CN106389504B - 一种同时含有绿原酸和挥发油成分的金银花露及制备方法 - Google Patents
一种同时含有绿原酸和挥发油成分的金银花露及制备方法 Download PDFInfo
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Abstract
本发明公开了一种同时含有绿原酸和挥发油成分的金银花露。所述金银花露同时含有绿原酸和挥发油成分，绿原酸的含量大于或等于10mg/100ml，其制备方法是以水为溶剂采用两段式分别萃取金银花中的有效成分，第一段采用低温逆流萃取金银花中绿原酸，第二段将经第一段提取产生的药渣采用高温连续热萃取挥发油成分，然后分别冷却，过滤后按生药量比例调配而成。所得金银花露同时含有绿原酸和挥发油成分，既保证了金银花露具有特征风味、色泽好、口感好，又保证金银花中的绿原酸、黄酮类、芳香成分等有效成分被有效的萃取出来。其优点是所得金银花露同时含有绿原酸和芳香物质，确保临床药效，所得金银花真正具有抗菌消炎、抗病毒、抗肿瘤、清热解毒、清凉去火的作用。
Description
技术领域
本专利公开一种中药制剂或保健食品的加工技术。具体地讲，是公开一种药食两用药材(食材)金银花加工得到的金银花露及其制备方法。
背景技术
金银花别名二花、银花、双花、为忍冬科植物忍冬、红腺忍冬、山银花或毛花柱忍冬的花蕾。我国南北各地均有分布。其性寒、味甘。中医认为金银花具有清热解毒、疏散风热；主治外感风热，温病发热，咽红肿痛、热毒血痢、痈肿疔疮等症。
现代研究表明，金银花含挥发油、木犀草素、黄酮类、绿原酸、皂甙等药效成分，同时富含多糖物质。金银花具有广谱抗菌作用，并有明显的抗炎及解热作用；可降低胆固醇、对某些肿瘤细胞有明显的细胞毒性作用；对胃溃疡有预防作用。
绿原酸具有抗肿瘤、抗菌消炎、抗病毒、增高白血球、保肝利胆、降血压，延缓衰老作用及兴奋中枢神经系统等多种药理作用，对大肠癌、肝癌和喉癌具有显著的抑制作用。
由于金银花以上明确的药理作用，金银花露产品在我国生产历史悠久，销量很大，生产厂家众多，最多时上千家生产企业。但是产品质量令人担忧，绝大多数产品根本不含绿原酸成分，根本无法保证金银花露具有抗病毒、抗菌消炎、抗肿瘤作用。传统的金银花露生产采煎煮法，如发明专利CN201410555429.7富含维C及其他微量元素的金银花露及其制备方法，又如发明专利CN102113694A金银花露的制作方法。传统煎煮法虽能基本保持临床药效，但因为芳香物质挥发损失较大，所得金银花露的金银花特征香味不浓，口感较差，且部分绿原酸长时间高温煎煮有所损失。随着技术进步，厂家一味追求感官和风味，忽视内在品质，现在大多采用蒸馏法制备金银花露，蒸馏法较好保持了金银花中特征芳香物质，金银花露风味突出，色泽好，口感好，但是这种方法生产的金银花露完全不含绿原酸，根本无法保证金银花露具有抗病毒、抗菌消炎、抗肿瘤作用。如发明专利CN1557225A金银花露饮料的制备方法，发明专利CN103120348A金银花露饮料及其生产方法等。
发明内容
为了克服现有技术的不足，本发明所要解决的技术问题是提供一种同时含有绿原酸和挥发油成分的金银花露。
本发明以水为溶剂，采取分段萃取金银花中的有效成分，第一段采取低温逆流萃取，第二段将经第一段提取产生的药渣采取高温连续热萃取，分别冷却、过滤后，按生药比例调配成金银花露。既保证了金银花露具有特征风味、色泽好、口感好，又保证金银花中的绿原酸、黄酮类、芳香成分等有效成分被有效的萃取出来。其优点是所得金银花露同时含有绿原酸和芳香物质，确保临床药效，所得金银花真正具有抗菌消炎、抗病毒、抗肿瘤、清热解毒、清凉去火的作用。
