CN108685712A - 一种植物甾醇纳米微乳液及其制备方法和应用 - Google Patents
一种植物甾醇纳米微乳液及其制备方法和应用 Download PDFInfo
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- CN108685712A CN108685712A CN201810564525.6A CN201810564525A CN108685712A CN 108685712 A CN108685712 A CN 108685712A CN 201810564525 A CN201810564525 A CN 201810564525A CN 108685712 A CN108685712 A CN 108685712A
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- phytosterol
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- polyalcohol
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Abstract
本发明提供一种植物甾醇纳米微乳液及其制备方法和应用。所述制备方法是将一种或多种表面活性剂,经均质化处理后分散于多元醇或多元醇和水的混合物中,得到表面活性剂乳液;将分散溶解于有机溶剂中的植物甾醇溶液或植物甾醇细粉末加入到上述表面活性剂乳液中,经均质化处理后,将所制得的混合乳液中的有机溶剂去除,加水稀释,得到含多元醇的植物甾醇纳米微乳液,最后经超滤膜分离、吸附柱吸附或排阻层折等方法,分离除去多元醇,既得植物甾醇纳米微乳液。本发明的制备方法简单,成本低,而且安全环保,所得微乳液的中位粒径在20‑600纳米之间,稳定性好。本发明制备的微乳液作为功能因子可广泛用于食品、功能食品或化妆品。
Description
技术领域
本发明涉及食品、功能食品、药品及化妆品加工技术以及化工技术领域,具体涉及一种植物甾醇纳米微乳液及其制备和应用。
背景技术
植物甾醇在结构上类似动物胆固醇,无法在体内合成,只能从膳食或药物中摄取,可以抑制小肠对胆固醇的吸收,从而能够降低血清胆固醇及低密度脂蛋白水平,因此也是治疗心血管疾病及冠心病的重要途径。此外,研究也表明植物甾醇在抑制肿瘤、抗炎、抗氧化、抗癌、防治前列腺疾病和调节免疫功能等方面都有重要作用。植物甾醇被美国FDA认可为“降低血脂、预防动脉硬化”的天然保健食品新原料,是FDA批准的十二种可以使用“有益健康”食品中的一种。植物甾醇于2007年被中国卫生部批准为“新资源食品”。但由于植物甾醇的油溶性和水溶性都很差,所以其生物利用率较低,在使用大剂量植物甾醇的情况下,仍然得不到明显且稳定的抑制胆固醇吸收的效果。例如,每日口服5-18克剂量的谷甾醇只能降低16-20%的血清胆固醇。剂量效应研究表明降低12%的血清胆固醇需3-9克/天剂量的谷甾醇。因此对于植物甾醇而言,大大限制了其在功能性食品、化妆品、药品等中的应用。
