加入,开始变浑浊,在此过程中会出现凝胶状态,此时应快速加水,加大转速至380转/分,让体系迅速渡过凝胶相,重新变得清透,加入63份超纯水后即得杜仲籽油微乳液。
实施例7
杜仲籽油微乳冻干粉的制备
以质量计,将26份实施例1~2制备的杜仲籽油、4份实施例1~2制备的中间层乳化液、19份复合表面活性剂(其中9份鼠李糖脂,10份吐温)、6份乙醇助表面活性剂混合,将上述混合液通过磁力搅拌器混匀,一边搅拌一边滴加去离子水,初始搅拌器的转速为320转/分,体系最初清透,随着去离子水的加入,开始变浑浊,在此过程中会出现凝胶状态,此时应快速加水,加大转速至400转/分,让体系迅速渡过凝胶相,重新变得清透,加入61份超纯水后即得杜仲籽油微乳液。将上述制备的微乳放入-40℃的冰箱内冻结12h,然后将其放入温度已降到零下65~71℃的真空冷冻干燥机内,冻干48h,既得杜仲籽油微乳冻干粉。
实施例8
杜仲籽油微乳液的制备
以质量计,将29份实施例1~2制备的杜仲籽油、5份实施例1~2制备的中间层乳化液、22份复合表面活性剂(其中16份鼠李糖脂,6份司盘)、8份乙醇助表面活性剂混合,将上述混合液通过磁力搅拌器混匀,一边搅拌一边滴加去离子水,初始搅拌器的转速为310转/分,体系最初清透,随着去离子水的加入,开始变浑浊,在此过程中会出现凝胶状态,此时应快速加水,加大转速至390转/分,让体系迅速渡过凝胶相,重新变得清透,加入68份超纯水后即得杜仲籽油微乳液。将上述制备的微乳放入-40℃的冰箱内冻结12h,然后将其放入温度已降到零下65~68℃的真空冷冻干燥机内,冻干48h,既得杜仲籽油微乳冻干粉。冻干粉呈现均匀的淡黄色针状结构,复水后再分散性好,复水后粒径为与冻干前相比粒径有所增大,冻干粉的性质稳定,包封率较高,不需冷藏,在室温干燥条件下贮存2个月无明显变化。
Claims (6)
1.一种杜仲籽油微乳液的制备方法,其特征在于所述方法包括了以下步骤:
1)制备杜仲籽油
取杜仲籽粉末,向其加入超纯水,搅拌后得到杜仲籽油提取液;将提取液加热至80~100°C进行灭酶;待降至常温后调节提取液pH值,并以杜仲籽粉末质量0.5~5%的量添加水解酶;将提取液置于振荡仪内进行酶解反应,酶解完成后超声处理;将经超声处理的提取液在转速为3000~5000 r/min的条件下离心,离心后分别收集上层杜仲籽油,中间层乳化液备用;所述水解酶为选自纤维素酶、蛋白酶、果胶酶中的任意一种或多种的混合酶;
2)制备微乳液
以质量计,将22~31份经步骤(1)制备的杜仲籽油、3~8份经步骤(1)制备的中间层乳化液、18~23份复合表面活性剂、5~11份助表面活性剂混合后搅拌,搅拌的同时滴加57~73份的超纯水,待溶液混匀后既得杜仲籽油微乳液;其中所述的复合表面活性剂为鼠李糖脂或槐糖脂任一与化学合成表面活性剂的混合物,所述助表面活性剂是已醇、丙醇、正丁醇中的一种或多种的等量混合物;所述化学合成表面活性剂为吐温、司盘、聚氧乙烯氢化蓖麻油中的任意一种。
2.如权利要求1所述的杜仲籽油微乳液制备方法,其特征在于,步骤(1)中的杜仲籽粉末粒度为30~50目。
3.如权利要求1所述的杜仲籽油微乳液制备方法,其特征在于,步骤(1)中杜仲籽粉末与添加超纯水的料液质量比为1∶6~11。
4.如权利要求1所述的杜仲籽油微乳液制备方法,其特征在于,步骤(2)中搅拌转速为280~400转/分。
5.如权利要求1所述的杜仲籽油微乳液制备方法,其特征在于,制备过程中所用超纯水的含盐量在0.1 mg/L以下,电导率小于0.1μs/cm。
6.如权利要求1所述的杜仲籽油微乳液制备方法,其特征在于,制备的杜仲籽油微乳液经干燥后以粉末态应用于食品、化妆品行业。
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