CN112402404A - 一种虾青素酯纳米复合物颗粒的制备方法 - Google Patents
一种虾青素酯纳米复合物颗粒的制备方法 Download PDFInfo
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- CN112402404A CN112402404A CN202011494944.0A CN202011494944A CN112402404A CN 112402404 A CN112402404 A CN 112402404A CN 202011494944 A CN202011494944 A CN 202011494944A CN 112402404 A CN112402404 A CN 112402404A
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- astaxanthin ester
- emulsification
- astaxanthin
- phase solution
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Abstract
本发明涉及虾青素技术领域,具体涉及一种虾青素酯纳米复合物颗粒的制备方法,包括将蛋白质溶于去离子水或缓冲溶液中水化,得到水相溶液;将虾青素酯溶于油相中制成虾青素酯的油溶液;将虾青素酯油溶液添加到水相溶液中,同时向体系中加入茶多酚,然后采用高压微射流充分均质乳化;将乳化后的体系用碱性物质调节体系pH值到11~13,进行二次均质乳化;将二次乳化后的体系边搅拌边用酸性物质调节体系pH至6.5~7.2;干燥。通过本方法制得的虾青素酯热稳定性和加工储运稳定性明显提高,在水中分散性良好,具备良好的加工应用性能;制备过程不使用醇类溶剂和表面活性剂,避免了醇类溶剂和表面活性剂所造成的残留问题,提高了安全性。
Description
技术领域
本发明涉及虾青素技术领域,具体涉及一种虾青素酯纳米复合物颗粒的制备方法。
背景技术
虾青素(Astaxanthin)是迄今为止自然界中已发现的最强天然抗氧化剂,被称为超级抗氧化剂。越来越多的研究结果表明,虾青素具有多种生理活性,如抗衰老、抗肿瘤、预防心脑血管疾病、保肝护肝、抗糖尿病、抗炎、改善运动机能,并且虾青素是目前发现的唯一能穿透血-脑、血-视网膜屏障的类胡萝卜素,对中枢神经系统和大脑功能可产生积极的影响。因此,将虾青素作为膳食功能因子添加到食品、化妆品等产品当中,对改善健康具有切实的意义。
在自然界中,90%以上的虾青素以虾青素酯的形式存在。发明人在前期的研究中发现,虾青素酯较游离虾青素表现出更好的稳定性和生物利用率。SHOWALTER L A,CARDOUNEL A J,WADEA N等研究表明,随着虾青素酯化程度的加深,虾青素体现为疏水性增强,且更容易被动物组织所吸收利用。在对龙虾等动物的研究中,就证实酯化虾青素比游离虾青素容易被吸收并与外骨骼结合,从而使动物有效着色。因此,将虾青素酯作为一种新型功能活性因子,具有广阔的发展空间。
但由于虾青素酯具有强的疏水结构,其水溶性极差,且凝聚态为油状树脂,使其在水相介质和固体基质产品中的应用受到严重限制。另外,虾青素酯在自然条件下极易被氧化并降解,使其活性功能丧失,贮藏稳定性差,该性质亦限制了虾青素酯的应用与消费。因此,如何提高虾青素酯在水相介质中的溶解性、固体基质中的适用性和贮藏稳定性,成为虾青素酯在生产和消费过程中的关键技术问题。
发明内容
针对虾青素酯水溶性和贮藏稳定性差的问题,本发明提供一种虾青素酯纳米复合物颗粒的制备方法,通过本方法制得的虾青素酯热稳定性和加工储运稳定性明显提高,在水中的分散性良好,因此具备良好的加工应用性能;制备过程不使用醇类溶剂和表面活性剂,从而避免了醇类溶剂和表面活性剂所造成的残留问题,提高了安全性。
一种虾青素酯纳米复合物颗粒的制备方法,所述制备方法包括如下步骤:
(1)水相溶液的制备:将蛋白质溶于去离子水或缓冲溶液中水化,得到水相溶液;
(2)油相溶液的制备:将虾青素酯溶于油相中制成虾青素酯的油溶液;
(3)一次乳化:将步骤(2)制备的虾青素酯油溶液添加到步骤(1)制备的水相溶液中,同时向体系中加入茶多酚,然后采用高压微射流充分均质乳化;