目前,针对于提高植物甾醇的水溶性和生物利用率常用的方法有:制备植物甾醇微乳液、将植物甾醇添加到脂质体中、环糊精包埋等方法,但都存在着植物甾醇在分散体系中所占比例过低的问题。也有研究通过将植物甾醇分散于食用高分子中、固体脂质体等方法来解决植物甾醇水溶性的问题,但这些方法所得固形物中植物甾醇比例并不高(5%),而且其生物利用率较低。制备一种高植物甾醇含量的微乳液,是提高其溶解性和生物利用率的有效手段。
美国专利US5932562A中提到一种植物甾醇微乳液的制备,可以制备植物甾醇:磷脂摩尔比为1:1~1:10的植物甾醇微乳液,当制备植物甾醇:表面活性剂的摩尔比为1:1的微乳液时,需在配方中加入昂贵的且对人体可能有害的溶血磷脂。一种植物甾醇更高含量的微乳液的制备方法还未出现。
发明内容
为了解决以上现有技术的缺点和不足之处,本发明的首要目的在于提供一种植物甾醇纳米微乳液,旨在利用表面活性剂的亲油亲水性质及表面活性剂与植物甾醇的相互作用,将植物甾醇快速、有效地分散于多元醇或多元醇和水的混合物中,随后用水稀释,除去多元醇,形成纳米植物甾醇微乳液,进而达到解决植物甾醇在水相中溶解性差的技术瓶颈问题。所使用的多元醇可回收后循环使用,经济环保。
本发明的另一目的在于提供一种通过上述方法制备得到的植物甾醇纳米微乳液的制备方法。
本发明的再一目的在于提供上述植物甾醇纳米微乳液在食品、功能食品、化妆品中的应用。
一种植物甾醇纳米微乳液,该微乳液通过如下方法制备得到:
(1)按照质量比为(0.1~5):100的比例将一种或多种表面活性剂在50~150℃温度下经搅拌、超声或均质化处理分散于多元醇或多元醇与水的混合物中,得到乳液;
(2)将含有机溶剂的植物甾醇溶液或植物甾醇粉末加入到步骤(1)所得乳液中,在50~150℃温度下经均质化处理,得到混合乳液;
(3)将步骤(2)所得混合乳液中的有机溶剂去除,加水稀释至原体积的1.5-100倍,得到含有多元醇的植物甾醇纳米微乳液;
(4)上述含多元醇的植物甾醇微乳液经超滤膜分离、吸附柱吸附或排阻层折分离除去多元醇,即得植物甾醇纳米微乳液。
本发明技术方案中:步骤(1)中所述的表面活性剂为脂肪醇聚氧乙烯聚氧丙烯醚、月桂醇硫酸钠、聚氧乙烯蓖麻油、琥珀酸二辛酯磺酸钠、槐糖脂、鼠李糖脂、海藻糖脂、氢化磷脂、卵磷脂、蔗糖脂肪酸酯、脂肪酸甘油酯、烷基多聚葡萄糖苷、蔗糖二月桂酸酯、辛烷氧乙烯月桂酸酯、脂肪醇聚氧乙烯醚、磺基琥珀酸酯、司盘和吐温中的一种或多种;
优选:步骤(1)中所述的表面活性剂为卵磷脂、蔗糖脂肪酸酯、脂肪酸甘油酯、烷基多聚葡萄糖苷、和吐温中的一种或多种。
本发明技术方案中:步骤(1)中所述的多元醇为乙二醇、丙三醇、丙二醇、丁二醇、丁三醇、麦芽糖醇、葡萄糖醇、山梨糖醇、异麦芽酮糖醇、赤藓糖醇、甘露糖醇和木糖醇中的一种或多种;
优选:步骤(1)中所述的多元醇为丙三醇、丙二醇、丁二醇、丁三醇、葡萄糖醇、山梨糖醇、异麦芽酮糖醇、赤藓糖醇、甘露糖醇和木糖醇中的一种或多种。
本发明技术方案中:步骤(2)中所述的植物甾醇是选自谷甾醇、菜油甾醇、豆固醇、谷甾烷醇、菜籽甾醇、菜油甾烷醇、燕麦甾醇、麦角甾醇、禾本甾醇、柠檬甾二烯醇、洛飞烯醇、环木菠萝醇、环木菠萝烯醇和2,4-亚甲基环木菠萝醇中的至少一种;优选步骤(2)中所述的植物甾醇是谷甾醇、菜籽甾醇和谷甾烷醇;进一步优选:谷甾醇、菜籽甾醇和谷甾烷醇的质量比为70~90:5~15:1~10。本发明技术方案中:步骤(1)中多元醇和水的混合物,其多元醇和水的质量比为5~80:300~500。
