CN1244344C - 山楂黄烷醇的分离提取方法 - Google Patents
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Abstract
本发明提供了一种从山楂果实干制品如山楂片或山楂粉中分离提取药理活性物质——-山楂黄烷醇以及山楂膳食纤维素、浓缩山楂汁等产品的方法，具有生产工艺简单、产品成本低等特点。
Description
本发明涉及一种山楂黄烷醇的分离提取方法，特别是一种从山楂果实干制品中分离提取药理活性物质——山楂黄烷醇以及山楂膳食纤维素、山楂汁等产品的方法。
山楂为蔷薇科山楂属植物，在中国有19种，其中以主产于北方的大果山楂(Crataegus pinnatifida Bge.Var.MajorN.E.Br.)最具经济价值，其果实中含有多种生理活性成分，(包括：表儿茶素、二聚原花色素B2、多聚原花色素、类黄酮、熊果酸、齐墩果酸、绿原酸、果酸、有机酸、矿质营养元素等)具有多种药理功效，是我国重要的生物资源，被国家列为药食兼用品种。目前国内山楂果实的粗加工产品有多种，如：山楂糕、果丹皮、山楂片、果酱、果肉型饮料(果茶)、浓缩山楂汁、山楂酒、固体山楂粉等。初级加工产品有速溶山楂茶、山楂果胶、山楂红色素、山楂核烟熏剂、山楂浸膏及一些用它生产的中成药产品。但这些产品没有涉及将山楂果实的主要药理活性成分与一般营养成分进行分离，其产品一般为高糖高热量的普通制品，这与其主要适用于老年心、脑血管疾病患者的特点相矛盾，从而湮没了其活性成分特有的价值。国外山楂深加工技术一般是用同属植物单子山楂(Crataegus monogyna L.)、锐刺山楂(Grataegus oxyacantha L.)、五籽山楂(Crataegus pentagyns W.et K.)等种山楂的叶、花为原料，提取山楂黄酮，不仅所用原料与中国山楂不同，而且主要药理活性部位也与山楂果实中的不同。山楂黄烷醇(flavonol)具有极好的抗氧化等一系列重要的保健药理作用，可用于生产药物、保健(功能)食品、功能性化妆品及食品抗氧化剂等广泛领域。我们已申请的发明专利——一种分离提取山楂黄烷醇的技术(申请号：01103986.8)，是以新鲜果实为原料，先加入水打浆，再经醇沉、浓缩等工序实现的，工艺较复杂，溶剂消耗较大，生产成本较高，且不能实现周年生产。
本发明的目的是提供一种以山楂果实干制品如山楂片或山楂粉为原料，分离提取山楂黄烷醇的新方法，与现有技术相比，它可以进一步简化生产工艺、降低成本，并可实现黄烷醇的周年生产，它同样也可以同时生产山楂膳食纤维素(dietary fiber)和浓缩山楂汁等副产品而无废弃物。
本发明的山楂果实干制品如山楂片或山楂粉中山楂黄烷醇、山楂膳食纤维素、山楂汁等各种物质的分离提取方法，是通过如下方法和步骤实现的：
1.将非粉状山楂干制品粉碎，过40目筛，得到固体山楂粉，或直接将山楂粉过40目筛；
2.取步骤1的山楂粉，加重量百分浓度为65-100％的乙醇浸提，并分离出浸提液和残渣；浸提方式可以是渗漉法，单级或多级浸渍法、连续逆流浸提法或回流法等；
3.将步骤2的残渣在温度低于60℃，真空度在0.08MPa以上条件下真空干燥，即得山楂膳食纤维素；
4.将步骤2中得到的浸提液浓缩并回收乙醇溶剂，为减少有效成分的损失，浓缩过程在真空下进行，其真空度保持在0.06MPa以上，温度不超过60℃，将浸提液浓缩至可溶性固型物的含量为20-60Bx°时，停止浓缩，并冷却；
5.用有机溶剂萃取步骤4中的浓缩液，萃取可以一次完成，也可以分多次进行，萃取后有机溶剂相中主要含黄烷醇；有机溶剂可以是乙酸乙酯或一元醇(包括伯、仲、叔醇，其通式为；CnH2n+10H，n＝3-6)；
6.对步骤5中的萃取液进行减压蒸馏浓缩，回收有机溶剂，然后用真空干燥法或喷雾干燥法得到山楂黄烷醇固体粉未，为保证黄烷醇不被破坏，浓缩温度不超过60℃，真空度在0.06MPa以上，干燥温度应不高于60℃；
