CN107286068A - 一种制备叶黄素晶体油悬剂的方法 - Google Patents
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Abstract
本发明公开了一种制备叶黄素晶体油悬剂的方法,属于保健品加工的技术领域,包括以下步骤:(1)叶黄素晶体制备;(2)按照植物油与乳化剂质量为50:1~100:7的比例加入乳化剂,搅拌,得到混合液;(3)按照混合液与抗氧化剂质量比为250:1~200:1的比例加入抗氧化剂,继续搅拌,并加入叶黄素晶体粉末,进行分阶段剪切乳化;(4)乳化完成后,冷却至室温,得到叶黄素油悬剂。本发明提供了一种稳定性高、保存时间长的叶黄素晶体油悬剂的制备方法。
Description
技术领域
本发明涉及一种制备叶黄素晶体油悬剂的方法,属于保健品加工的技术领域。
背景技术
叶黄素是一种类胡萝卜素,广泛存在于植物的花、叶、果实以及某些藻类生物中,尤其在万寿菊的花瓣中大量存在,其在植物中的存在形式为叶黄素酯,行业内一般釆用皂化植物提取物的方法得到叶黄素。
近年来,有关叶黄素的生物学功能越来越引起人们的关注。叶黄素具有较强的抗氧化作用,可以清除人体内生理代谢过程中产生的有害物质“自由基”,此类“自由基”可造成组织损伤、细胞衰老等病变。早在1995年,美国FDA即已批准叶黄素作为食品补充剂用于食品饮料。我国最近新发布的“食品添加剂新品种及食品用香料名单(卫生部2007年第8号公告)”公告中,叶黄素作为着色剂和营养补充剂可以应用于食品中。
然而,由于叶黄素晶体对光、热和氧的稳定性差;同时叶黄素晶体不溶于水,在植物油中也是微溶,这些弊端都制约了叶黄素晶体的使用。
发明内容
本发明需要解决的技术问题是如何提供一种制备叶黄素晶体油悬剂的方法,制备出易于保存和利用的叶黄素油悬剂,使得其稳定性高、保存时间长。
为解决上述技术问题,本发明所采用的技术方案是:一种制备叶黄素晶体油悬剂的方法,包括以下步骤,
(1)叶黄素晶体制备:
①用乙醇溶解叶黄素油膏,混合均匀,得到稀释液;
②将质量浓度为50~70%的KOH溶液滴加至稀释液中,超声进行皂化反应;
③向皂化完成后的溶液中加入去离子水,搅拌洗涤,重复洗涤2~3次;
④将洗涤液离心分离得到叶黄素晶体;
⑤将叶黄素晶体冷冻干燥,得叶黄素晶体粉末;
(2)按照植物油与乳化剂质量为50:1~100:7的比例加入乳化剂,搅拌,得到混合液;
(3)按照混合液与抗氧化剂质量比为250:1~200:1的比例加入抗氧化剂,继续搅拌,并加入叶黄素晶体粉末,进行分阶段剪切乳化;
(4)乳化完成后,冷却至室温,得到叶黄素油悬剂。
本发明技术方案的进一步改进在于:步骤(1)的②中超声皂化温度为40~50℃,超声时间为2~3小时。
本发明技术方案的进一步改进在于:步骤(2)中植物油是大豆色拉油、菜籽油、葵花籽油、玉米胚芽油、红花油中的一种或多种。
本发明技术方案的进一步改进在于:步骤(2)中乳化剂是蜂蜡与卵磷脂的混合物、斯盘-80、斯盘-20中的一种或两种。
本发明技术方案的进一步改进在于:步骤(2)中蜂蜡与卵磷脂的质量比为2:1~3:1。
本发明技术方案的进一步改进在于:步骤(3)中抗氧化剂为天然VE、迷迭香提取物、茶多酚或植酸。
