CN108451996A - 一种制备玛咖提取物的方法 - Google Patents
一种制备玛咖提取物的方法 Download PDFInfo
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- CN108451996A CN108451996A CN201810349330.XA CN201810349330A CN108451996A CN 108451996 A CN108451996 A CN 108451996A CN 201810349330 A CN201810349330 A CN 201810349330A CN 108451996 A CN108451996 A CN 108451996A
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/31—Brassicaceae or Cruciferae (Mustard family), e.g. broccoli, cabbage or kohlrabi
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K2236/30—Extraction of the material
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
本发明公开了一种制备玛咖提取物的方法，采取酶解处理新鲜玛咖根，细胞破碎充分，保证了提取效率，且原料不需干燥直接使用，耗能少，安全隐患低；采用低温冷冻干燥，干燥过程是在很低的温度下进行，而且基本隔绝了空气，因此有效地抑制了提取物的生物、化学或物理变化，并较好地保存了活性物质，保持原料的色泽。
Description
技术领域
本发明涉及一种提取方法，特别涉及一种制备玛咖提取物的方法。
背景技术
玛咖(Maca)植物学名称及俗称：是十字花科(Cruciferae,Brassicaceae)独行菜属(Lapidium)一年生或两年生草本植物。学名：LepidiummeyeniiWalp.；中文名：玛咖(或玛咖)、秘鲁人参等；英文名：Maca,Pinseng；西班牙文名:maca,maka,maino。原产秘鲁安第斯山区南纬5‐15°的区域，生长地海拔达3800‐4500米，属高原药食两用植物。我国于2001年开始引进玛卡试种，于2003‐2010年，先后在西藏日革则、云南丽江、四川阿坝(小金县、松潘县)海拔3000米以上区域试种成功，从2010年开始，云南丽江和绘绎、四川阿坝(小金、松潘、马尔康等县)进行了规模化种植，种植面积达3万余余，其中云南2.3万余亩、四川0.7万余亩。
玛咖(Maca)主要是利用根茎，富含55种活力营养素，干燥根茎含蛋白质10‐20％、脂肪1.6‐2.2％(含量虽不高但其中多为不饱和脂肪酸，亚油酸和亚麻酸含量达53％以上)、碳水化合物43‐59％、膳食纤维15‐25％，另含有丰富的锌、钙、铁、钛、铷、钾、钠、铜、锰、镁、锶、磷、碘等矿物元素，以及含有维生素C、B1、B2、B6、A、E、B12、B5。天然活性成份包括生物碱、芥子油苷及其分解产物异硫氰酸苄酯、甾醇、多酚类物质等。1999年，美国科学家发现了玛卡中含有两类新的植物活性成份，玛咖酰胺(macamides)和玛咖稀(macaenes)，并确定这两种物质对平衡人体荷尔蒙分泌有显著作用，所以玛咖又被称为天然荷尔蒙发动机。由于玛咖含有多种均衡合理的营养成份以及多种具有生物活性的次生代谢产物，具备多种保健和治疗功效，用于保健主要在增强精力、提高生育力、改善性功能等方面有功效，用于治疗主要对更年期综合症、风湿症、抑郁症、贫血症等症状效果明显，它还具有抗癌和抗白血病等作用。
玛咖的利用主要分两种，一种是以原料利用，玛咖鲜根茎或干根茎作蔬菜食用或以药膳方式食用；二是加工利用，初级加工产品有玛咖片(鲜根茎切片烘干品)、玛咖粉(干根茎、烘干片后粉碎的粉剂品)、玛咖饼干(玛咖粉与面粉等调配而成)玛咖压片糖(玛咖粉与甜味剂、贴合剂配合压制而成)、玛咖与其它中草药配伍的复方产品(如玛咖人参咀嚼片等)、玛咖配制酒与果酒(玛咖根茎、烘干片或粉用60度粮食白酒泡制后调配而成，玛咖粉与葡萄等果实发酵制成玛咖果酒)，深加工产品主要以提取玛咖生物碱等有效成分制成的产品，如玛咖糖果、玛咖饮料、玛咖咖啡、玛咖胶囊、玛咖口服液等食品和保健品。目前，已有多家科研院校和企业正在开展玛咖的芥子油苷及其分解产物异硫氰酸苄酯、甾醇、多酚类物质等营养成分的提取分离技术研发，包括分离纯化玛咖酰胺(macamides)和玛咖稀(macaenes)，已取得积极进展。玛咖生物碱是玛咖根茎组织中最重要的活性成分之一，要了解、利用它们，首先需要把它们从根茎组织体中提取分离出来。到目前提取植物生物碱的方法有多种，传统方法主要有浸渍法、渗漉法、煎煮法、热回流法和索氏提取法等，近20余年来，先后兴起了超声波、微波、超临界、双水相等现代提取新技术的逐渐应用。