7.将步骤5中的萃余液在温度不高于60℃、真空度在0.06MPa以上的条件下，用真空浓缩法制取浓缩山楂汁，其中可溶性固形物的含量可达65Bx°以上，总酸度可达8％以上，富含钙、磷、铁、锌等微量元素。
通过上述方法制取的山楂黄烷醇为多种生理活性成分的混合物，其中主要成分包括表儿茶素(epicatechin)、二聚原花色素B2(procyanidin B2)等黄烷醇类化合物，此外还含有少量绿原酸(chlorogenic acid)、黄酮类(flavonoids)、熊果酸(ursolic acid)和齐墩果酸(oleanolic acid)等。通过上述方法制取的山楂黄烷醇中含有50％(W％)的黄烷醇类化合物。
与以往技术相比，本发明具有以下优点：
1)由于原料改用山楂果实的干制品，其中水分含量低，总体积小，减少了乙醇的用量，降低了溶剂损耗；
2)由于乙醇的蒸发潜热比水小，浸提液中水分含量低，总体积小，因此蒸馏时能耗较低。
3)由于采用高浓度乙醇为提取溶剂，使浸提液中果胶含量降低，对提取液的后续操作(澄清、过滤、浓缩等)也十分有利，易于提高浓缩果汁的浓度。
4)以山楂片或山楂粉为原料，可以实现产品的周年生产，提高了设备的利用率。
5)免去了高温下的打浆、醇沉等工艺环节，减少了黄烷醇的氧化损失，产品得率高且质量好。
下面通过实施例进一步说明本发明：
在本实施例中，通过下列方法和步骤，从山楂片中进行山楂黄烷醇、山楂膳食纤维素和山楂浓缩果汁的分离和提取：
1.将干燥的山楂片粉碎，过40目筛，得固体山楂粉；
2.取步骤1的山楂粉50kg与等重量的浓度为80％的乙醇加入到渗漉桶中，再用150kg80％乙醇淋洗，收集全部浸提液；
3.对步骤2的残渣液进行固液分离，分离出浸提液和残渣，所得浸提液与步骤2的浸提液合并；
4.将残渣在60℃，真空度为0.09MPa的条件下真空干燥，得山楂膳食纤维素约10kg；
5.将步骤2和3中得到的浸提液在60℃，真空度为0.085MPa条件下浓缩至100升，冷却至25℃以下；
6.用200升乙酸乙酯溶剂，分三次萃取步骤5得到的浓缩液，合并萃取液；
7.在0.075MPa真空度和50℃温度下，对步骤6中的萃取液进行减压蒸馏，得膏状固形物，同时回收乙酸乙酯；
8.在真空度0.09MPa和温度低于50℃条件下，对步骤7中的膏状物进行烘干，得固体山楂黄烷醇约1kg；
9.步骤6中的萃余液在真空度为0.090Mpa、温度为60℃条件下浓缩至70BX°，冷却，得浓缩山楂汁约50kg，其中总酸含量为13％。
Claims (1)
1.一种从山楂果实干制品中分离提取山楂黄烷醇、山楂膳食纤维素、山楂汁的方法，其特征在于该分离提取方法是通过如下方法和步骤实现的：
(1)将非粉状山楂干制品粉碎，过40目筛，得到固体山楂粉，或直接将山楂粉过40目筛；
(2)取步骤(1)的山楂粉，用重量百分浓度为65-100％的乙醇浸提，并分离出浸提液和残渣；
(3)将步骤(2)中的残渣在温度低于60℃，真空度在0.08MPa以上条件下真空干燥，得山楂膳食纤维素；
(4)将步骤(2)中得到的浸提液浓缩，浓缩过程在真空下进行，其真空度保持在0.06MPa以上，温度不超过60℃，将浸提液浓缩至可溶性固型物的含量为20-60Bx°时，停止浓缩，并冷却；
(5)用有机溶剂萃取步骤(4)中的浓缩液，有机溶剂为乙酸乙酯或一元醇包括伯、仲、叔醇，其通式为：CnH2n+1OH，n＝3-6；
(6)对步骤(5)中的萃取液进行减压蒸馏浓缩，然后用真空干燥法或喷雾干燥法得到山楂黄烷醇固体粉末，浓缩温度不超过60℃，真空度在0.06MPa以上，干燥温度应不高于60℃；
(7)将步骤(5)中的萃余液在温度不高于60℃、真空度在0.06MPa以上的条件下，用真空浓缩法制取浓缩山楂汁。
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