为解决上述技术问题，本发明采用的技术方案如下：
提供一种同时含有绿原酸和挥发油成分的金银花露，其特征在于：所述金银花露同时含有绿原酸和挥发油成分，绿原酸的含量大于或等于10mg/100ml，其制备方法是不使用任何有机溶剂，以水为溶剂采用两段式分别萃取金银花中的有效成分，第一段采用低温逆流萃取金银花中绿原酸，第二段将经第一段提取产生的药渣采用高温连续热萃取挥发油成分，然后分别冷却，过滤后按生药量比例调配而成。
按上述方案，所述的低温逆流萃取为：将金银花药材(食材)用5-10倍量的纯净水，盐酸调pH值3.5-6.8，采用低温(30℃-60℃)逆流萃取，萃取温度为30℃-60℃。
按上述方案，所述的高温连续热萃取为以低温逆流萃取后所收集药渣为原料，采用高温连续热萃取(100℃-115℃)，收集挥发油馏分，萃取温度100℃-115℃。
按上述方案，所述的金银花药材(食材)，别名为二花、银花、双花，为忍冬科植物忍冬、或红腺忍冬、或山银花或毛花柱忍冬的花蕾。
提供一种同时含有绿原酸和挥发油成分的金银花露的制备方法，包括以下步骤：
1.取金银花药材(食材),经含0.1wt％-2.0wt％NaCl的溶液浸润4-8小时，清洗、离心机甩干备用。
2.将经浸润的金银花药材(食材)用5-10倍量的纯净水，盐酸调pH值3.5-6.8，采用低温(30℃-60℃)逆流萃取，萃取温度为30℃-60℃，然将萃取液冷却，静置4-8小时过滤，收集滤液A保存待用。
3.以上述低温逆流萃取后所收集药渣为原料，采用高温连续热萃取(100℃-115℃)，萃取温度100℃-115℃，收集挥发油馏分，快速冷却，静置4-8小时，过滤，收集滤液B保存待用。
4.所得滤液A与上述所得滤液B按比例配伍，减压浓缩或不浓缩，添加适量食品级柠檬酸、苯甲酸钾，添加或不添加蔗糖调配，高温瞬时杀菌，灌装，即得同时含绿原酸和挥发油成分的金银花露；
或将所得滤液A与上述所得滤液B按比例配伍，添加一定比例的果汁或添加一定比例的蔬菜汁调配，添加适量食品级柠檬酸、苯甲酸钾，添加(或不添加)糖调配，高温瞬时杀菌，灌装，即得金银花露饮品。
所得金银花露按照《中国药典》(2015年版P221)绿原酸含量测定，采用HPLC法(通则0512)检测绿原酸的含量。
所得金银花露按《中国药典》(2015年版P1056)采用气相色谱法(通则0521)检测芳樟醇成分。
金银花露绿原酸含量测定：
按照《中国药典》(2015年版P221)绿原酸含量测定，采用HPLC法(通则0512)检测绿原酸的含量。
1260系列高效液相色谱仪(DAD检测器，美国angilent公司)。绿原酸对照品(成都植标化纯生物技术有限公司，PCS0348，Lot:150511)，乙腈为色谱纯，水为超纯水，其余试剂为分析纯。
色谱条件：采用C18色谱柱(4.0mm*250mm，5μm)，流动相乙腈(A)-0.4％磷酸溶液(B)13：87，检测波长327nm，流速1.0mL·min-1，柱温30℃。
根据峰面积计算金银花露绿原酸的含量。
金银花露芳樟醇检测
以芳樟醇为对照品，按《中国药典》(2015年版P1056)采用气相色谱法(通则0521)检测芳樟醇成分。色谱条件：Agilent HP-5毛细管色谱柱(30m×0.25mm×0.25μm)；程序升温，柱温初始50℃，以每分钟10℃升温至80℃，保持10min；进样口温度240℃；检测器温度230℃，MS检测；载气为氮气，流速2.0mL/min；分流进样，分流比10：1；理论塔板数按芳樟醇峰计算不少于20000。