(4)一次调节体系pH和二次乳化:将步骤(3)乳化后的体系用碱性物质调节体系pH值到11~13,然后进行二次均质乳化;
(5)二次调节体系pH:将步骤(4)得到的二次乳化后的体系边搅拌边用酸性物质调节体系pH至6.5~7.2;
(6)干燥。
进一步的,所述步骤(1)为:将蛋白质按质量体积比0.5~5g/100mL的添加量溶于pH为6.5~7.5的去离子水或磷酸盐缓冲溶液中,于1~20℃环境下水化2~12h,得到水相溶液。
优选的,所述蛋白质为玉米醇溶蛋白、小麦醇溶蛋白、高粱醇溶蛋白、大麦醇溶蛋白中的一种或几种。
优选的,步骤(1)还包括向水相溶液中添加质量体积比为0.1~5g/100mL的稳定剂,所述稳定剂为藻酸丙二醇酯、大豆蛋白、酪蛋白、酪蛋白酸钠、乳清蛋白、溶菌酶、半乳甘露聚糖、果胶、羧甲基纤维素、壳聚糖、海藻酸钠、阿拉伯胶、葡聚糖中的一种或几种。
进一步的,所述步骤(2)为:将虾青素酯在10~80℃条件下,按质量分数为2%~50%的添加量溶于油相中,制成虾青素酯的油相溶液。
优选的,所述油相为直链脂肪酸酯、脂肪酸甘油酯中的一种或两种。
进一步的,所述步骤(3)为:将步骤(2)制备的虾青素酯油溶液按质量比1:1~20添加到步骤(1)制备的水相溶液中,同时向体系中加入质量体积比为0.0005~1g/100mL的茶多酚,然后采用高压微射流充分均质乳化,乳化条件为均质压力40~120MPa,处理次数1~3次。
进一步的,所述步骤(4)为:将步骤(3)乳化后的体系用碱性物质调节体系pH值到11~13,然后进行二次均质乳化,乳化方法为剪切均质乳化和高压微射流均质乳化中的至少一种,其中剪切均质乳化的转速为3000~30000rpm,时间为1~10min;高压微射流均质乳化的压力为40~120MPa,处理次数为1~3次。
优选的,所述碱性物质为氢氧化钠、氢氧化钾、氢氧化铵、碳酸氢钠、碳酸氢钾、碳酸钠、碳酸钾中的一种或几种。
进一步的,所述步骤(5)为:将步骤(4)得到的二次乳化后的体系在200~2000rpm搅拌条件下,边搅拌边用酸性物质调节体系pH至6.5~7.2。
优选的,所述酸性物质为醋酸、柠檬酸、盐酸、苹果酸、乳酸、酒石酸、磷酸、葡萄糖酸内酯中的一种或几种。
进一步的,所述步骤(6)的干燥方式为喷雾干燥或冷冻干燥。
本发明的有益效果在于,
1、本发明构建了一种虾青素酯纳米复合物颗粒体系。该体系显著提高了虾青素酯的热稳定性及加工储运稳定性;该体系对虾青素酯具有良好的保护、分散和缓控释效果,因此可有效改善虾青素的水分散性和生物利用率。
2、本发明通过采用二次乳化和二次pH响应的方法,制备到虾青素酯纳米复合物,不使用醇类溶剂和表面活性剂,即可制备得到稳定性良好的虾青素酯颗粒。
3、本发明制备得到的虾青素酯纳米复合物中虾青素酯的包埋率达95%以上,制备得到的粉末干爽,流动性好,在水中分散后的粒径分布为538nm附近,加工应用性能良好。
4、本发明的制备方法简单易操作、成本低、条件温和,过程中虾青素酯不发生化学变化,不改变虾青素酯的结构和生理活性,适合大规模工业化推广;本发明得到的虾青素酯纳米复合物颗粒可广泛用于化工产品、日化用品、药品、食品及保健品等行业,尤其是在固体基质产品领域,市场前景广阔。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,对于本领域普通技术人员而言,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是本发明提供的虾青素酯纳米复合物颗粒制备方法流程图。
具体实施方式
为了使本技术领域的人员更好地理解本发明中的技术方案,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都应当属于本发明保护的范围。
实施例1
如图1所示,一种虾青素酯纳米复合物颗粒的制备方法,制备方法包括如下步骤:
(1)水相溶液的制备:将玉米醇溶蛋白按质量体积比1g/100mL的添加量溶于pH为6.5的磷酸盐缓冲溶液中,于5℃环境下水化4h,得到水相溶液;
(2)油相溶液的制备:将虾青素酯在25℃条件下,按质量体积比为10g/100mL的添加量溶于直链脂肪酸酯中,制成虾青素酯的油溶液;
