CN115192624B - 一种凉山杜鹃的提取工艺及其应用 - Google Patents
一种凉山杜鹃的提取工艺及其应用 Download PDFInfo
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Abstract
本发明公开了一种凉山杜鹃的提取工艺,包括以下步骤:对凉山杜鹃进行分拣,除去老枝和杂质;对凉山杜鹃加水煎煮,煎煮三次,合并三次煎液,过滤;将过滤后的煎液进行浓缩,浓缩成清膏;在清膏中加入pH调节剂调pH,边搅拌边加入明胶水溶液,开启冷却,冷却至40℃以下;加入乙醇,静置72h,过滤,滤液回收乙醇得到。本发明通过采用质量分数为2%的明胶水溶液和乙醇溶液,可以提高对凉山杜鹃提取物的精制效果,减少凉山杜鹃提取物中杂质的干扰,并且通过采用三次煎煮,并且使煎煮时采用不同的煎煮水量和煎煮温度,使提取的活性物质产率较高,其中含有较高的槲皮素含量。
Description
技术领域
本发明涉及一种凉山杜鹃的提取工艺及其应用,涉及A61K,具体涉及医用的配置品领域。
背景技术
凉山杜鹃生长于海拔1300-2700米的地区中,产于中国四川西部和东南部,贵州东北部以及云南东北部,由于独特的生理环境使得凉山杜鹃中的槲皮素、黄酮类,黄酮苷类物质含量丰富,将凉山杜鹃入药,具有消炎,止咳,平喘,抗氧化的效果。现有技术中的杜鹃提取方法有醋酸乙酯提取、氯仿提物、结晶提取等方法,但是凉山杜鹃提取物与提取基质的分离较困难,并且部分提取介质毒性较高,不适合应用于药物产品的制备中。
中国发明专利CN201610848272.6公开了一种提取白花杜鹃中生物活性成分的方法,通过采用超临界二氧化碳萃取生物活性成分,提高了萃取效率,但是针对杜鹃的花结构进行萃取,萃取工艺较容易,对杜鹃的叶结构萃取时,萃取难度会大大增加。中国发明专利CN200410064550.6公开了一种满山红提取物及其提取方法,采用聚酰胺树脂分离柱,并用澄清剂对上柱液进行澄清,纯化,提高了杜鹃提取物的精制程度,但是分离效率较低,不适合大规模的工业化生产。
发明内容
为了提高凉山杜鹃的提取效率,改善凉山杜鹃提取物的精制程度,本发明的第一个方面提供了一种凉山杜鹃的提取工艺,包括以下步骤:
(1)对凉山杜鹃进行分拣,除去老枝和杂质;
(2)对凉山杜鹃加水煎煮,煎煮三次,合并三次煎液,过滤;
(3)将过滤后的煎液进行浓缩,浓缩至70-80℃下相对密度为1.15的清膏;
(4)在清膏中加入pH调节剂调pH至4-6,边搅拌边加入明胶水溶液,开启冷却,冷却至40℃以下;
(5)加入乙醇,静置72h,过滤,滤液回收乙醇,即得。
作为一种优选的实施方式,所述步骤1中分拣,选择凉山杜鹃的叶或根部分保留。
作为一种优选的实施方式,所述步骤2中煎煮分为三次,第一次煎煮时间为2h,第二处煎煮时间为1.5h,第三次煎煮时间为1h。
作为一种优选的实施方式,所述第一次煎煮水与凉山杜鹃的重量比为(7-9):1,第二次煎煮水与凉山杜鹃的重量比为(5-7):1,第三次煎煮水与凉山杜鹃的重量比为(4-6):1。
作为一种优选的实施方式,所述第一次煎煮水与凉山杜鹃的重量比为8:1,第二次煎煮水与凉山杜鹃的重量比为6:1,第三次煎煮水与凉山杜鹃的重量比为5:1。
作为一种优选的实施方式,所述煎液过80目筛后合并。
申请人发现通过对凉山杜鹃进行三次煎煮,可以提高提取物中活性成分的溶出率,采用不同的加水量和煎煮时间,可以在提高溶出率的基础上改善提取效率。并且每次煎液过滤后重新加水进行煎煮,使细碎的物质也能重新煎煮溶出,煎煮过程中破碎的凉山杜鹃能够在下一次煎煮时溶出更多的组分。
作为一种优选的实施方式,所述步骤2的煎液过80-120目筛后,进行浓缩。