本发明的有益效果是：本发明克服了现有技术不足，既保证了金银花露具有特征风味、色泽好、口感好，又保证金银花中的绿原酸、黄酮类、芳香成分等有效成分被有效的萃取出来，所得金银花露同时含绿原酸和挥发油功效成分，真正具有抗菌消炎、抗病毒、抗肿瘤、清热解毒、清凉去火的作用，确保临床药效。
具体实施方式
下面以具体实施例对本发明的技术实施方案做进一步说明。
实施例一：
1.取金银花药材(食材)10千克，经鉴定为忍冬科植物忍冬的花蕾。经含1.0％NaCL溶液浸润 4小时，清洗、离心机甩干用于萃取有效成分。
2.将经浸润的金银花药材(食材)用50L的纯净水，盐酸调pH值3.5，采用低温 (30℃)逆流萃取，萃取液冷却，静置4-8小时过滤，收集滤液A保存待用。
3.以逆流萃取后所收集药渣为原料，采用高温连续热萃取(105℃)，收集挥发油馏分，快速冷却，静置4小时，过滤，收集滤液B保存待用。
4.所得滤液A与上述所得滤液B按生药量比例配伍，减压浓缩(或不浓缩)，添加适量食品级柠檬酸、苯甲酸钾，添加(或不添加)蔗糖调配，高温瞬时杀菌，灌装，即得同时含绿原酸和挥发油成分的金银花露。
5.所得滤液A与上述所得滤液B按比例配伍，或添加一定比例的果汁调配，或添加一定比例的蔬菜汁调配，添加适量食品级柠檬酸、苯甲酸钾，添加(或不添加)糖调配，高温瞬时杀菌，灌装，即得具有特征风味、色泽好、口感好的金银花露饮品。
6.所得金银花露按照《中国药典》(2015年版P221)绿原酸含量测定，采用HPLC法(通则0512)检测绿原酸的含量，按《中国药典》(2015年版P1056)采用气相色谱法(通则0521)可检测芳樟醇含量。
7.经检测，所得金银花露绿原酸含量为11mg/100ml，经检测含有芳樟醇成分。
实施例二：
1.取金银花药材(食材)10千克，经鉴定为山银花的花蕾。经含2.0％NaCL溶液浸润8小时，清洗、离心机甩干用于萃取有效成分。
2.将经浸润的金银花药材(食材)用100L的纯净水，盐酸调pH值6.5，采用低温 (60℃)逆流萃取，萃取液冷却，静置8小时过滤，收集滤液A保存待用。
3.以逆流萃取后所收集药渣为原料，采用高温连续热萃取(115℃)，收集挥发油馏分，快速冷却，静置4小时，过滤，收集滤液B保存待用。
4.所得滤液A与上述所得滤液B按生药量比例配伍，减压浓缩(或不浓缩)，添加适量食品级柠檬酸、苯甲酸钾，添加(或不添加)蔗糖调配，高温瞬时杀菌，灌装，即得同时含绿原酸和挥发油成分的金银花露。
5.所得滤液A与上述所得滤液B按比例配伍，或添加一定比例的果汁调配，或添加一定比例的蔬菜汁调配，添加适量食品级柠檬酸、苯甲酸钾，添加(或不添加)糖调配，高温瞬时杀菌，灌装，即得具有特征风味、色泽好、口感好的金银花露饮品。
6.所得金银花露按照《中国药典》(2015年版P221)绿原酸含量测定，采用HPLC法(通则0512)检测绿原酸的含量，按《中国药典》(2015年版P1056)采用气相色谱法(通则0521)可检测芳樟醇含量。
7 .经检测所得金银花露，绿原酸含量为16mg/100ml，经检测含有芳樟醇成分。
实施例三：
1.取金银花药材(食材)20千克，经鉴定为毛花柱忍冬的花蕾。经含0.5％NaCL溶液浸润6小时，清洗、离心机甩干用于萃取有效成分。
2.将经浸润的金银花药材(食材)用180L的纯净水，盐酸调pH值5.5，采用低温 (50℃)逆流萃取，萃取液冷却，静置6小时过滤，收集滤液A保存待用。
3.以逆流萃取后所收集药渣为原料，采用高温连续热萃取(110℃)，收集挥发油馏分，快速冷却，静置6小时，过滤，收集滤液B保存待用。