本发明技术方案中:所述的均质化处理是高剪切均质处理、高压均质处理、超声均质处理和微射流处理中的任意一种。
本发明技术方案中:步骤(2)中所述的有机溶剂为正己烷、乙醚、二氯甲烷、三氯甲烷和四氯化碳中的一种或多种。
本发明技术方案中:步骤(2)中植物甾醇与表面活性剂的质量比为(0.01~6):1。
一种上述的植物甾醇纳米微乳液的制备方法,该方法包括以下步骤:
(1)按照质量比为(0.1~5):100的比例将一种或多种表面活性剂在50~150℃温度下经搅拌或均质化处理分散于多元醇或多元醇与水的混合物中,得到乳液;
(2)将含有机溶剂的植物甾醇溶液或植物甾醇粉末加入到步骤(1)所得乳液中,在50~150℃温度下经均质化处理,得到混合乳液;
(3)将步骤(2)所得混合乳液中的有机溶剂去除,加水稀释至原体积的1.5-100倍,得到含有多元醇的植物甾醇纳米微乳液;
(4)上述含多元醇的植物甾醇微乳液经超滤膜分离、吸附柱吸附或排阻层折等方法分离除去多元醇,即得植物甾醇纳米微乳液。
本发明技术方案将一定量植物甾醇高效分散于含有表面活性剂及助乳化剂的水分散体系中,利用表面活性剂的乳化作用以及助乳化剂对微乳体系的稳定作用,进而形成O/W乳液。制备得到的植物甾醇纳米微乳液,不仅可以作为食品添加剂添加到食品中,还可以作为功能因子应用于食品、保健食品、药品或化妆品的研发。
本发明的制备方法及所得到的产物具有如下优点及有益效果:
(1)本发明制备植物甾醇纳米微乳液,所采用的表面活性剂均为食品体系中广泛应用的,天然安全,且均具有营养价值高、功能性质好、安全无毒的优点。如采用有机溶剂,在最后被去除,因此制备的植物甾醇纳米微乳液可认为是安全可食用的;
(2)本发明利用表面活性剂的乳化性质和助乳化剂对微乳体系的稳定作用,将植物甾醇原料制备成植物甾醇微乳液,可以在0.01:1~6:1的质量比范围内,调节植物甾醇和表面活性剂比例,可以极大的提高植物甾醇的水溶性、水分散性和荷载率;
(3)本发明所得植物甾醇纳米微乳液粒径较小,水溶性好,植物甾醇含量高,生物利用率高,在水中完全溶解分散,可作为功能因子用于功能食品、药品及化妆品的生产中,大大提高了植物甾醇的可利用性;
(4)本发明制备植物甾醇纳米微乳液过程中,无需油脂,提高了甾醇密度,同时也避免了在摄入植物甾醇时,不必要的油脂摄入。
(5)本发明的制备方法所涉及的生产工艺简单、安全、要求低,最后分离得到的多元醇可重复使用,是一种绿色的生产技术,适用于大规模生产。
具体实施方式
下面结合实施例对本发明做进一步说明,但本发明的保护范围不限于此:
比较实施例1至5
根据美国专利US5932562A中提到植物甾醇微乳液的制备方法:
(1)按照表1所给的质量比,将植物甾醇(β-谷甾烷醇≥99%)和大豆磷脂,在30℃下,搅拌,完全溶于500毫升氯仿中,随后在65℃下旋转蒸发10小时,完全除去氯仿。
(2)在(1)所得磷脂和植物甾醇的混合物中加入1200毫升去离子水,剧烈搅拌1小时,随后超声45分钟,得到植物甾醇/磷脂微乳液。
表1
对所得植物甾醇乳液进行粒径分析,结果如表2所示。将制得的植物甾醇乳液在10000rpm条件下离心5分钟,观察离心管内乳液分层和沉淀情况,结果见表2。乳液的粒径测定结果见表2。如表2所示,在植物甾醇:大豆磷脂:溶血磷脂为1:1:0.5时,可以制备得到较稳定微乳液。而在不加溶血磷脂的情况下,植物甾醇:大豆磷脂比例大于1:4时,不能得到稳定的植物甾醇微乳液。以上数据表明,美国专利US5932562A中提到植物甾醇微乳液的制备方法无法制备得到高植物甾醇/磷脂比的微乳液。