作为一种优选的实施方式,所述步骤2的煎液过110-120目筛后,进行浓缩。
作为一种优选的实施方式,所述步骤2的煎液过120目筛后,进行浓缩。
作为一种优选的实施方式,所述步骤3的浓缩条件为:采用双效浓缩器减压浓缩,蒸汽压力≤0.09MPa,一效真空度为-0.02~-0.08MPa,温度为50-90℃;二效真空度为-0.03~-0.09MPa,温度为40-80℃。
作为一种优选的实施方式,所述pH调节剂选自枸橼酸、苹果酸、葡萄酸、柑橘酸、杏仁酸、酒石酸中的一种或几种的组合。
作为一种优选的实施方式,所述pH调节剂为枸橼酸。
作为一种优选的实施方式,所述步骤4中水的加入体积为清膏体积的2.5-3.5倍,明胶溶液的质量分数为1-3%。
作为一种优选的实施方式,所述步骤4中水的加入体积为清膏体积的3倍,明胶溶液的质量分数为2%。
作为一种优选的实施方式,所述明胶水溶液的制备方法为:加入清膏体积2.5-3.5倍的饮用水,加热至70-80℃,搅拌过程中加入明胶,配成质量分数为1-3%明胶溶液。
作为一种优选的实施方式,所述步骤5中加入乙醇前降温至40℃以下,加入乙醇,使乙醇的体积分数为70-80%。
作为一种优选的实施方式,所述步骤5中加入乙醇前降温至40℃以下,加入乙醇,使乙醇的体积分数为75%。
申请人发现在pH为4-5的环境中,引入明胶溶液与乙醇可以去除凉山杜鹃清膏中含有的部分杂质,减少药物杂质对凉山杜鹃提取物的影响,削弱中药植物提取物中杂质对身体的代谢负担,提高药物纯度,改善药物疗效。猜测可能的原因是明胶微粒溶于水后,能相互吸引,交织形成层层叠叠的网状结构,在清膏中的细小纤维素类杂质由于清膏的粘度较高采用物理沉降的方式难以沉淀过滤,因此通过引入明胶溶液,形成的网状结构可以与细小的纤维素类杂质吸附,凝聚,成块而共沉,经过滤除去。但是申请人发现凉山杜鹃叶和根中含有较多的单宁类物质,具有良好的抑菌,抗氧化效果,采用明胶溶液可以将单宁与杂质一块凝聚排出,影响凉山杜鹃提取物的药物效果。申请人意外发现,通过引入乙醇,使其醇含量达到75%时,单宁与乙醇中的羟基亲和力高于与明胶溶液的亲和力,使单宁重新溶解于凉山杜鹃提取物中,丰富了凉山杜鹃提取物的药物效果。
本发明的第二个方面提供了一种凉山杜鹃的提取工艺的应用,应用于止咳药物的开发制备中。
与现有技术相比,本发明具有以下有益效果:
(1)本发明所述凉山杜鹃的提取工艺,通过采用三次煎煮,并且使煎煮时采用不同的煎煮水量和煎煮温度,使提取的活性物质产率较高,其中含有较高的槲皮素含量。
(2)本发明所述凉山杜鹃的提取工艺,通过采用质量分数为2%的明胶水溶液和乙醇溶液,可以提高对凉山杜鹃提取物的精制效果,减少凉山杜鹃提取物中杂质的干扰。
(3)本发明所述凉山杜鹃的提取工艺,制备得到的凉山杜鹃提取物水分和灰分都较少,槲皮素含量较高,应用于药物中具有止咳,祛痰的功效,特别适用于慢性支气管炎,咳嗽痰多的症状。
具体实施方式
下面通过实施例对本发明进行具体描述。有必要在此指出的是,以下实施例只用于对本发明作进一步说明,不能理解为对本发明保护范围的限制,该领域的专业技术人员根据上述本发明的内容做出的一些非本质的改进和调整,仍属于本发明的保护范围。
另外,如果没有其它说明,所用原料都是市售得到的。
实施例1
一种凉山杜鹃的提取工艺,包括以下步骤:
(1)对凉山杜鹃进行分拣,除去老枝和杂质,保留凉山杜鹃的叶部位;
(2)对凉山杜鹃加水煎煮,煎煮三次,合并三次煎液,过滤,过120目筛;
(3)将过滤后的煎液进行浓缩,浓缩至75℃下相对密度为1.15的清膏;
(4)在清膏中加入pH调节剂调pH至4.5,边搅拌边加入明胶水溶液,开启冷却,冷却至40℃;
