CN106723010A - 从藜麦籽实中提取富集多酚的方法 - Google Patents
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Abstract
本发明公开了从藜麦籽实中提取富集多酚的方法，得到藜麦多酚含量为40%的藜麦籽实萃取物，属于植物的有效成分提取分离技术领域。其步骤为将藜麦籽实原料经过乙醇提取后浓缩，调节PH值，充分静置沉淀后过滤，取过滤液上DM130树脂，水洗除杂后用乙醇洗脱，将洗脱液浓缩干燥得到藜麦多酚提取物。
Description
技术领域
本发明属于植物的有效成分的分离提取技术领域，具体涉及从藜麦籽实中提取富集多酚的方法。
背景技术
藜麦是南美洲安第斯地区古老文明的一种主粮，主要种植于秘鲁和玻利维亚等安第斯地区的国家，在我国的西藏、山西、青海等地也开始种植。为了宣传藜麦的营养价值，联合国曾宣布2013年为“国际藜麦年”。由于其外形像谷物，有时候被称为“伪谷物”，但有时又因为其油脂含量较高而被称为“伪油料”。
藜麦口感非常细腻，带有坚果味和泥土的芳香。藜麦含有皂甙，通常在销售前通过机械手段将之除去，或是在烹煮前仔细冲洗，以除去苦味。根据皂甙含量高低，藜麦品种有“苦”、“甜”之分。甜藜麦品种内的皂甙含量非常低。
藜麦的品种多样性，可以在-4到35摄氏度的温度区间、从海平面至海拔4000米以下的空间内生长。有些品种具有耐旱和耐盐的特性，可在恶劣条件下生长，种植成本低，对水的利用效率高。
藜麦的营养价值很高，是一种健康食物。藜麦与大多数其他植物类食物（不包括豆类）的不同之处在于其蛋白质含量较高。藜麦可提供所有必须氨基酸，而且含量均衡，并富含矿物质、维生素、脂肪酸和其他营养成分，是热能和膳食纤维的良好来源。
藜麦整棵植株都可用作青饲料，收获后的残茬也可用于牛、羊、猪、马和家禽的饲料；传统上安第斯地区的土著居民将藜麦的叶茎和籽用于愈合伤口、消肿、舒缓牙痛和尿道消毒，也用来正骨、治疗内出血和驱虫；藜麦的蛋白浓缩物可用于人类或动物营养补充剂的配料；从苦藜麦中提取的皂甙能诱导改变肠道渗透性，促进特定药物的吸收，皂甙由于能形成泡沫可用于洗涤剂、牙膏、洗发香波中，还具有杀虫剂的潜力；藜麦淀粉具有极好的冻融稳定性，可以作为化学改性淀粉的替代品。
多酚是植物次生代谢产物，具有生物活性，广泛存在于植源性食物中。多酚主要分为3 种：黄酮、酚酸和儿茶素。Repo-Carrasco-Valencia等检测了藜麦、苋菜和尾穗苋总酚和可溶性酚酸含量，发现总酚含量变化范围为16.8～59.7 mg/100 g，可溶性酚酸所占比例为7%～61%，且多酚表现出较强的体外抗氧化活性。Zhu Nanqun等从藜麦中分离鉴定了6 种黄酮醇苷、4 种山奈酚苷和2 种槲皮素苷，发现藜麦籽粒中山奈酚3-O-（β-D-呋喃醛（1-2））-β-D-半乳糖皮蒽、山奈酚3-O-（2,6-di-α-L-吡喃鼠李糖苷）-β-D-半乳糖皮蒽、槲皮素3-O-（2,6-di-α-L-吡喃鼠李糖苷）-β-D-半乳糖皮蒽和槲皮素3-O-（2,6-双-α-L-吡喃鼠李糖苷）-β-Dq-半乳糖皮蒽是主要的黄酮苷。Gorinstein等报道藜麦的阿魏酸含量为251.5 μg/g，β-香豆酸含量为0.8 μg/g，咖啡酸含量为6.31 μg/g。卢宇等研究了藜麦种子中多酚的浸提工艺条件，并考察了各因素对多酚得率的影响。结果表明，影响藜麦多酚浸提得率的因素大小顺序为：料液比> 浸提温度> 乙醇体积分数> 浸提时间。最佳工艺条件是：以体积分数49% 的乙醇溶液为提取剂，料液比1:26(g:mL)，浸提温度73℃，浸提时间62min。该工艺条件下，藜麦种子中多酚的浸提得率为226.77mg/100g。阙淼琳等在单因素试验的基础上，采用响应面法优化了藜麦种子中多酚的提取工艺。确定的最佳提取工艺条件为：乙醇体积分数56％，料液比为1:40(g:mL)，浸提温度84℃，浸提时间1.0h。该工艺条件下，藜麦多酚提取量为2.273mg/g。另外，王桂林等研究了藜麦多酚的超声辅助提取工艺，结果表明，最佳提取工艺为：体积分数70% 的乙醇溶液为提取剂，料液比1:25(g:mL)，超声温度50℃，超声波功率320W，超声时间20min。此提取工艺条件下，藜麦多酚的得率为0.215%。
以上对藜麦籽实中多酚提取方法的研究仅限于实验室的研究，如果进行工业化操作，需要对提取条件进行进一步的细致化和提高效率，同时为满足保健品等下游商家的需要，需要一个能获得更高多酚含量的工艺。
发明内容