表2
比较实施例6至9
根据Chin-Ping Tan等人在文献(J.Agric.Food Chem.2009,57,8426–8433)中提到植物甾醇微乳液的制备方法进行制备:
(1)按照表3所给的比例,将植物甾醇(β-谷甾烷醇≥99%)在45℃下,完全溶于无水
乙醇中。
(2)按照表3所给的质量比,表面活性剂完全溶于去离子水中。
(3)将步骤(1)所得植物甾醇溶液缓慢加入步骤(2)所得表面活性剂中,同时进行均质化处
理,得乳液。
(4)将步骤(3)所得乳液进行高压均质,随后旋转蒸发(压力0.17bar,转数100rpm),除去有
机溶剂,得到植物甾醇乳液。
表3
对所得植物甾醇乳液进行粒径分析,结果如表4所示。将制得的植物甾醇乳液在10000rpm条件下离心5分钟,观察离心管内乳液分层和沉淀情况,结果见表4。乳液的粒径测定结果见表4。如表4所示,在植物甾醇:蔗糖脂肪酸酯(吐温20)为1:1时,可以制备得到较稳定微乳液。而当植物甾醇:蔗糖脂肪酸酯或植物甾醇:吐温20大于2:1时,则不能得到稳定的植物甾醇微乳液。以上数据表明,比较实施例6-9的植物甾醇微乳液制备方法无法制备得到高植物甾醇/表面活性剂比的微乳液。
表4
实施例1至9:
(1)按照表5中所示的质量,将一种或多种表面活性剂加入到相应浓度的多元醇水溶液或多元醇中。实施例1、2和3在100℃,100rpm转速下,搅拌10min;实施例4、5和6在90℃下,8,000rpm转速下,均质化处理10min;实施例7、8和9在80℃下,400w功率下,超声均质10min;实施例10、11和12在7,000psi下,高压均质10分钟,分别得到相应的混合乳液;
(2)按照表5中所示的质量,将植物甾醇(β-谷甾醇85%,菜油甾醇10%,以及谷甾烷醇5%)加入到100ml乙醚中,在30℃下,磁力搅拌20min,使其完全溶解,得到植物甾醇溶液;
(3)将步骤(2)所得植物甾醇溶液,加入到步骤(1)所得混合乳液中。实施例1至6在80℃下,在400w功率下超声均质10min。实施例7-12在120℃,在10,000rpm转速下均质化处理10min。在实施例2、5、8和11的情况中,得到的溶液进一步在8,000psi下高压均质5分钟。在实施例3、6、9和12情况中,得到的溶液进一步在40MPa条件下微射流1次。
(4)将步骤(3)所得混合乳液收集于蒸馏瓶中,在50℃、0.094MPa真空度条件下旋转蒸发去除乙醚,实施例1至3加水稀释至原体积的2倍,实施例4至6加水稀释至原体积的4倍,实施例7至9加水稀释至原体积的6倍,实施例10至12加水稀释至原体积的8倍,得到含有多元醇的植物甾醇纳米微乳液。
(5)实施例1至6所得含多元醇的植物甾醇微乳液经超滤膜分离除去多元醇,既得植物甾醇纳米微乳液。实施例7至12所得含多元醇的植物甾醇微乳液经大孔树脂吸附除去多元醇,既得植物甾醇纳米微乳液。实施例1至12中,分离得到的多元醇可重复使用。
将制得的植物甾醇乳液在10000rpm条件下离心5分钟,观察离心管内乳液分层和沉淀情况,结果见表6。乳液的粒径测定结果见表6。如表6所示,实施例1至12所制备的植物甾醇微乳液具有纳米级的粒径以及合理的PDI值,且在10000rpm离心后均未出现沉淀和分层。以上数据表明,本实施例的植物甾醇纳米微乳液可极大地提高植物甾醇的水溶性和水分散性。
