CN102308987B - 从沙棘叶中提取糖苷型沙棘黄酮的生产方法 - Google Patents
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Abstract
从沙棘叶中提取糖苷型沙棘黄酮的生产方法，利用新鲜沙棘叶片或挑选的落叶经清洗、磨浆等预处理加工后，用乙醇做溶剂，在超声波的作用下，进一步破碎植物细胞，释放出糖苷型沙棘黄酮——异鼠李素，提取率可达95.6％。相对传统方法具有低温、常压、无有毒溶剂残留、低能耗、萃取周期短、不破坏和降解有效成份、提取率高的优点，适用规模化生产，提升了农产品的附加值。
Description
技术领域
本发明涉及国际专利分类A23L食品或食料的加工提取方法的技术领域，尤其是从沙棘叶中提取糖苷型沙棘黄酮的生产方法。
背景技术
沙棘又名醋柳、酸刺。果汁含有多种维生素、氨基酸、微量元素和黄酮类化合物。沙棘的果实可以治疗烧伤、顽固性溃疡、冻伤、撕裂伤、皮肤表面溃疡、顽固性溃疡，提取物和沙棘片、浸膏等还可治疗胃溃疡、气管炎、褥疮等，以及预防和治疗铅、磷、苯等职业性病，对消化不良、皮下出血、***等均有一定疗效。配方或煎服还治咳嗽、痰多、肺脓肿、肺结核等。种子可作泻药。沙棘果糖浆治疗慢性气管炎，祛痰效果比较好。
沙棘有多种产品，如沙棘冲剂、沙棘酮片、沙棘精、沙棘油等，这些产品对慢性支气管炎、咳嗽、消化不良、缺血性心肌病、缓解心绞痛等，均有良好的效果。沙棘冲剂的功能是止咳祛痰，消食化滞，活血散瘀，补脾健胃。
沙棘籽油对四氯化碳性肝损伤有保护作用，并无急、慢性毒性反应。沙棘油降脂实验表明，具有明显降低外源性高脂实验大鼠血清总胆固醇的作用，能增高大鼠血清HDL-C，使肝脏脂质含量增高。有保护及加速修复胃粘膜的能力，有助于增强抗肿瘤药的治疗作用。沙棘油中含有A族、B族维生素及大量不饱和脂肪酸，给母鸡喂每份含0.5～1.0％沙棘油，可以提高蛋黄和鸡体的脂肪色素。沙棘油有麻醉性质，曾用于治疗烧伤、甲种维生素缺乏、急性糜烂性湿疹、慢性湿疹、霉菌性湿疹、皮脂溢性湿疹、婴儿湿疹、鳞屑状疹、脓性皮炎、皮肤结核等共72人，总有效率62/72。沙棘油治疗创伤，可制成各种剂型，如滴丸或乳剂等。沙棘油治疗烧伤效果显著，青海医学院用西北高原生物研究所提供的沙棘脂溶性溶液，治疗烧伤100例，有效率90％以上。用沙棘制剂浸棉纱覆盖创面，脓性渗出明显减少，上皮肉芽组织生长加快，创面愈合均提高一周左右。
沙棘精中含有丰富的维生素C，对提高运动员能力、改善心血管***机能以及尽快消除疲劳有良好影响，所含钾、镁、钙、钠、铁、锌、铜等，对保证运动员大运动量所消耗的元素及微量元素的补充有重要意义。沙棘精对慢性气管炎咳、喘均有较好的疗效。经治疗61例，对咳嗽、咯痰、喘息、气短等主要症状均有明显疗效，同时对睡眠、促进消化、消除脘腹胀满亦有一定疗效，对肺血流图有不同程度的改善。
沙棘(H ipp op hae rham noid es L.)是胡颓子科沙棘属的灌木亚乔木，沙棘叶中富含黄酮类化合物。总黄酮的提取主要有水浸提法、碱水浸提法以及溶剂回流提取法，这些方法操作繁琐、提取率低。超声波可以使提取介质中的微小气泡压缩、爆裂，破碎原料的细胞壁，加速有效成分的溶出、扩散，可大大缩短提取时间，提高提取效率。超声技术作为一种有效的提取方法，已经应用于天然产物的提取研究中，而超声循环技术是在料液循环流动的过程中施加超声波，是一种提取天然产物的新技术。
沙棘总黄酮对动物多种房性和室性心律失常模型有对抗作用，增加受试小鼠的心肌营养血流量，改善心肌微循环，降低心肌耗氧量作用。临床证明能改善心肌供血状态，改善微循环，缓解心绞痛，改善心悸、胸闷、气短，降低血清胆固醇和甘油三酯，对四氯化碳所致实验性慢性肝炎。有抗病毒、抗硬化、抗炎及增强毛细管的作用。已公开的沙棘加工方法较少。主要从干植物沙棘果肉中提取沙棘黄酮。由于沙棘果可直接食用，或易于作为多种深加工原料，而价格较高，使得现有工艺获得沙棘黄酮成本昂贵，影响进一步应用开发。
例如：在生产工艺方面，又如：专利申请号CN86108906沙棘油的提炼方法，以沙棘种子、果肉、果渣、果汁漂浮物为原料，综合利用了各种制油材料。为了尽可能多地保留活性成份，采用脂肪烃与酮的混合溶剂或单一脂肪烃溶剂进行浸取，以膜式蒸发脱溶，再将所得毛油于同一容器中在温度15～25℃的条件下进行脱胶、脱酸、脱蜡、然后再在低于65℃的条件下脱色、脱臭即得精制制沙棘油。
另外，研究分析认为，沙棘叶片中的黄酮与沙棘果肉中黄酮含量较为接近，一般为0.9-1.3％。其不同之处仅在于，沙棘果肉中苷元型黄酮比例较大，而叶片中以糖苷型为主的沙棘黄酮，以沙棘叶片为原料提取黄酮的方法尚未见公开。
发明内容