本发明的目的在于提供从藜麦籽实中提取富集多酚的方法，为藜麦多酚的进一步深化应用，提供了一条有效制备途径。
为了实现上述目的，本发明的技术解决方案为从藜麦籽实中提取富集多酚的方法，包括以下步骤：
（1）将藜麦籽实，用乙醇加热回流提取，然后浓缩得浸膏；
（2）将浓缩浸膏用自来水稀释，用盐酸调节PH值，充分搅拌后静置分层，板框过滤；
（3）将过滤液过DM130树脂进行吸附，吸附完毕先用自来水冲洗至色淡，再用70%乙醇洗脱；
（4）将洗脱液继续浓缩、干燥得到40%含量的藜麦多酚。
本发明从藜麦籽实中提取富集多酚的方法，其中所述步骤（1）中乙醇的浓度为50~90%，提取1~6次，提取真空度为0.04~0.08MPa，提取溶剂和原料的比例为1.5~5∶1，第一次提取加热到20~40℃温浸20~60分钟后，再开始提取。
本发明从藜麦籽实中提取富集多酚的方法，其中所述步骤（1）中浓缩操作，是先进行常压浓缩，当检测浓缩液的乙醇纯度低于40%时进行减压浓缩，减压浓缩的真空度为0.04~0.08MPa，当检测浓缩液的比重为1~1.2时停止浓缩。
本发明从藜麦籽实中提取富集多酚的方法，其中所述步骤（2）中的自来水稀释倍数为5~10倍，调节PH值为5~6，搅拌时间为10~60分钟，静置时间为2~24小时。
本发明从藜麦籽实中提取富集多酚的方法，其中所述步骤（3）中通过DM130树脂的流速为0.5~5升/分钟，70%乙醇洗脱的体积为树脂体积的3~8倍量。
本发明的工艺具有如下特点：
1 对乙醇提取工艺进行了进一步的细化和便于操作，如在提取加加上温浸环节，提高提取得率，在乙醇浓缩时采用常压和减压两步浓缩，提高了乙醇的回收纯度和回收率；
2 使用了树脂吸附和调PH值改变溶解度的方式，富集有效成分，去除杂质，降低了生产成本，便于操作。
具体实施方式
下面结合实施例具体说明从藜麦籽实中提取富集多酚的方法。
实施例1
本发明含从藜麦籽实中提取富集多酚的方法实施例，其制备步骤为：
（1）将干燥的藜麦籽实用80%乙醇回流提取2次，提取真空度为0.04MPa，提取溶剂和原料的比例为2.5∶1，第一次提取加热到20~40℃温浸30分钟后，再开始提取；
（2）提取完毕后，先进行常压浓缩，当检测浓缩液的乙醇纯度低于40%时进行减压浓缩，减压浓缩的真空度为0.04MPa，当检测浓缩液的比重为1.05时停止浓缩；
（3）将浓缩浸膏用8倍量的自来水稀释，用盐酸调节PH值为5~6，搅拌20分钟后静置分层4小时，用板框过滤；
（4）将过滤液过DM130树脂进行吸附，流速为2.0~3.0升/分钟，吸附完毕先用自来水冲洗至色淡，再用树脂体积5倍量的70%乙醇洗脱；
（5）将洗脱液继续浓缩、干燥得到藜麦多酚，按照植物多酚常规测定方法测试，含量为42.5%。
以上所述实施例仅仅是对本发明的优选实施方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通工程技术人员对本发明的技术方案作出的各种变形和改进，均应落入本发明的权利要求书确定的保护范围内。
Claims (5)
1.从藜麦籽实中提取富集多酚的方法，其特征在于，包括以下步骤：
（1）将藜麦籽实，用乙醇加热回流提取，然后浓缩得浸膏；
（2）将浓缩浸膏用自来水稀释，用盐酸调节PH值，充分搅拌后静置分层，板框过滤；
（3）将过滤液过DM130树脂进行吸附，吸附完毕先用自来水冲洗至色淡，再用70%乙醇洗脱；
（4）将洗脱液继续浓缩、干燥得到40%含量的藜麦多酚。
2.如权利要求1所述的制备方法，其特征在于，所述步骤（1）中乙醇的浓度为50~90%，提取1~6次，提取真空度为0.04~0.08MPa，提取溶剂和原料的比例为1.5~5∶1，第一次提取加热到20~40℃温浸20~60分钟后，再开始提取。
3.如权利要求1所述的制备方法，其特征在于，所述步骤（1）中浓缩操作，是先进行常压浓缩，当检测浓缩液的乙醇纯度低于40%时进行减压浓缩，减压浓缩的真空度为0.04~0.08MPa，当检测浓缩液的比重为1~1.2时停止浓缩。
4.如权利要求1所述的制备方法，其特征在于，所述步骤（2）中的自来水稀释倍数为5~10倍，调节PH值为5~6，搅拌时间为10~60分钟，静置时间为2~24小时。
5.如权利要求1所述的制备方法，其特征在于，所述步骤（3）中通过DM130树脂的流速为0.5~5升/分钟，70%乙醇洗脱的体积为树脂体积的3~8倍量。
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