CN113966839B - 一种含核桃油和二氢杨梅素的复合乳液及其制备方法 - Google Patents
一种含核桃油和二氢杨梅素的复合乳液及其制备方法 Download PDFInfo
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- CN113966839B CN113966839B CN202111197935.XA CN202111197935A CN113966839B CN 113966839 B CN113966839 B CN 113966839B CN 202111197935 A CN202111197935 A CN 202111197935A CN 113966839 B CN113966839 B CN 113966839B
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- Prior art keywords
- dihydromyricetin
- composite emulsion
- walnut oil
- preparation
- phospholipid
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Classifications
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- A—HUMAN NECESSITIES
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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Abstract
本发明公开了一种含核桃油和二氢杨梅素的复合乳液,由以下百分比质量的组分组成:二氢杨梅素0.05‑2%,核桃油1‑15%,磷脂0.5‑10%,酪蛋白酸钠0.5‑10%,乳清蛋白0.5‑10%,疏水性二氧化硅0.5‑1%,余量为去离子水,复合乳液的制备时对水相和油相进行乳化均质处理,选用磷脂、酪蛋白、乳清蛋白、疏水性二氧化硅作为复配乳化剂,冷却至室温,获得含核桃油和二氢杨梅素的复合乳液。本发明具有良好的抗氧化性能,改善核桃油和二氢杨梅素的水溶解性,平均粒径变化范围小,制备方便等优点。
Description
【技术领域】
本发明属于复合乳液的技术领域,尤其涉及一种含核桃油和二氢杨梅素的复合乳液及其制备方法。
【背景技术】
在食品工业中常需要添加活性成分进行营养强化,这样可以增加食品的功能性,提高产品的附加值,弥补原有食品中营养成分的缺陷,使食品的品质得到一定的提升。核桃油含有大量的不饱和脂肪酸,其脂肪的主要成分为亚油酸甘油酯、亚麻酸以及油酸甘油酯,这些都是我们人体所必需的脂肪酸。核桃油中含有人体必需的矿物质元素,钾、钠、锌、钙、磷、铁等含量较高。核桃油含有的多种维生素,包括维生素A、维生素E、维生素D、维生素K、维生素P等,不仅对人体有防病、治病的功效,还能够起到抗衰老、黑发、延年益寿的作用。
二氢杨梅素广泛存在于葡萄科、杜鹃科、杨梅科、大戟科、藤黄科及柳科等植物中。二氢杨梅素生理活性广泛且安全性好,具有抗氧化、抗炎、抗肿瘤、解酒保肝、抗病原微生物及调血脂等多方面的药理作用,在减少动脉粥样硬化病变方面也有显著效果,另外,二氢杨梅素可能潜在影响预防斑块破裂和随后的血栓性闭塞。
然而核桃油中含大量的不饱和键,二氢杨梅素含有邻三酚羟基结构,稳定性和水溶性较差,对环境(氧气、光、热、酸性条件等)敏感,容易发生降解和异构化,影响产品品质和功能性。且天然状态下的二氢杨梅素在消化道内往往不能完全释放,生物利用度较低,这给其在食品工业中的应用带来诸多不便。核桃油和二氢杨梅素存在水溶性差、易氧化变质等瓶颈问题。
