CN101434568A - 一种由金盏菊提取物制备高含量叶黄素晶体的方法 - Google Patents
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Abstract
本发明涉及一种由金盏菊提取物制备高含量叶黄素晶体的方法。该方法首先对金盏菊提取物溶于醇碱溶液中和添加抗氧化剂和惰性气体保护进行皂化反应，转化为游离态叶黄素，用去离子水稀释并洗涤至pH值为6.5～7.0，真空干燥得到叶黄素粗品。粗品用非极性或弱极性有机溶剂进行重结晶，离心过滤、冷冻干燥得到产品，产品纯度达到98％以上。本生产工艺简单，溶剂毒量小，且用量少易于回收，易实现工业化生产。该产品可安全有效的应用到食品着色剂、营养添加剂和医药保健品等领域。
Description
(一)技术领域
本发明涉及一种由金盏菊提取物制备高含量叶黄素晶体的方法。
(二)背景技术
类胡萝卜素是自然界中广泛存在的天然色素，到目前为止，人们已发现并分离纯化了700多种类胡萝卜素，叶黄素是类胡萝卜素的一种，目前已发现叶黄素主要有以下几方面的功能：①利用其着色性作为饲料及食品添加剂；②作为其他物质的稳定剂；③防止老年人视黄斑退化；④具有抗癌作用；⑤对心脑血管疾病有防治作用。
叶黄素是绿叶蔬菜和其他多种植物中的一种主要类胡萝卜素，植物体内叶黄素有两种存在形式，游离态和叶黄素酯；游离叶黄素可被人体直接吸收利用，而叶黄素酯则必须在体内水解成游离叶黄素后才能被吸收，因此分离制备高纯度的游离叶黄素已成为许多研究者的课题。金盏菊花叶黄素含量高，是叶黄素生产的主要原料。金盏菊花的有机溶剂萃取物含有大量叶黄素酯，经皂化后虽可转变为游离叶黄素，但皂化产物杂质含量高，直接皂化后的叶黄素仍然不适合作为食品及药物添加剂，须经进一步分离纯化才能达到要求。
浙江海宁凤鸣有限公司开发的从万寿菊制备叶黄素结晶的方法(CN1436774A)，该方法用四氢呋喃、石油醚等混合溶剂重结晶得到叶黄素纯品，提取率在60％以下，皂化反应时间较长，工艺复杂、成本高、溶剂不易回收。
美国专利US 5382714，皂化时有机溶剂用量大，叶黄素分离难度大，产品含量低，重结晶使用有毒溶剂，不利于产品在食品和药品种的应用；
美国专利US 5648564，用45％碱丙二醇溶液皂化，由于丙二醇粘度高，因此同样存在分离难的问题，而且废液种的丙二醇极难回收利用，容易对环境造成污染；
(三)发明内容
本发明的目的在于提供一种工艺简化，成本低、提取率高、污染低且易于规模化生产的从金盏菊提取物制备高含量叶黄素晶体的方法。
本发明提供的高含量叶黄素晶体的制备方法具体步骤如下：
(a)金盏菊提取物溶于醇碱溶液中，进行皂化反应，添加抗氧化剂及惰性气体进行保护，保持温度恒定；
(b)用10～30份无离子水对皂化反应产物进行稀释；
(c)从稀释液中分离、收集叶黄素结晶；
(d)用无离子水洗涤(c)项所得的叶黄素结晶至中性，真空干燥；无离子水的稳定控制在0～15℃；pH值控制在6.5～7.0。
(e)将(d)项所得叶黄素结晶用非极性或弱极性有机溶剂进行重结晶。
(f)离心分离；
(g)进行冷冻干燥。
本发明还有这样一些技术特征：
1、所述的皂化反应中所采用醇碱溶液，有机溶剂为甲醇、乙醇，金属碱化物为氢氧化钾、氢氧化钠；其浓度为20％～30％(重量百分比)；
2、所述的抗氧化剂是维生素C、维生素E，其用量为0.2％～0.5％(重量百分比)；
3、所述的惰性气体为高纯氮气；
4、所述的皂化反应的反应温度20～70℃，皂化时间2～8小时；
5、所述的叶黄素结晶用非极性或弱极性有机溶剂为正己烷、二氯甲烷，具体为将叶黄素结晶用5～20份正己烷洗涤，离心分离，将叶黄素结晶在常温下溶于二氯甲烷中制得饱和溶液，向饱和溶液中滴加0.1～0.5倍正己烷至出现浑浊，离心分离：
6、所述的冷冻干燥时间为20～30小时。
本发明提供的制备方法具有如下优点：
1、工艺简化，直接经皂化、中和、沉淀、提取、结晶、重结晶等步骤，即可得到高纯度的叶黄素晶体；
2、制备工艺中叶黄素破坏和损失均小，故而叶黄素提取率可达90％；
3、制备成本降低20～40％，且有机溶剂毒性低且易回收，残留少，对环境污染小；
4、适用于工业规模化生产，且最终得到的叶黄素符合食品和药品的原料要求。
(四)具体实施方式
下面结合具体实施例对本发明作进一步的说明：
实施例1：
称取40g金盏菊提取物(含量为150g/kg)于100ml圆底烧瓶种，电磁搅拌下依次氢氧化钠5g，甲醇10g，加入维生素C0.2g，60℃水浴，充氮气保护，反应2.5小时，加入5℃去离子水20份进行稀释，离心分离，收集滤渣，用5℃去离子水洗涤滤渣至流出液体pH值为6.5，真空干燥制得叶黄素粗品。将叶黄素粗品各用10份正己烷洗涤两次，离心分离，将叶黄素结晶在常温下溶于二氯甲烷中制得饱和溶液，向饱和溶液中滴加0.2倍正己烷至出现浑浊，离心分离。冷冻干燥时间20小时。得到98％叶黄素晶体5.6g。有效转化率为91.5％。