(3)一次乳化:将步骤(2)制备的虾青素酯油相溶液按质量比1:5添加到步骤(1)制备的水相溶液中,同时向体系中加入质量体积比为0.0025g/100mL的茶多酚,然后采用高压微射流充分均质乳化,乳化条件为均质压力60MPa,处理次数2次;
(4)一次调节体系pH和二次乳化:将步骤(3)乳化后的体系用碳酸氢钾调节体系pH值到11,然后采用高压微射流进行二次均质乳化,乳化条件为均质压力100MPa,处理次数2次;
(5)二次调节体系pH:将步骤(4)得到的二次乳化后的体系在500rpm搅拌条件下,边搅拌边用盐酸调节体系pH至6.5;
(6)喷雾干燥,得到虾青素酯纳米复合物颗粒。
实施例2
一种虾青素酯纳米复合物颗粒的制备方法,制备方法包括如下步骤:
(1)水相溶液的制备:将小麦醇溶蛋白、高粱醇溶蛋白的混合物(小麦醇溶蛋白、高粱醇溶蛋白的质量比为1:1)按质量体积比4g/100mL的添加量溶于pH为7.5的磷酸盐缓冲液中,于15℃环境下水化10h,得到水相溶液;
(2)油相溶液的制备:将虾青素酯在70℃条件下,按质量体积比为45g/100mL的添加量溶于脂肪酸甘油酯中,制成虾青素酯的油溶液;
(3)一次乳化:将步骤(2)制备的虾青素酯油相溶液按质量比1:15添加到步骤(1)制备的水相溶液中,同时向体系中加入质量体积比为0.75g/100mL的茶多酚,然后采用高压微射流充分均质乳化,乳化条件为均质压力80MPa,处理次数3次;
(4)一次调节体系pH和二次乳化:将步骤(3)乳化后的体系用氢氧化钠调节体系pH值到13,然后采用剪切法进行二次均质乳化,乳化条件为转速25000rpm,时间3min;
(5)二次调节体系pH:将步骤(4)得到的二次乳化后的体系在1800rpm搅拌条件下,边搅拌边用乳酸调节体系pH至7.0;
(6)冷冻干燥,得到虾青素酯纳米复合物颗粒。
实施例3
一种虾青素酯纳米复合物颗粒的制备方法,制备方法包括如下步骤:
(1)水相溶液的制备:将大麦醇溶蛋白按质量体积比2.5g/100mL的添加量溶于pH为7.0的去离子水中,于10℃环境下水化8h,得到水相溶液,向水相溶液中添加质量体积比为2.5g/100mL的稳定剂,稳定剂包括质量比为1:1:0.5的大豆蛋白、溶菌酶和壳聚糖;
(2)油相溶液的制备:将虾青素酯在40℃条件下,按质量体积比为30g/100mL的添加量溶于脂肪酸甘油酯中,制成虾青素酯的油溶液;
(3)一次乳化:将步骤(2)制备的虾青素酯油相溶液按质量比1:10添加到步骤(1)制备的水相溶液中,同时向体系中加入质量体积比为0.05g/100mL的茶多酚,然后采用高压微射流充分均质乳化,乳化条件为均质压力80MPa,处理次数3次;
(4)一次调节体系pH和二次乳化:将步骤(3)乳化后的体系用氢氧化铵调节体系pH值到12,然后采用剪切法进行二次均质乳化,乳化条件为转速5000rpm,时间10min;
(5)二次调节体系pH:将步骤(4)得到的二次乳化后的体系在1200rpm搅拌条件下,边搅拌边用醋酸调节体系pH至7.0;
(6)冷冻干燥,得到虾青素酯纳米复合物颗粒。
对比例1
一种虾青素酯纳米复合物颗粒的制备方法,制备方法包括如下步骤:
(1)水相溶液的制备:将大麦醇溶蛋白按质量体积比2.5g/100mL的添加量溶于pH为7.0的去离子水中,于10℃环境下水化8h,得到水相溶液,向水相溶液中添加质量体积比为2.5g/100mL的稳定剂,稳定剂包括质量比为1:1:0.5的大豆蛋白、溶菌酶和壳聚糖;
(2)油相溶液的制备:将虾青素酯在40℃条件下,按质量体积比为30g/100mL的添加量溶于脂肪酸甘油酯中,制成虾青素酯的油溶液;
(3)乳化:将步骤(2)制备的虾青素酯油相溶液按质量比1:10添加到步骤(1)制备的水相溶液中,同时向体系中加入质量体积比为0.05g/100mL的茶多酚,然后采用高压微射流充分均质乳化,乳化条件为均质压力80MPa,处理次数3次;
(4)调节体系pH:将步骤(3)得到的乳化后的体系在1200rpm搅拌条件下,边搅拌边调节体系pH至7.0;
(6)冷冻干燥,得到虾青素酯纳米复合物颗粒。
试验例1稳定性试验
将实施例3和对比例1制得的虾青素酯纳米复合物颗粒于自然条件下密封贮藏30天,然后分别测定其包埋率、虾青素酯保留率、粒径分布和产品状态变化。试验结果分别如下表1、下表2所示。
表1实施例3制得的虾青素酯纳米复合物颗粒稳定性试验数据表
表2对比例1制得的虾青素酯纳米复合物颗粒稳定性试验数据表