乳液是目前应用最广泛的脂溶性成分共同传递的胶体分散***之一。它是一种非均相体系,其中一种不互溶液体以液滴的形式分散在另一种表面活性剂稳定的液体中。乳液能有效改善脂溶性活性成分的水分散性和口服生物利用度。然而,乳液由于其乳化剂界面厚度薄、比表面积大、光穿透性高而不能有效抑制不饱和脂肪酸的氧化。
【发明内容】
本发明的目的就是解决背景技术中的问题,提出一种含核桃油和二氢杨梅素的复合乳液及其制备方法。
为实现上述目的,本发明提出了一种含核桃油和二氢杨梅素的复合乳液,所述复合乳液由以下百分比质量的组分组成:二氢杨梅素0.05-2%,核桃油1-15%,磷脂0.5-10%,酪蛋白酸钠0.5-10%,乳清蛋白0.5-10%,疏水性二氧化硅0.5-1%,余量为去离子水。
作为优选,所述磷脂为大豆卵磷脂、蛋黄卵磷脂、氢化卵磷脂、脑磷脂、磷脂酰丝氨酸、磷脂酰肌醇、磷脂酰甘油中的一种或几种。
作为优选,所述复合乳液由以下百分比质量的组分组成:二氢杨梅素0.05%,核桃油1%,磷脂0.5%,酪蛋白酸钠10%,乳清蛋白2%,疏水性二氧化硅0.5%,去离子水85.95%。
作为优选,所述复合乳液由以下百分比质量的组分组成:二氢杨梅素2%,核桃油15%,磷脂3%,酪蛋白酸钠0.5%,乳清蛋白10%,疏水性二氧化硅1%,去离子水68.5%。
作为优选,所述复合乳液由以下百分比质量的组分组成:二氢杨梅素1%,核桃油7%,磷脂10%,酪蛋白酸钠2%,乳清蛋白0.5%,疏水性二氧化硅0.5%,去离子水79%。
本发明还提出了一种含核桃油和二氢杨梅素的复合乳液的制备方法,包括以下几个步骤:
油相的制备:将二氢杨梅素加入核桃油中溶解搅拌均匀,均质至无明显可见颗粒,获得油相;
水相的制备:将磷脂、酪蛋白酸钠、乳清蛋白、疏水性二氧化硅依次溶解分散在去离子水中,获得水相;
复合乳液的制备:将水相在搅拌条件下添加到油相中,搅拌预乳化,进行均质处理,冷却至室温,获得含核桃油和二氢杨梅素的复合乳液。
作为优选,所述均质处理为高剪切均质处理、高压均质处理或微射流均质处理。
作为优选,所述均质处理为高剪切均质处理,高剪切均质处理由高剪切分散乳化机进行,并设置高剪切分散乳化机的转速为9000~11000rpm,剪切时间为12~18min。
作为优选,所述均质处理为高压均质处理,高压均质处理由高压均质机进行,并设置高压均质机的压强为500~700Bar,循环2~4次。
作为优选,所述均质处理为微射流均质处理,微射流均质处理由微射流均质机进行,并设置微射流均质机的微射流压力为9000~11000psi,循环2~4次。
本发明的有益效果:本发明通过将二氢杨梅素溶解于核桃油并通过乳化处理,有效解决了核桃油和二氢杨梅素水溶性差,生物利用度低的应用瓶颈;通过核桃油和二氢杨梅素最优化复配,二氢杨梅素作为抗氧化剂,可有效保护核桃油中的不饱和脂肪酸,延长货架期,制得的复合乳液具有良好的抗氧化性能;磷脂是具有较高营养价值的保健原料,酪蛋白酸钠和乳清蛋白是牛奶蛋白的主要成分且安全性较高具有一定的营养价值和生物相容性,疏水性二氧化硅是一种安全的食品添加剂,将这四种乳化剂进行最优化复配作为复合乳化剂,各乳化剂在油水界面处起到结构互补的作用,形成的界面膜更紧密,乳化效果优于单一乳化剂,使得复合乳液的平均粒径在200-500nm范围,复合乳化剂可改善核桃油和二氢杨梅素的水溶解性;复合乳液具有健脑、益智、抗氧化、护肝等保健功效;制备方法操作简单。
本发明的特征及优点将通过实施例结合附图进行详细说明。
【附图说明】
图1是本发明一种实施例的制备方法流程图;
图2是本发明一种实施例的复合乳液55℃加速氧化15天过氧化物浓度变化示意图;
图3是本发明一种实施例的复合乳液55℃加速氧化15天过硫代***酸反应物浓度变化示意图;