本发明技术方案的进一步改进在于:步骤(3)中分阶段剪切乳化,第一阶段剪切速率为10000~13000rpm,剪切2~3min,第二阶段的剪切速率为13000~16000rpm,剪切时间为12~15min,乳化的温度为55~65℃。
由于采用了上述技术方案,本发明取得的技术进步是:
本发明提出了一种制备叶黄素晶体油悬剂的方法,由于叶黄素晶体对光、热和氧的稳定性差,同时晶体不溶于水,在植物油中也是微溶,这些弊端制约了叶黄素晶体的使用。在本发明的制备方法中将叶黄素晶体充分的分散在食用油中,加入了适当、适量的乳化剂蜂蜡和卵磷脂,做到乳化性好且没有出现油圈,也避免出现叶黄素的沉降的现象。同时,本发明的制备方法中选择加入了适当的抗氧化剂VE,在空气中的稳定性较好,从而将叶黄素制作成了易于保存和利用的叶黄素油悬剂。可以有效的保护叶黄素免于过分的氧化,同时也扩大了叶黄素的使用范围,可以更有效的用于油基食品。
叶黄的功能性产品更逐渐蓬勃发展,用于食品着色和提高视力水平,预防和治疗AMD等眼病。本发明制备的叶黄素油悬剂可以进一步做成软胶囊,作为保健品方便人们口服用,适宜各类人群缓解视疲劳,抗氧化等。
本发明的原料来自于新疆伊犁的万寿菊种植基地,所产万寿菊鲜花采摘后,经过酶解发酵、脱水、烘干、粉碎、制成颗粒;其次,颗粒经过低温四号溶剂萃取得粗品叶黄素油膏;然后,油膏经过皂化、洗涤、分离、冷冻干燥得叶黄素晶体;最后,把叶黄素晶体粉末均匀分散在植物油中,加入适量的抗氧化剂和乳化剂,通过高剪切乳化机在一定温度和转速下进行乳化,得到叶黄素晶体油悬剂。由此形成了完整的叶黄素油悬剂生产产业链,实现了产业化生产。
本发明将万寿菊系列产品进行进一步的深加工,应用领域广泛,公司利用自身优势对万寿菊种植基地提供先进的技术,使其与国际市场接轨,带动区域经济发展,可完成人均增收3000元。因此,将万寿菊进一步加工制备叶黄素油悬剂,提高了万寿菊产业的科技含量及经济附加值,以此带动万寿菊产业向更宽更深的领域迈进。为我国带来巨大的经济效益和社会效益,并实现绿色农业可持续发展和推进农业现代化奠定坚实的基础。本发明的实施形成完整的产业链,最终把高质量的产品直接应用于医药保健品的生产,完美的实现了从种植、加工、再到高端产品一条高科技产业链。
本发明在制备叶黄素晶体的过程中采用超声皂化技术,降低了皂化温度,加快了皂化时间,使得在皂化过程中降低了叶黄素的损失;同时,采用TLC实验实时监测超声皂化的完成情况,能够及时掌握叶黄素浸膏的皂化进度,有利于缩短皂化的时间,节省成本。在叶黄素晶体制备的后期,用去离子水搅拌并多次洗涤,有利于去离子水与皂化完成后的混合液体充分接触,使得洗涤更彻底,缩短洗涤次数和去离子水的用量。
具体实施方式
下面对本发明做进一步详细说明:
一种制备叶黄素晶体油悬剂的方法,包括有以下步骤:
(1)叶黄素晶体制备:
①用乙醇溶解叶黄素油膏,混合均匀,得到稀释液;
②将配置好的质量浓度为50~70%的KOH溶液滴加至植物提取液中,温度为40~50℃下进行超声皂化反应,超声时间为2~3小时;在超声皂化过程中,采用TLC实验,实时监测叶黄素进浸膏的皂化完成情况,TLC采用展开剂为石油醚与丙酮的混合液,石油醚与丙酮溶液的质量比为10:0.3~10:0.5;
③向皂化完成后的溶液中加入2~3倍的去离子水,搅拌洗涤,重复洗涤2~3次;
④将洗涤液离心分离得到叶黄素晶体,离心转速为4000r/min,离心时间为10~15min;