试验结果表明,实施例3制备的虾青素酯纳米复合物颗粒中虾青素酯的包埋率达95%以上,贮藏30天后,虾青素酯的包埋率、保留率、粒径和外观状态均无显著变化。而对比例1制备的产品在包埋率、保留率、粒径分布方面都显著低于实施例3,且对比例制备的产品表面存在残留油迹,流动性差,存放一段时间后,会出现结块的现象。该结果表明,本发明通过采用二次乳化和二次pH响应的方法制备纳米复合物,可有效提高虾青素酯的包埋率和稳定性,产品适用性强。
综上所述,本发明方法制备的虾青素酯纳米复合物颗粒,可以显著改善虾青素酯的贮藏稳定性,并且保持优良的水分散性能,实现了虾青素酯的稳态化,充分满足热加工过程需要,并保证产品货架期。
尽管通过参考附图并结合优选实施例的方式对本发明进行了详细描述,但本发明并不限于此。在不脱离本发明的精神和实质的前提下,本领域普通技术人员可以对本发明的实施例进行各种等效的修改或替换,而这些修改或替换都应在本发明的涵盖范围内/任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以权利要求所述的保护范围为准。
Claims (10)
1.一种虾青素酯纳米复合物颗粒的制备方法,其特征在于,所述制备方法包括如下步骤:
(1)水相溶液的制备:将蛋白质溶于去离子水或缓冲溶液中水化,得到水相溶液;
(2)油相溶液的制备:将虾青素酯溶于油相中制成虾青素酯的油溶液;
(3)一次乳化:将步骤(2)制备的虾青素酯油溶液添加到步骤(1)制备的水相溶液中,同时向体系中加入茶多酚,然后采用高压微射流充分均质乳化;
(4)一次调节体系pH和二次乳化:将步骤(3)乳化后的体系用碱性物质调节体系pH值到11~13,然后进行二次均质乳化;
(5)二次调节体系pH:将步骤(4)得到的二次乳化后的体系边搅拌边用酸性物质调节体系pH至6.5~7.2;
(6)干燥。
2.如权利要求1所述的制备方法,其特征在于,所述步骤(1)为:将蛋白质按质量体积比0.5~5g/100mL的添加量溶于pH为6.5~7.5的去离子水或磷酸盐缓冲溶液中,于1~20℃环境下水化2~12h,得到水相溶液;
所述蛋白质为玉米醇溶蛋白、小麦醇溶蛋白、高粱醇溶蛋白、大麦醇溶蛋白中的一种或几种。
3.如权利要求1所述的制备方法,其特征在于,步骤(1)还包括向水相溶液中添加质量体积比为0.1~5g/100mL的稳定剂,所述稳定剂为藻酸丙二醇酯、大豆蛋白、酪蛋白、酪蛋白酸钠、乳清蛋白、溶菌酶、半乳甘露聚糖、果胶、羧甲基纤维素、壳聚糖、海藻酸钠、阿拉伯胶、葡聚糖中的一种或几种。
4.如权利要求1所述的制备方法,其特征在于,所述步骤(2)为:将虾青素酯在10~80℃条件下,按质量分数为2%~50%的添加量溶于油相中,制成虾青素酯的油相溶液;
所述油相为直链脂肪酸酯、脂肪酸甘油酯中的一种或两种。
5.如权利要求1所述的制备方法,其特征在于,所述步骤(3)为:将步骤(2)制备的虾青素酯油溶液按质量比1:1~20添加到步骤(1)制备的水相溶液中,同时向体系中加入质量体积比为0.0005~1g/100mL的茶多酚,然后采用高压微射流充分均质乳化,乳化条件为均质压力40~120MPa,处理次数1~3次。
6.如权利要求1所述的制备方法,其特征在于,所述步骤(4)为:将步骤(3)乳化后的体系用碱性物质调节体系pH值到11~13,然后进行二次均质乳化,乳化方法为剪切均质乳化和高压微射流均质乳化中的至少一种,其中剪切均质乳化的转速为3000~30000rpm,时间为1~10min;高压微射流均质乳化的压力为40~120MPa,处理次数为1~3次。
7.如权利要求6所述的制备方法,其特征在于,所述碱性物质为氢氧化钠、氢氧化钾、氢氧化铵、碳酸氢钠、碳酸氢钾、碳酸钠、碳酸钾中的一种或几种。
8.如权利要求1所述的制备方法,其特征在于,所述步骤(5)为:将步骤(4)得到的二次乳化后的体系在200~2000rpm搅拌条件下,边搅拌边用酸性物质调节体系pH至6.5~7.2。
9.如权利要求8所述的制备方法,其特征在于,所述酸性物质为醋酸、柠檬酸、盐酸、苹果酸、乳酸、酒石酸、磷酸、葡萄糖酸内酯中的一种或几种。
10.如权利要求1所述的制备方法,其特征在于,所述步骤(6)的干燥方式为喷雾干燥或冷冻干燥。
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