图4是本发明一种实施例的复合乳液25℃储存4周的体积平均粒径变化示意;
图5是本发明一种实施例的复合乳液25℃储存4周的体积平均粒径变化示意;
图6是本发明一种实施例的复合乳液的DPPH抗氧化能力检测结果示意图。
【具体实施方式】
一种含核桃油和二氢杨梅素的复合乳液,由以下百分比质量的组分组成:二氢杨梅素0.05-2%,核桃油1-15%,磷脂0.5-10%,酪蛋白酸钠0.5-10%,乳清蛋白0.5-10%,疏水性二氧化硅0.5-1%,余量为去离子水。
进一步地,磷脂为大豆卵磷脂、蛋黄卵磷脂、氢化卵磷脂、脑磷脂、磷脂酰丝氨酸、磷脂酰肌醇、磷脂酰甘油中的一种或几种。
以下通过具体实施例进一步对本发明进行说明,下述实施例仅用于说明本发明而对本发明没有限制:
实施例1
一种含核桃油和二氢杨梅素的复合乳液由以下百分比质量的组分组成:二氢杨梅素0.05%,核桃油1%,大豆卵磷脂0.5%,酪蛋白酸钠10%,乳清蛋白2%,疏水性二氧化硅0.5%,去离子水85.95%。
参阅图1,一种含核桃油和二氢杨梅素的复合乳液的制备方法,包括以下几个步骤:
S01油相的制备:称取0.05g二氢杨梅素和1g核桃油,将核桃油、二氢杨梅素依次加入搅拌锅中混合溶解,并搅拌均质至肉眼观察下无明显可见颗粒,获得油相;
S02水相的制备:称取0.5g大豆卵磷脂、10g酪蛋白酸钠、2g乳清蛋白、0.5g疏水性二氧化硅和85.95g去离子水,将去离子水添加至乳化锅内,依次将大豆卵磷脂、酪蛋白酸钠、乳清蛋白、疏水性二氧化硅依次添加至乳化锅内使其溶解分散到去离子水中,获得水相;
S03复合乳液的制备:将水相在500rpm搅拌条件下添加到油相中,搅拌预乳化30min得到初乳,通过微射流均质机对初乳进行微射流均质处理,设置微射流均质机的微射流压力为10000psi,循环3次,均质完成后冷却至室温,获得含核桃油和二氢杨梅素的复合乳液。
将该复合乳液分散至去离子水中,该分散液通过马尔文粒度仪ZS90测定其平均粒径为255.9nm。
实施例2
一种含核桃油和二氢杨梅素的复合乳液由以下百分比质量的组分组成:二氢杨梅素1%,核桃油7%,蛋黄卵磷脂10%,酪蛋白酸钠2%,乳清蛋白0.5%,疏水性二氧化硅0.5%,去离子水79%。
参阅图1,一种含核桃油和二氢杨梅素的复合乳液的制备方法,包括以下几个步骤:
S01油相的制备:称取1g二氢杨梅素和7g核桃油,将核桃油、二氢杨梅素依次加入搅拌锅中混合溶解,并搅拌均质至肉眼观察下无明显可见颗粒,获得油相;
S02水相的制备:称取10g蛋黄卵磷脂、2g酪蛋白酸钠、0.5g乳清蛋白、0.5g疏水性二氧化硅和79g去离子水,将去离子水添加至乳化锅内,依次将大豆卵磷脂、酪蛋白酸钠、乳清蛋白、疏水性二氧化硅依次添加至乳化锅内使其溶解分散到去离子水中,获得水相;
S03复合乳液的制备:将水相在500rpm搅拌条件下添加到油相中,搅拌预乳化30min得到初乳,通过高剪切分散乳化机对初乳进行高剪切均质处理,设置高剪切分散乳化机的转速为10000rpm,剪切时间为15min,均质完成后冷却至室温,获得含核桃油和二氢杨梅素的复合乳液。
将该复合乳液分散至去离子水中,该分散液通过马尔文粒度仪ZS90测定其平均粒径为357.2nm。
实施例3
一种含核桃油和二氢杨梅素的复合乳液由以下百分比质量的组分组成:二氢杨梅素2%,核桃油15%,氢化卵磷脂3%,酪蛋白酸钠0.5%,乳清蛋白10%,疏水性二氧化硅1%,去离子水68.5%。
参阅图1,一种含核桃油和二氢杨梅素的复合乳液的制备方法,包括以下几个步骤:
S01油相的制备:称取2g二氢杨梅素和15g核桃油,将核桃油、二氢杨梅素依次加入搅拌锅中混合溶解,并搅拌均质至肉眼观察下无明显可见颗粒,获得油相;