本发明的目的是提供一种以沙棘叶片为原料提取黄酮加工处理技术，该技术针对沙棘叶片的特性进行预处理和提取，以期获得较好的提取纯度和提取率。
本发明的发明目的是通过如下技术措施实现的：沙棘叶经过包括磨浆在内的预处理后，加入乙醇经过超声波萃取后，对萃取液进行低温分离、乙醇回收、有效物干燥制得。
磨浆等预处理加工后，用乙醇做溶剂，在超声波的作用下，进一步破碎植物细胞，释放出糖苷型沙棘黄酮——异鼠李素，提取率可达95.6％。相对传统方法具有低温、常压、无有毒溶剂残留、低能耗、萃取周期短、不破坏和降解有效成份、提取率高的优点，适用规模化生产，提升了农产品的附加值。
本发明的有益效果是：利用新鲜沙棘叶片或挑选的落叶经清洗、磨浆等预处理加工后，用乙醇做溶剂，在超声波的作用下，进一步破碎植物细胞，释放出糖苷型沙棘黄酮——异鼠李素，提取率可达95.6％。相对传统方法具有低温、常压、无有毒溶剂残留、低能耗、萃取周期短、不破坏和降解有效成份、提取率高的优点，适用规模化生产，提升了农产品的附加值。
附图说明：
图1是本发明的工艺流程示意简图
具体实施方式
下面结合具体实施方式，进一步阐述本发明。
沙棘叶经过包括磨浆在内的预处理后，加入乙醇经过超声波萃取后，对萃取液进行低温分离、乙醇回收、有效物干燥制得。
具体来说，将沙棘落叶经分拣，用自来水进行浸泡20min并清洗3遍，再用离心机脱水后放入60℃的烘干室内，烘干24h备用。取10kg干燥叶片用粉碎机进行粉碎，用20kg自来水对粉末浸泡20min，搅拌下送入磨浆机进行磨浆预处理；再将液浆注入超声波反应釜内，并加入95％的食用乙醇150kg，输入功率为200W、25kHz间歇式工作方式的超声波，工作和停止时间均设定为2min，反应釜温度保持45℃，整个超声波萃取时间为20min。再将萃取液放入低温分离器中，温度保持10℃，静置12h，取上清液经离心分离器过滤后送入减压蒸馏釜中，升温至50℃，减压至0.08MPa，回收乙醇。釜底萃取物冷却至室温时滤去水，并用去离子水洗涤4次，滤干后放入真空冷冻箱内干燥12h，产品经检测得到糖苷型沙棘黄酮-异鼠李素94.65g，提取率达95.6％。
使用沙棘叶片作为原料，关键是清洗后，应使叶片上的污物及农药残留得到充分的去除，保证了产品的无毒性。
将浸泡过的物料进行磨浆预处理，使物料更加细化，粒度很容易达到0.3-1μm。
当超声波作用于植物浆液时，由于高频振动产生的冲击波形成的空泡在崩溃时形成的高压射流，会对植物细胞产生强大的剪切作用，使植物细胞破裂，加速细胞内的有效物质得到充分释放。
在45-50度温度条件下，利用黄酮易溶于乙醇的特性进行萃取，整个萃取过程需10-30min。
作为较佳实施方式，以低频超声波效果较好，超声波的频率和输出功率，选定为20-30KHz，功率为100-500w。
采用的短暂的间歇式工作方式，并且工作停止时间均设定为2min。采用短暂的间歇式工作方式，以防止超声波在细胞内产生热能累积效应。
本实施例中物料在浸泡润湿状态下磨浆，确保规模化生产时，又不会因粉碎产生的局部高温破坏有效成份，同时减少粉尘。
浸提溶剂采用95％的食用乙醇，与浸泡时加入的水量合并计算，平均乙醇含量在60-70％，满足了萃取时乙醇的有效浓度。
沙棘叶片，特别是落叶原本是一种废弃物，开发叶片提取有效物质，可较大的提升农产品的附加值，使生产成本大幅度下降。
Claims (2)
1.从沙棘叶中提取糖苷型沙棘黄酮的生产方法，其特征是：沙棘叶经过包括磨浆在内的预处理后，加入乙醇经过超声波萃取后，对萃取液进行低温分离、乙醇回收、有效物干燥制得；将沙棘落叶经分拣，用自来水进行浸泡20min并清洗3遍，再用离心机脱水后放入60℃的烘干室内，烘干24h备用，取10kg干燥叶片用粉碎机进行粉碎，用20kg自来水对粉末浸泡20min，搅拌下送入磨浆机进行磨浆预处理；再将液浆注入超声波反应釜内，并加入95％的食用乙醇150kg，输入功率为200W、25kHz间歇式工作方式的超声波，工作和停止时间均设定为2min，反应釜温度保持45℃，整个超声波萃取时间为20min，再将萃取液放入低温分离器中，温度保持10℃，静置12h，取上清液经离心分离器过滤后送入减压蒸馏釜中，升温至50℃，减压至0.08MPa，回收乙醇，釜底萃取物冷却至室温时滤去水，并用去离子水洗涤4次，滤干后放入真空冷冻箱内干燥12h，产品经检测得到糖苷型沙棘黄酮-异鼠李素94.65g，提取率达95.6％。
2.如权利要求1所述的从沙棘叶中提取糖苷型沙棘黄酮的生产方法，其特征在于，将浸泡过的物料进行磨浆，粒度达到0.3-1μm。
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