表6
实施例13至24:
(1)按照表7中所示的质量,将一种或多种表面活性剂加入到相应浓度的多元醇水溶液或多元醇中。实施例13、14和15在100℃,100rpm转速下,搅拌10min;实施例16、17和18在90℃下,8,000rpm转速下,均质化处理10min;实施例19、20和21在80℃下,400w功率下超声均质10min;实施例22、23和24在7,000psi下,高压均质10分钟,分别得到相应的混合乳液;
(2)将植物甾醇粉末(β-谷甾醇50%,豆甾醇25%,菜油甾醇20%,以及菜籽甾醇5%),按照表7中所示的质量,加入到步骤(1)所得混合乳液中。实施例13至18在80℃下,在400w功率下超声均质10min。实施例19至24在120℃下,在10,000rpm转速下均质化处理10min。在实施例14、17、20和23的情况中,得到的溶液进一步在8,000psi下高压均质5分钟。在实施例15、18和21和24情况中,得到的溶液进一步在40MPa条件下微射流1次。
(3)实施例13至15所得混合乳液加水稀释至原体积的2倍,实施例16至18所得混合乳液加水稀释至原体积的4倍,实施例19至21所得混合乳液加水稀释至原体积的6倍,实施例22至24所得混合乳液加水稀释至原体积的4倍,得到含有多元醇的植物甾醇纳米微乳液。
(4)实施例13至18所得含多元醇的植物甾醇微乳液经超滤膜分离除去多元醇,既得植物甾醇纳米微乳液。实施例19至24所得含多元醇的植物甾醇微乳液经大孔树脂吸附除去多元醇,既得植物甾醇纳米微乳液。实施例13至24中,分离得到的多元醇可重复使用。
将制得的植物甾醇乳液在10000rpm条件下离心5分钟,观察离心管内乳液分层和沉淀情况,结果见表8。乳液的粒径测定结果见表8。如表8所示,实施例13至24所制备的植物甾醇微乳液具有纳米级的粒径以及合理的PDI值,且在10000rpm离心后均未出现沉淀和分层。以上数据表明,本实施例的植物甾醇纳米微乳液可极大地提高植物甾醇的水溶性和水分散性。
表8
实施例25:
将实施例9和24中制备的含有1克植物甾醇的微乳液加入到400克水性饮料中,所述水性饮料选自水、碳酸饮料、牛奶、豆浆、谷物饮料、果汁饮料以及其他饮料,搅拌混匀。
实施例26:
将实施例25中制备的饮料分别在室温下和冰箱中(4℃),放置1年以上时间,监测其物理形态,不仅观察到饮料保持正常分散态,而且没有发现其他异样。
实施例27:
将实施例12和21中制备的含有1克植物甾醇的微乳液加入到300克水性化妆品中,所述水性化妆品选自市面上常见的美白水、活肤水、祛痘水、防晒水等,搅拌混匀。
实施例28:
将实施例27中制备的饮料分别在室温下和冰箱中(4℃),放置1年以上时间,监测其物理形态,不仅观察到水性化妆品保持正常分散态,而且没有发现其他异样。
Claims (10)
1.一种植物甾醇纳米微乳液,其特征在于:该微乳液通过如下方法制备得到:
(1)按照质量比为(0.1~5):100的比例将一种或多种表面活性剂在50~150℃温度下经搅拌、超声或均质化处理分散于多元醇或多元醇与水的混合物中,得到乳液;
(2)将含有机溶剂的植物甾醇溶液或植物甾醇粉末加入到步骤(1)所得乳液中,在50~150℃温度下经均质化处理,得到混合乳液;