S02水相的制备:称取3g氢化卵磷脂、0.5g酪蛋白酸钠、10g乳清蛋白、1g疏水性二氧化硅和68.5g去离子水,将去离子水添加至乳化锅内,依次将大豆卵磷脂、酪蛋白酸钠、乳清蛋白、疏水性二氧化硅依次添加至乳化锅内使其溶解分散到去离子水中,获得水相;
S03复合乳液的制备:将水相在500rpm搅拌条件下添加到油相中,搅拌预乳化30min得到初乳,通过高压均质机对初乳进行高压均质处理,设置高压均质机的压强为600Bar,循环3次,均质完成后冷却至室温,获得含核桃油和二氢杨梅素的复合乳液。
将该复合乳液分散至去离子水中,该分散液通过马尔文马尔文粒度仪ZS90ZS90测定其平均粒径为407.2nm。
性能检测:
按如下方法进行不饱和油脂的氧化稳定性测试:
设置实验组和对照组,其中实验组为本发明制备方法制得的含核桃油和二氢杨梅素的复合乳液样品,对照组(不添加二氢杨梅素)也采用本发明制备方法制得的含核桃油的复合乳液样品,将两组复合乳液样品均置于55℃的恒温培养箱中培养15天,分别测定油脂氧化的初级产物(过氧化物)和次级产物(硫代***酸反应物)。
(1)过氧化物浓度测定
将0.2mL的乳液加入到1.6mL 2-丙醇/异辛烷(1:3,v/v)的混合溶剂中,并剧烈震荡。取上述混合溶液在3400×g的条件下离心10min,然后取上层清液,将0.2mL清液与2.8mL的甲醇/1-丁醇(2:1,v/v)混合均匀。随后加入30μL Fe2+溶液/3.94M硫氰酸铵溶液(1:1,v/v),迅速混匀上述混合溶液,置于避光处反应20min,并于510nm处使用紫外可见分光光度法测定吸光度值,根据过氧化氢异丙苯标准曲线计算过氧化值,其中,0.144M FeSO4溶液和0.132M BaCl2溶液反应得到Fe2+溶液。
(2)硫代***酸反应物浓度
取0.2mL乳液加入到3.8mL TBA反应液(1.76mL 12M HCl、0.375g TBA和15g三氯乙酸溶解于82.9mL的去离子水中)中,保持总体积为4mL。然后剧烈震摇试管,并将其置于沸水浴中加热15min,冷却至室温后,将试管放置在3000×g的条件下离心10min,取上层清液,于532nm处使用紫外可见分光光度法测定吸光度值,根据1,1,3,3-四乙氧基丙烷标准曲线计算硫代***酸反应物浓度。
上述两组氧化稳定性检测结果如图2、3所示。由图可知,仅含核桃油的复合乳液氧化稳定性较差,氧化物产物变化波动较大说明储存过程中发生了较强烈的不饱和脂肪酸的氧化;而含二氢杨梅素和核桃油的复合乳液氧化稳定性较好,氧化产物变化波动较小。以上结果表明本发明含核桃油和二氢杨梅素复合乳液,由于二氢杨梅素的存在,氧化稳定性较好,二氢杨梅素对核桃油具有较好的保护作用。
按如下方法进行体积平均粒径的稳定性测试:
设置实验组1和实验组2、对照组1、对照组2,其中实验组1和实验组2分按实施例1和实施例3的配比进行制备,对照组1除了采用同质量浓度的酪蛋白酸钠为乳化剂替代本发明中的复合乳化剂(即磷脂、酪蛋白酸钠、乳清蛋白和疏水性二氧化硅复配的混合乳化剂)外其余成分配比及制备均与实验组1相同,对照组2采用同质量浓度的乳清蛋白为乳化剂替代本发明中的复合乳化剂外其余成分配比及制备均与实验组2相同,将四组复合乳液样品在25℃的条件下储存4周,每周去一定样品,使用马尔文粒度仪ZS90测定乳液的平均粒径。
实验组1和对照组1的复合乳液、实验组2和对照组2的复合乳液存储过程中体积平均粒径分别如图4、图5所示。由图4和图5可知,单一乳化剂制得的复合乳液在存储过程中体积平均粒径增大较为剧烈,而由混合乳化剂制得的复合乳液在存储过程中体积平均粒径的增大程度要远小于单一乳化剂制得的复合乳液。主要是由于多种乳化剂的空间互补作用,使得乳化剂界面层较为致密,进而降低了复合乳液存储过程中体积平均粒径的增加量。
按如下方法进行复合乳液的DPPH抗氧化性能检测:
设置实验组3、对照组3和对照组4,实验组3按实施例3的配比进行制备,对照组3除了采用同质量浓度的饱和中链油脂辛癸酸甘油三酯替代核桃油外其余成分配比及制备均与实验组3相同,对照组4除了采用同质量浓度的吐温80替代配方中的复合乳化剂(即磷脂、酪蛋白酸钠、乳清蛋白和疏水性二氧化硅复配的混合乳化剂)外其余成分配比及制备均与实验组3相同。
精密称取15mg DPPH溶解定容于50mL的容量瓶中得标准溶液。反应前,复合乳液样品用去离子水分散并稀释100倍。随后,分别向0.6mL的DPPH标准溶液中加入20μL稀释液或乙醇溶液,并加入乙醇保持总体积为4mL。上述混合溶液震摇均匀,室温下避光静置30min。然后过滤,并于517nm处使用紫外可见分光光度法测定吸光度值。抗氧化能力的计算方法为:[(A0-A1)/A0]×100,其中A0为空白溶液的吸光度值,A1为测试样品的吸光度值。
各组复合乳液的1,1-二苯基-2-三硝基苯肼(DPPH)自由基清除能力如图6所示。由图6可知,实验组3的自由基清除能力明显高于对照组3的自由基清除能力,而实验组和对照组4相比二者自由基清除能力基本相同,表明核桃油的存在可以提高二氢杨梅素的自由基清除能力,表明复合乳化剂对二氢杨梅素的自由基清除能力影响不大。二氢杨梅素乙醇溶液的自由基清除能力较好,这归功于二氢杨梅素结构中的羟基。
本发明的各种原料均可从市场购得,制备方法中采用设备均采用现有设备,上述实施例是对本发明的说明,不是对本发明的限定,任何对本发明简单变换后的方案均属于本发明的保护范围。
Claims (5)
1.一种含核桃油和二氢杨梅素的复合乳液,其特征在于:所述复合乳液由以下百分比质量的组分组成:二氢杨梅素0.05-2%,核桃油1-15%,磷脂0.5-10%,酪蛋白酸钠0.5-10%,乳清蛋白0.5-10%,疏水性二氧化硅0.5-1%,余量为去离子水;所述复合乳液的制备方法包括以下几个步骤:
油相的制备:将二氢杨梅素加入核桃油中溶解搅拌均匀,均质至无明显可见颗粒,获得油相;
水相的制备:将磷脂、酪蛋白酸钠、乳清蛋白、疏水性二氧化硅依次溶解分散在去离子水中,获得水相;
复合乳液的制备:将水相在搅拌条件下添加到油相中,搅拌预乳化,进行均质处理,冷却至室温,获得含核桃油和二氢杨梅素的复合乳液;
其中,所述均质处理为高剪切均质处理或高压均质处理或微射流均质处理,所述高剪切均质处理由高剪切分散乳化机进行,并设置高剪切分散乳化机的转速为9000~11000rpm,剪切时间为12~18min;所述高压均质处理由高压均质机进行,并设置高压均质机的压强为500~700Bar,循环2~4次;所述微射流均质处理由微射流均质机进行,并设置微射流均质机的微射流压力为9000~11000psi,循环2~4次。
2.如权利要求1所述的含核桃油和二氢杨梅素的复合乳液,其特征在于:所述磷脂为大豆卵磷脂、蛋黄卵磷脂、氢化卵磷脂、脑磷脂、磷脂酰丝氨酸、磷脂酰肌醇、磷脂酰甘油中的一种或几种。
3.如权利要求1所述的含核桃油和二氢杨梅素的复合乳液,其特征在于:所述复合乳液由以下百分比质量的组分组成:二氢杨梅素0.05%,核桃油1%,磷脂0.5%,酪蛋白酸钠10%,乳清蛋白2%,疏水性二氧化硅0.5%,去离子水85.95%。
4.如权利要求1所述的含核桃油和二氢杨梅素的复合乳液,其特征在于:所述复合乳液由以下百分比质量的组分组成:二氢杨梅素2%,核桃油15%,磷脂3%,酪蛋白酸钠0.5%,乳清蛋白10%,疏水性二氧化硅1%,去离子水68.5%。
5.如权利要求1所述的含核桃油和二氢杨梅素的复合乳液,其特征在于:所述复合乳液由以下百分比质量的组分组成:二氢杨梅素1%,核桃油7%,磷脂10%,酪蛋白酸钠2%,乳清蛋白0.5%,疏水性二氧化硅0.5%,去离子水79%。
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