⑤将叶黄素晶体冷冻干燥,得叶黄素晶体粉末;
(2)按照植物油与乳化剂质量为50:1~100:7的比例加入乳化剂,搅拌,得到混合液,植物油是大豆色拉油、菜籽油、葵花籽油、玉米胚芽油、红花油中的一种或多种,乳化剂是蜂蜡与卵磷脂的混合物、斯盘-80、斯盘-20中的一种或两种;
(3)按照混合液与抗氧化剂质量比为250:1~200:1的比例加入抗氧化剂,抗氧化剂为天然VE、迷迭香提取物、茶多酚或植酸,继续搅拌,并加入叶黄素晶体粉末进行分阶段的的剪切乳化,乳化的温度为55~65℃,第一阶段的剪切速率是10000~13000rpm,剪切2~3min,第二阶段的剪切速率是13000~16000rpm,剪切时间为12~15min;
(4)乳化完成后,冷却至室温,得到叶黄素油悬剂。
下面结合实施例对本发明做进一步详细说明:
实施例1、
(1)叶黄素晶体制备:
①用乙醇溶解叶黄素浸膏,混合均匀,得到稀释液;
②将质量浓度为50~70%的KOH溶液滴加至植物提取液中,超声进行皂化反应;
③向皂化完成后的溶液中加入去离子水,搅拌洗涤,重复洗涤2~3次;
④将洗涤液离心分离得到叶黄素晶体;
⑤将叶黄素晶体冷冻干燥,得叶黄素晶体粉末;
(2)称量88g玉米胚芽油,6g蜂蜡与卵磷脂的混和物(包括4g蜂蜡与2g卵磷脂),在80℃水浴锅中加热,充分混合30min;
(3)向步骤(2)中加入0.5克的VE,继续搅拌5min,将上述混合液冷却至室温,然后加入11.76g由步骤(1)中得到的叶黄素晶体,在55℃的水浴条件下转速为10000rpm,剪切3min,接着13000rpm剪切15min,得到的叶黄素油悬剂冷却至室温。
实施例2、
(1)叶黄素晶体制备:
①用乙醇溶解叶黄素浸膏,混合均匀,得到稀释液;
②将质量浓度为50~70%的KOH溶液滴加至植物提取液中,超声进行皂化反应;
③向皂化完成后的溶液中加入去离子水,搅拌洗涤,重复洗涤2~3次;
④将洗涤液离心分离得到叶黄素晶体;
⑤将叶黄素晶体冷冻干燥,得叶黄素晶体粉末;
(2)称量大豆色拉油和葵花籽油,一共为82g,6g的斯盘-80,在80℃水浴锅中加热,充分混合30min;
(3)向步骤(2)中加入0.5克的迷迭香提取物,继续搅拌5min,将上述混合液冷却至室温,然后加入11.76g由步骤(1)中得到的叶黄素晶体,在60℃的水浴条件下转速为13000rpm,剪切2min,接着16000rpm剪切12min,得到的叶黄素油悬剂冷却至室温。
实施例3、
(1)叶黄素晶体制备:
①用乙醇溶解叶黄素浸膏,混合均匀,得到稀释液;
②将质量浓度为50~70%的KOH溶液滴加至植物提取液中,超声进行皂化反应;
③向皂化完成后的溶液中加入去离子水,搅拌洗涤,重复洗涤2~3次;
④将洗涤液离心分离得到叶黄素晶体;
⑤将叶黄素晶体冷冻干燥,得叶黄素晶体粉末;
(2)称量82g红花油,6g斯盘-20,在80℃水浴锅中加热,充分混合30min;
(3)向步骤(2)中加入0.5克的VE,继续搅拌5min,将上述混合液冷却至室温,然后加入11.76g由步骤(1)中得到的叶黄素晶体,在65℃的水浴条件下转速为12000rpm,剪切3min,接着15000rpm剪切12min,得到的叶黄素油悬剂冷却至室温。