(3)将步骤(2)所得混合乳液中的有机溶剂去除,加水稀释至原体积的1.5-100倍,得到含有多元醇的植物甾醇纳米微乳液;
(4)上述含多元醇的植物甾醇微乳液经超滤膜分离、吸附柱吸附或排阻层折分离除去多元醇,即得植物甾醇纳米微乳液。
2.根据权利要求1所述的植物甾醇纳米微乳液,其特征在于:步骤(1)中所述的表面活性剂为脂肪醇聚氧乙烯聚氧丙烯醚、月桂醇硫酸钠、聚氧乙烯蓖麻油、琥珀酸二辛酯磺酸钠、槐糖脂、鼠李糖脂、海藻糖脂、氢化磷脂、卵磷脂、蔗糖脂肪酸酯、脂肪酸甘油酯、烷基多聚葡萄糖苷、蔗糖二月桂酸酯、辛烷氧乙烯月桂酸酯、脂肪醇聚氧乙烯醚、磺基琥珀酸酯、司盘和吐温中的一种或多种;优选:步骤(1)中所述的表面活性剂为卵磷脂、蔗糖脂肪酸酯、脂肪酸甘油酯、烷基多聚葡萄糖苷和吐温中的一种或多种。
3.根据权利要求1所述的植物甾醇纳米微乳液,其特征在于:步骤(1)中所述的多元醇为乙二醇、丙三醇、丙二醇、丁二醇、丁三醇、麦芽糖醇、葡萄糖醇、山梨糖醇、异麦芽酮糖醇、赤藓糖醇、甘露糖醇和木糖醇中的一种或多种;优选:步骤(1)中所述的多元醇为丙三醇、丙二醇、丁二醇、丁三醇、葡萄糖醇、山梨糖醇、异麦芽酮糖醇、赤藓糖醇、甘露糖醇和木糖醇中的一种或多种。
4.根据权利要求1所述的植物甾醇纳米微乳液,其特征在于:步骤(2)中所述的植物甾醇是选自谷甾醇、菜油甾醇、豆固醇、谷甾烷醇、菜籽甾醇、菜油甾烷醇、燕麦甾醇、麦角甾醇、禾本甾醇、柠檬甾二烯醇、洛飞烯醇、环木菠萝醇、环木菠萝烯醇和2,4-亚甲基环木菠萝醇中的至少一种;优选步骤(2)中所述的植物甾醇是谷甾醇、菜籽甾醇和谷甾烷醇;进一步优选:谷甾醇、菜籽甾醇和谷甾烷醇的质量比为70~90:5~15:1~10。
5.根据权利要求1所述的植物甾醇纳米微乳液的制备方法,其特征在于:步骤(1)中多元醇和水的混合物,其多元醇和水的质量比为5~80:300~500。
6.根据权利要求1所述的植物甾醇纳米微乳液,其特征在于:所述的均质化处理是高剪切均质处理、高压均质处理、超声均质处理和微射流处理中的任意一种。
7.根据权利要求1所述的植物甾醇纳米微乳液,其特征在于:步骤(2)中所述的有机溶剂为正己烷、乙醚、二氯甲烷、三氯甲烷和四氯化碳中的一种或多种。
8.根据权利要求1所述的植物甾醇纳米微乳液,其特征在于:步骤(2)中植物甾醇与表面活性剂的质量比为(0.01~6):1。
9.一种权利要求1所述的植物甾醇纳米微乳液的制备方法,其特征在于:该方法包括以下步骤:
(1)按照质量比为(0.1~5):100的比例将一种或多种表面活性剂在50~150℃温度下经搅拌或均质化处理分散于多元醇或多元醇与水的混合物中,得到乳液;
(2)将含有机溶剂的植物甾醇溶液或植物甾醇粉末加入到步骤(1)所得乳液中,在50~150℃温度下经均质化处理,得到混合乳液;
(3)将步骤(2)所得混合乳液中的有机溶剂去除,加水稀释至原体积的1.5-100倍,得到含有多元醇的植物甾醇纳米微乳液;
(4)上述含多元醇的植物甾醇微乳液经超滤膜分离、吸附柱吸附或排阻层折等方法分离除去多元醇,即得植物甾醇纳米微乳液。
10.权利要求1所述的植物甾醇纳米微乳液在制备食品、功能食品及化妆品中的应用。
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