4.所得滤液A与上述所得滤液B按生药量比例配伍，减压浓缩(或不浓缩)，添加适量食品级柠檬酸、苯甲酸钾，添加(或不添加)蔗糖调配，高温瞬时杀菌，灌装，即得同时含绿原酸和挥发油成分的金银花露。
5.所得滤液A与上述所得滤液B按比例配伍，或添加一定比例的果汁调配，或添加一定比例的蔬菜汁调配，添加适量食品级柠檬酸、苯甲酸钾，添加(或不添加)糖调配，高温瞬时杀菌，灌装，即得具有特征风味、色泽好、口感好的金银花露饮品。
6.所得金银花露按照《中国药典》(2015年版P221)绿原酸含量测定，采用HPLC法(通则0512)检测绿原酸的含量，按《中国药典》(2015年版P1056)采用气相色谱法(通则0521)可检测芳樟醇含量。
经检测所得金银花露经检测含有挥发油，绿原酸含量为14mg/100ml经检测含有芳樟醇成分。
以上是本发明的具体实施技术路线和效果，但专利保护并不局限于此。
Claims (3)
1.一种同时含有绿原酸和挥发油成分的金银花露，其特征在于：所述金银花露同时含有绿原酸和挥发油成分，绿原酸的含量大于或等于10mg/100ml，其制备方法是不使用任何有机溶剂，以水为溶剂采用两段式分别萃取金银花中的有效成分，第一段采用低温逆流萃取金银花中绿原酸，第二段将经第一段提取产生的药渣采用高温连续热萃取挥发油成分，然后分别冷却，过滤后按生药量比例调配而成；
所述金银花露的具体制备方法包括以下步骤：
(1)取金银花药材,经含0.1wt％-2.0wt％NaCl的溶液浸润4-8小时，清洗、离心机甩干备用；
(2)将经浸润的金银花药材用5-10倍量的纯净水，盐酸调pH值3.5-6.8，采用低温逆流萃取，萃取温度为30℃-60℃，将萃取液冷却，静置4-8小时过滤，收集滤液A保存待用；
(3)以上述低温逆流萃取后所收集药渣为原料，采用高温连续热萃取，萃取温度100℃-115℃，收集挥发油馏分，快速冷却，静置4-8小时，过滤，收集滤液B保存待用；
(4)所得滤液A与上述所得滤液B按比例配伍，减压浓缩或不浓缩，添加适量食品级柠檬酸、苯甲酸钾，添加或不添加蔗糖调配，高温瞬时杀菌，灌装，即得同时含绿原酸和挥发油成分的金银花露；
或将所得滤液A与上述所得滤液B按比例配伍，添加一定比例的果汁或添加一定比例的蔬菜汁调配，添加适量食品级柠檬酸、苯甲酸钾，添加或不添加糖调配，高温瞬时杀菌，灌装，即得金银花露饮品。
2.根据权利要求1所述的同时含有绿原酸和挥发油成分的金银花露，其特征在于：所述的金银花药材，别名为二花、银花、双花，为忍冬科植物忍冬、或红腺忍冬、或山银花或毛花柱忍冬的花蕾。
3.一种同时含有绿原酸和挥发油成分的金银花露的制备方法，其特征在于：包括以下步骤：
(1)取金银花药材,经含0.1wt％-2.0wt％NaCl的溶液浸润4-8小时，清洗、离心机甩干备用；
(2)将经浸润的金银花药材用5-10倍量的纯净水，盐酸调pH值3.5-6.8，采用低温逆流萃取，萃取温度为30℃-60℃，将萃取液冷却，静置4-8小时过滤，收集滤液A保存待用；
(3)以上述低温逆流萃取后所收集药渣为原料，采用高温连续热萃取，萃取温度100℃-115℃，收集挥发油馏分，快速冷却，静置4-8小时，过滤，收集滤液B保存待用；
(4)所得滤液A与上述所得滤液B按比例配伍，减压浓缩或不浓缩，添加适量食品级柠檬酸、苯甲酸钾，添加或不添加蔗糖调配，高温瞬时杀菌，灌装，即得同时含绿原酸和挥发油成分的金银花露；
或将所得滤液A与上述所得滤液B按比例配伍，添加一定比例的果汁或添加一定比例的蔬菜汁调配，添加适量食品级柠檬酸、苯甲酸钾，添加或不添加糖调配，高温瞬时杀菌，灌装，即得金银花露饮品。
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