实施例2：
称取250g金盏菊提取物(含量为150g/kg)于500ml圆底烧瓶种，电磁搅拌下依次氢氧化钾16g，甲醇34g，加入维生素E 1.2g，60℃水浴，充氮气保护，反应2.5小时，加入5℃去离子水20份进行稀释，离心分离，收集滤渣，用5℃去离子水洗涤滤渣至流出液体pH值为6.7，真空干燥制得叶黄素粗品。将叶黄素粗品各用10份正己烷洗涤两次，离心分离，将叶黄素结晶在常温下溶于二氯甲烷中制得饱和溶液，向饱和溶液中滴加0.3倍正己烷至出现浑浊，离心分离。冷冻干燥时间20小时。得到97.7％叶黄素晶体35.5g。有效转化率为92.5％。
实施例3：
称取100g金盏菊提取物(含量为150g/kg)于250ml圆底烧瓶种，电磁搅拌下依次氢氧化钾6g，乙醇22g，加入维生素E 0.5g，60℃水浴，充氮气保护，反应2.5小时，加入5℃去离子水20份进行稀释，离心分离，收集滤渣，用5℃去离子水洗涤滤渣至流出液体pH值为7.0，真空干燥制得叶黄素粗品。将叶黄素粗品各用8份正己烷洗涤两次，离心分离，将叶黄素结晶在常温下溶于二氯甲烷中制得饱和溶液，向饱和溶液中滴加0.3倍正己烷至出现浑浊，离心分离。冷冻干燥时间20小时。得到97.5％叶黄素晶体14.3g。有效转化率为93.0％。
Claims (7)
1.一种从金盏菊提取物中制备高含量叶黄素晶体的方法，其特征在于它包括下列步骤：
(a)金盏菊提取物溶于醇碱的混合溶液中，进行皂化反应，添加抗氧化剂及惰性气体进行保护，保持温度恒定；
(b)用10～30份无离子水对皂化反应产物进行稀释；
(c)从稀释液中分离、收集叶黄素结晶；
(d)用无离子水洗涤(c)项所得的叶黄素结晶至中性，真空干燥；无离子水的稳定控制在0～15℃；pH值控制在6.5～7.0；
(e)将(d)项所得叶黄素结晶用非极性或弱极性有机溶剂进行重结晶。
(f)离心分离；
(g)进行冷冻干燥。
2.根据权利要求1所述的从金盏菊提取物中制备高含量叶黄素晶体的方法，其特征在于所述的皂化反应中所采用醇碱溶液，有机溶剂为甲醇或乙醇，金属碱化物为氢氧化钾或氢氧化钠；其浓度重量百分比为20％～30％。
3.根据权利要求2所述的从金盏菊提取物中制备高含量叶黄素晶体的方法，其特征在于所述的抗氧化剂是维生素C或维生素E，其用量重量百分比为0.2％～0.5％。
4.根据权利要求3所述的从金盏菊提取物中制备高含量叶黄素晶体的方法，其特征在于所述的惰性气体为高纯氮气。
5.根据权利要求4所述的从金盏菊提取物中制备高含量叶黄素晶体的方法，其特征在于所述的反应温度20～70℃，皂化时间2～8小时。
6.根据权利要求5所述的从金盏菊提取物中制备高含量叶黄素晶体的方法，其特征在于所述的叶黄素结晶用非极性或弱极性有机溶剂为正己烷、二氯甲烷。具体为将叶黄素结晶用5～20份正己烷洗涤，离心分离，将叶黄素结晶在常温下溶于二氯甲烷中制得饱和溶液，向饱和溶液中滴加0.1～0.5倍正己烷至出现浑浊，离心分离。
7.根据权利要求6所述的从金盏菊提取物中制备高含量叶黄素晶体的方法，其特征在于所述的冷冻干燥时间为20～30小时。
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| CN103058906A (zh) * | 2013-01-31 | 2013-04-24 | 甘肃省农垦农业研究院 | 叶黄素饲料添加剂生产工艺 |
| CN106631952A (zh) * | 2016-12-26 | 2017-05-10 | 晨光生物科技集团股份有限公司 | 叶黄素纯化晶体的快速脱除溶残的方法 |
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| CN1309693C (zh) * | 2002-02-05 | 2007-04-11 | 海宁凤鸣叶绿素有限公司 | 一种从万寿菊花制备叶黄素结晶的方法 |
| CN1259309C (zh) * | 2004-06-03 | 2006-06-14 | 成都枫澜科技有限公司 | 一种由万寿菊浸膏制备叶黄素晶体的方法 |
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| CN103058906A (zh) * | 2013-01-31 | 2013-04-24 | 甘肃省农垦农业研究院 | 叶黄素饲料添加剂生产工艺 |
| CN106631952A (zh) * | 2016-12-26 | 2017-05-10 | 晨光生物科技集团股份有限公司 | 叶黄素纯化晶体的快速脱除溶残的方法 |
| CN106631952B (zh) * | 2016-12-26 | 2019-03-19 | 晨光生物科技集团股份有限公司 | 叶黄素纯化晶体的快速脱除溶残的方法 |
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