(5)加入乙醇,静置72h,过滤,滤液回收乙醇,干燥即得。
步骤2中煎煮分为三次,第一次煎煮时间为2h,水与凉山杜鹃的重量比为8:1;第二处煎煮时间为1.5h,水与凉山杜鹃的重量比为6:1;第三次煎煮时间为1h,水与凉山杜鹃的重量比为5:1。
步骤3的浓缩条件为:采用双效浓缩器减压浓缩,蒸汽压力为0.09MPa,一效真空度为-0.05MPa,温度为85℃;二效真空度为-0.07MPa,温度为65℃。
所述pH调节剂为枸橼酸。
步骤4中水的加入体积为清膏体积的3倍,明胶溶液的质量分数为2%。
所述明胶水溶液的制备方法为:加入清膏体积3倍的饮用水,加热至75℃,搅拌过程中加入明胶,配成质量分数为2%明胶溶液。
步骤5中加入乙醇前降温至40℃以下,加入乙醇,使乙醇的体积分数为75%。
实施例2
一种凉山杜鹃的提取工艺,具体步骤同实施例1,不同点在于,配成明胶溶液后不加入乙醇。
实施例3
一种凉山杜鹃的提取工艺,具体步骤同实施例1,不同点在于,煎煮过程中第一次煎煮时间为2h,水与凉山杜鹃的重量比为10:1;第二处煎煮时间为1.5h,水与凉山杜鹃的重量比为5:1;第三次煎煮时间为1h,水与凉山杜鹃的重量比为4:1。
性能测试
1.浸出物含量测试:依据《中国药典》2010版通则2201,采用醇溶性浸出物测定法项下的热浸法测定,用乙醇做溶剂。
2.槲皮素含量测定:依据《中国药典》2010版通则0521,采用高效液相色谱法测定槲皮素的含量。
3.总灰分:依据《中国药典》2010版通则2302,测定提取物的总灰分。
测试结果见表1。
表1
浸出物含量/% | 槲皮素含量/% | 总灰分/% | |
实施例1 | 32 | 1.32 | 3.6 |
实施例2 | 28 | 1.25 | 3.1 |
实施例3 | 27 | 0.95 | 4.0 |
Claims (4)
1.一种凉山杜鹃的提取工艺,其特征在于,包括以下步骤:
(1)对凉山杜鹃进行分拣,除去老枝和杂质;
(2)对凉山杜鹃加水煎煮,煎煮三次,合并三次煎液,过滤;
(3)将过滤后的煎液进行浓缩,浓缩至70-80℃下相对密度为1.15的清膏;
(4)在清膏中加入pH调节剂调pH至4-6,边搅拌边加入明胶水溶液,开启冷却,冷却至40℃以下;
(5)加入乙醇,静置72h,过滤,滤液回收乙醇,即得;
所述步骤(1)中分拣,选择凉山杜鹃的叶或根部分保留;
所述步骤(2)中煎煮分为三次,第一次煎煮时间为2h,第二处煎煮时间为1.5h,第三次煎煮时间为1h;所述第一次煎煮水与凉山杜鹃的重量比为(7-9):1,第二次煎煮水与凉山杜鹃的重量比为(5-7):1,第三次煎煮水与凉山杜鹃的重量比为(4-6):1;
所述步骤(3)的浓缩条件为:采用双效浓缩器减压浓缩,蒸汽压力≤0.09MPa,一效真空度为-0.02~-0.08MPa,温度为50-90℃;二效真空度为-0.03~-0.09 MPa,温度为40-80℃;
所述步骤(4)明胶溶液中水的体积为清膏体积的2.5-3.5倍,明胶溶液的质量分数为1-3%;所述步骤(5)中加入乙醇前降温至40℃以下,加入乙醇,使乙醇的体积分数为70-80%。
2.根据权利要求1所述凉山杜鹃的提取工艺,其特征在于,所述步骤(2)的煎液过80-120目筛后,进行浓缩。
3.根据权利要求1所述凉山杜鹃的提取工艺,其特征在于,所述pH调节剂选自枸橼酸、苹果酸、葡萄酸、柑橘酸、杏仁酸、酒石酸中的一种或几种的组合。
4.一种根据权利要求1-3任一项所述凉山杜鹃的提取工艺的应用,其特征在于,应用于止咳药物的开发制备中。
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