专利号CN201310523259提到的采用逆流提取玛卡提取物方法，其未对玛卡粉进行酶类灭活，超微破壁处理，从而会对芥子油苷类成分造成破坏。专利号CN201310457767由于采用了乙酸乙酯等有机溶剂残留，会造成提取物的污染，对未来产品应用有极大的影响。专利号CN201210371187其未对玛卡粉进行酶类的灭活，从而会对芥子油苷类成分造成破坏。CN03128262、CN201410014874采用HP‐20大孔树脂柱、中性氧化铝柱、高速逆流色谱制备等方法制备提取物，在工业生产中较难应用。因此，寻找到一种玛咖提取效率高、纯度高的提取工艺方法是非常必要的。
发明内容
本发明的目的在于提供一种高效低耗、操作简便且得到的制备玛咖提取物的方法。
为了实现上述目的，本发明所采用的技术方案是：一种制备玛咖提取物的方法，它包括如下步骤：
(1)粗提取：将新鲜的玛咖根粉碎，加入相当于玛咖根重量0.1％～0.3％的果胶酶和相当于玛咖根重量0.9％～1.6％的半纤维素酶，25～40℃下酶解处理获得酶解液，将酶解液采用超高压处理进行酶蛋白灭活，获得超高压灭活处理后的原料，然后加入一定量的蒸馏水并搅拌均匀，高压匀浆处理1～3小时，得到匀浆液；
(2)然后在输出功率为600W的微波条件下处理6～10分钟，用乙醇‐表面活性剂在温度为70～90℃条件下提取2～5次，搅拌、离心、收集浸提液；
(3)将浸提液依次经过板框过滤、超滤膜过滤，收集截留分子量大于8000Da的滤液；然后进行超低温冷冻干燥处理，即得到玛咖提取物。
其中，步骤1)所述玛咖选自紫色玛咖、黑色玛咖、白色玛咖中的任意一种或几种的混合。所述高压匀浆处理的压力为60MPa，时间为1小时。
步骤(2)中所述表面活性剂选自聚氧乙烯山梨醇酐单月桂酸酯、聚氧乙烯山梨醇酐单棕榈酸酯、聚氧乙烯山梨醇酐单硬脂酸酯、以及聚氧乙烯山梨醇酐单油酸酯中的任意一种或多种的混合。所述乙醇‐表面活性剂混合浸提液的制备方法为：向乙醇浓度为50～80v/v％的乙醇水溶液中加入乙醇水溶液总质量0.2～2wt％的表面活性剂。
步骤(2)中匀浆液与乙醇‐表面活性剂混合浸提液的质量比为1:5～1:30。所述搅拌的速度为15～45rpm，搅拌时间为10～40分钟。所述离心转速为2000～12000rpm。
步骤(3)中板框过滤所用滤纸过滤目数为100‐300目；所述超滤膜膜分离的截留分子量为8000～10000Da，操作温度25～40℃。所述超低温冷冻干燥的温度为‐20～‐40℃，处理时间为6‐12h。
与现有技术相比，本发明提供的提取玛咖提取物的方法，采取酶解处理新鲜玛咖根，细胞破碎充分，保证了提取效率，且原料不需干燥直接使用，耗能少，安全隐患低；采用低温冷冻干燥，干燥过程是在很低的温度下进行，而且基本隔绝了空气，因此有效地抑制了提取物的生物、化学或物理变化，并较好地保存了活性物质，保持原料的色泽。
具体实施方式
下面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的前提下所获得的所有其他实施例，都属于本发明保护的范围。
【实施例1】
(1)粗提取：将10kg新鲜的白玛咖根粉碎，加入相当于玛咖根重量0.3％的果胶酶和相当于玛咖根重量1.6％的半纤维素酶，40℃下酶解处理获得酶解液，将酶解液采用超高压处理进行酶蛋白灭活，获得超高压灭活处理后的原料，然后加入一定量的蒸馏水并搅拌均匀，高压匀浆处理3小时，得到匀浆液；
(2)然后在输出功率为600W的微波条件下处理10分钟，加入匀浆液10倍重量的乙醇‐聚氧乙烯山梨醇酐单棕榈酸酯在温度为85℃条件下提取4次，然后心在搅拌速度30rpm下搅拌30分钟、在离心转速为10000rpm下离心、收集浸提液；
(3)将浸提液依次经过目数为200目板框过滤、在35℃下超滤膜过滤，收集截留分子量大于8000Da的滤液；然后在‐30℃进行超低温冷冻干燥处理8h，即得到玛咖提取物，经测量茶玛咖总生物碱得率达0.56％。