叶黄素油悬剂的质量高低取决于产品的稳定性,质量高的产品可以保存长久且不会出现沉降或植物油上浮的现象。因此,采用本专利方法制备得到的叶黄素晶体油悬剂用离心-紫外的方法评价产品的稳定性。具体做法是:称一定量的叶黄素油悬剂产品在离心管中离心15min,转速为5000r/min;然后,取适量的上层油悬圈,用正己烷稀释一定的倍数后,以正己烷为空白,在波长474nm下,用紫外分光度计测定吸光度A1和离心前的吸光度A0的比值就是衡量产品稳定性情况的一个稳定系数F=(F=A1/A0)。各个实施例中的产品稳定系数如表1:
表1
实施例 | 实施例1 | 实施例2 | 实施例3 |
稳定系数 | 0.84 | 0.80 | 0.88 |
Claims (7)
1.一种制备叶黄素晶体油悬剂的方法,其特征在于:包括以下步骤,
(1)叶黄素晶体制备:
①用乙醇溶解叶黄素油膏,混合均匀,得到稀释液;
②将质量浓度为50~70%的KOH溶液滴加至稀释液中,超声进行皂化反应;
③向皂化完成后的溶液中加入去离子水,搅拌洗涤,重复洗涤2~3次;
④将洗涤液离心分离得到叶黄素晶体;
⑤将叶黄素晶体冷冻干燥,得叶黄素晶体粉末;
(2)按照植物油与乳化剂质量为50:1~100:7的比例加入乳化剂,搅拌,得到混合液;
(3)按照混合液与抗氧化剂质量比为250:1~200:1的比例加入抗氧化剂,继续搅拌,并加入叶黄素晶体粉末,进行分阶段剪切乳化;
(4)乳化完成后,冷却至室温,得到叶黄素油悬剂。
2.根据权利要求1所述的一种制备叶黄素晶体油悬剂的方法,其特征在于:步骤(1)的②中超声皂化温度为40~50℃,超声时间为2~3小时。
3.根据权利要求2所述的一种制备叶黄素晶体油悬剂的方法,其特征在于:步骤(2)中植物油是大豆色拉油、菜籽油、葵花籽油、玉米胚芽油、红花油中的一种或多种。
4.根据权利要求2所述的一种制备叶黄素晶体油悬剂的方法,其特征在于:步骤(2)中乳化剂是蜂蜡与卵磷脂的混合物、斯盘-80、斯盘-20中的一种或两种。
5.根据权利要求4所述的一种制备叶黄素晶体油悬剂的方法,其特征在于:步骤(2)中蜂蜡与卵磷脂的质量比为2:1~3:1。
6.根据权利要求3所述的一种制备叶黄素晶体油悬剂的方法,其特征在于:步骤(3)中抗氧化剂为天然VE、迷迭香提取物、茶多酚或植酸。
7.根据权利要求1~6任一项所述的一种制备叶黄素晶体油悬剂的方法,其特征在于:步骤(3)中分阶段剪切乳化,第一阶段剪切速率为10000~13000rpm,剪切2~3min,第二阶段的剪切速率为13000~16000rpm,剪切时间为12~15min,乳化的温度为55~65℃。
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CN108813616A (zh) * | 2018-07-05 | 2018-11-16 | 河北东之星生物科技股份有限公司 | 一种制备叶黄素水溶性微乳液的方法 |
CN113797182A (zh) * | 2021-10-14 | 2021-12-17 | 云南博瑞生物科技有限公司 | 一种制备叶黄素油悬液的方法 |
CN113797182B (zh) * | 2021-10-14 | 2023-03-10 | 云南博瑞生物科技有限公司 | 一种制备叶黄素油悬液的方法 |
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