【实施例2】
(1)粗提取：将10kg新鲜的黑玛咖根粉碎，加入相当于玛咖根重量0.3％的果胶酶和相当于玛咖根重量1.6％的半纤维素酶，40℃下酶解处理获得酶解液，将酶解液采用超高压处理进行酶蛋白灭活，获得超高压灭活处理后的原料，然后加入一定量的蒸馏水并搅拌均匀，在压力为60MPa条件下，高压匀浆处理2小时，得到匀浆液；
(2)然后在输出功率为600W的微波条件下处理80分钟，加入匀浆液5倍质量的乙醇‐聚氧乙烯山梨醇酐单月桂酸酯在温度为85℃条件下提取3次，然后心在搅拌速度45rpm下搅拌40分钟、在离心转速为10000rpm下离心、收集浸提液；
(3)将浸提液依次经过目数为300目板框过滤、在40℃下超滤膜过滤，收集截留分子量大于8000Da的滤液；然后在‐40℃进行超低温冷冻干燥处理10h，即得到玛咖提取物，经测量茶玛咖总生物碱得率达0.82％。
【实施例3】
(1)粗提取：将10kg新鲜的紫玛咖根粉碎，加入相当于玛咖根重量0.3％的果胶酶和相当于玛咖根重量1.6％的半纤维素酶，40℃下酶解处理获得酶解液，将酶解液采用超高压处理进行酶蛋白灭活，获得超高压灭活处理后的原料，然后加入一定量的蒸馏水并搅拌均匀，在压力为60MPa条件下，高压匀浆处理3小时，得到匀浆液；
(2)然后在输出功率为600W的微波条件下处理90分钟，加入匀浆液15倍质量的乙醇‐聚氧乙烯山梨醇酐单月桂酸酯在温度为85℃条件下提取3次，然后心在搅拌速度30rpm下搅拌35分钟、在离心转速为12000rpm下离心、收集浸提液；
(3)将浸提液依次经过目数为200目板框过滤、在40℃下超滤膜过滤，收集截留分子量大于8000Da的滤液；然后在‐30℃进行超低温冷冻干燥处理12h，即得到玛咖提取物，经测量茶玛咖总生物碱得率达3.66％。
上述说明已经充分揭露了本发明的具体实施方式。需要指出的是，熟悉该领域的技术人员对本发明的具体实施方式所做的任何改动均不脱离本发明的权利要求书的范围。相应地，本发明的权利要求的范围也并不仅仅局限于前述具体实施方式。
Claims (8)
1.一种制备玛咖提取物的方法，其步骤如下：
(1)粗提取：将新鲜的玛咖根粉碎，加入相当于玛咖根重量0.1％～0.3％的果胶酶和相当于玛咖根重量0.9％～1.6％的半纤维素酶，25～40℃下酶解处理获得酶解液，将酶解液采用超高压处理进行酶蛋白灭活，获得超高压灭活处理后的原料，然后加入一定量的蒸馏水并搅拌均匀，高压匀浆处理1～3小时，得到匀浆液；
(2)然后在输出功率为600W的微波条件下处理6～10分钟，用乙醇‐表面活性剂在温度为70～90℃条件下提取2～5次，搅拌、离心、收集浸提液；
(3)将浸提液依次经过板框过滤、超滤膜过滤，收集截留分子量大于8000Da的滤液；然后进行超低温冷冻干燥处理，即得到玛咖提取物。
2.根据权利要求1所述的制备玛咖提取物的方法，步骤(1)步骤1)所述玛咖选自紫色玛咖、黑色玛咖、白色玛咖中的任意一种或几种的混合。
3.根据权利要求1所述的制备玛咖提取物的方法，步骤(1)所述高压匀浆处理的压力为60MPa，时间为1小时。
4.根据权利要求1所述的制备玛咖提取物的方法，步骤(2)中所述表面活性剂选自聚氧乙烯山梨醇酐单月桂酸酯、聚氧乙烯山梨醇酐单棕榈酸酯、聚氧乙烯山梨醇酐单硬脂酸酯、以及聚氧乙烯山梨醇酐单油酸酯中的任意一种或多种的混合。
5.根据权利要求4所述的制备玛咖提取物的方法，所述乙醇‐表面活性剂混合浸提液的制备方法为：向乙醇浓度为50～80v/v％的乙醇水溶液中加入乙醇水溶液总质量0.2～2wt％的表面活性剂。
6.根据权利要求1所述的制备玛咖提取物的方法，步骤(2)中匀浆液与乙醇‐表面活性剂混合浸提液的质量比为1:5～1:30。
7.根据权利要求1所述的制备玛咖提取物的方法，步骤(2)中所述搅拌的速度为15～45rpm，搅拌时间为10～40分钟；所述离心转速为2000～12000rpm。
8.根据权利要求1所述的制备玛咖提取物的方法，步骤(3)中板框过滤所用滤纸过滤目数为100‐300目；所述超滤膜膜分离的截留分子量为8000～10000Da，操作温度25～40℃；所述超低温冷冻干燥的温度为‐20～‐40℃，处理时间为6‐12h。
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Application publication date: 20180828 |