CN104274505B - 一种独活止痛搽剂的制备方法 - Google Patents
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Abstract
本发明属于中药技术领域,涉及一种独活止痛搽剂的制备方法。具体为采用新鲜独活采用水蒸气法获得独活挥发油,在向挥发油中加入玫瑰香精,并通过纤维滤膜进行过滤从而获得,所得独活止痛搽剂不仅活性好而且稳定性高。
Description
技术领域
本发明属于中药技术领域,涉及一种独活止痛搽剂的制备方法。
背景技术
独活止痛搽剂为伞形科植物独活经提取挥发油制成的搽剂,具有止痛、消肿、散瘀的作用。用于小关节挫伤,韧带、肌肉拉伤及风湿痛。本品为纯中药制剂,辅料为乙醇和玫瑰香精。
目前,独活止痛搽剂(见《中华人民共和国卫生部药品标准》·第十五册)的制法为取独活挥发油10g,加玫瑰香精10g,混匀,加入70%乙醇适量,搅匀,再用70%乙醇调整总量至1000ml,滤过,分装,即得。但是,此工艺中由于独活挥发油中含有大分子的物质(例如,蛋白)从而导致制剂容易浑浊,随着储存时间的延长会产生沉淀,从而影响制剂的稳定性。
另外,在现有技术中,独活挥发油的提取工艺主要有水蒸气蒸馏法、微波萃取法、超临界流体萃取法等,其中微波萃取法需要微波萃取装置,超临界流体萃取需要超临界萃取装置,相对成本较高,水蒸气蒸馏法简单,经典,容易操作,但产率一般较低。就目前而言,本领域中并不存在提取率较高的独活挥发油水蒸气蒸馏法的相关工艺。
发明内容
本发明的目的就是提供一种具有止痛、消肿、散瘀的作用。用于小关节挫伤,韧带、肌肉拉伤及风湿痛的外用药。因本品主要成份为独活挥发油,本发明同时提供了一种独活挥发油的提取方法。
本发明主要解决的问题:一、采用新鲜独活粉碎到最佳粒度,提高挥发油收率;二、对蒸馏后分离的母液采用盐析冷藏法,提高挥发油的收率;三、对配制好的药液采用中空纤维超滤法提高药液的澄清度及在贮藏过程中的稳定性。
本发明一种独活止痛搽剂的制备方法,其包括如下步骤:
(1)取新鲜独活药材,粉碎成粗粉,置多功能提取罐中,药材量为提取罐容积的1/4,加水润湿60分钟。从罐底通入蒸汽,加热,保持蒸汽压力0.12- 0.15Mpa,温度为100-120℃,蒸馏8小时,
(2)从油水分离器中分别接收独活挥发油和母液。母液收集在带冷凝装置的不锈钢贮罐中,加入无机盐溶液,使成浓度为5%,开启制冷机组,用冷水循环保温,使母液温度保持在2-10℃,保温12-24小时。收集上面的油层置油水分离器中,分取挥发油即得。
(3)取独活挥发油10g,加玫瑰香精10g,搅拌混匀,加入70%乙醇300g,搅拌混匀,再用70%乙醇调整总量至1000ml。经过板框过滤,滤膜孔径10μm,再经过超滤,材质:中空纤维,孔径10000道尔顿分子量。超滤完后的药液灌装,即得。
在本发明进一步地的实施方案中,在步骤(1)中,所述粉碎优选将药材粉碎成4-16目筛的粗粉,所述加水优选加入药材量1/10的水。
在步骤(2)中,所述无机盐溶液优选为氯化钠溶液,氯化钠的终浓度优选为5%(重量),母液温度优选为4℃,保温时间优选为16小时。
本发明与现有技术相比,具有如下所述的技术优势:
1、选用新鲜独活,粉碎成粗粉。新鲜独活挥发油含量高,粉碎成过8目筛的颗粒出油率最高,太粗挥发油不易蒸馏出,太细,药材会软化,发粘,同样不利于挥发油的蒸出。
2、油水分离器分离的母液中仍有部分挥发油,采用盐析冷藏法分离母液中的挥发油,提高了挥发油的收率。
3、配制好的药液采用孔径为10000道尔顿分子量中空纤维超滤,使药液澄清,同时在贮藏程中不会出现析油和浑浊现象,保证产品稳定性。
具体实施方式
下面将进一步的详细说明本发明。需要指出的是,以下说明仅仅是对本发明要求保护的技术方案的举例说明,并非对这些技术方案的任何限制。本发明的保护范围以所附权利要求书记载的内容为准。
实施例1
独活挥发油的提取:取新鲜独活药材,粉碎成过8目筛的粗粉,置多功能提取罐中,药材量为提取罐容积的1/4,加药材量1/10的水润湿60分钟。从罐底通入蒸汽,加热,保持蒸汽压力0.12-0.15Mpa,温度为100-120℃,蒸馏8小时,从油水分离器中分别接收独活挥发油和母液。母液收集在带冷凝装置的不锈钢贮罐中,加入氯化钠溶液,使成浓度为5%,开启制冷机组,用冷水循环保温,使母液温度保持在4℃,保温16小时。收集上面的油层置油水分离器中,分取挥发油即得(0.43%重量)。GC-MS分析测定表明所得独活挥发油中主要活性成分含量:蒿本内酯的含量为7.92%(重量);4-异丙基苯甲醇7.36%(重量);α-甜没药醇2.87%(重量)。
配料:取独活挥发油10g,加玫瑰香精10g,搅拌混匀,加入70%乙醇300g,搅拌混匀,再用70%乙醇调整总量至1000ml。
过滤及超滤:经过板框过滤,滤膜孔径10μm,再经过超滤,材质:中空纤维,孔径10000道尔顿分子量。
实施例2
采用不同工艺参数制备独活挥发油,除下表参数外,其他制备方法均同实施例1。
各工艺下独活挥发油得率和主要成分含量
实施例3
(1)采用蛋清致大鼠足肿胀模型考察实施例1和实施例2制备的独活挥发油的抗炎效果,试验方法为:取雄性SD大鼠,220g左右,在大鼠右后足踝关节做标记,按足容积测定法测定右后足容积。ig.给药独活挥发油50mg/kg,模型组给予等量的生理盐水。给药30min后,在大鼠右后足注射10%的鲜鸡蛋清溶液0.1ml致炎,在致炎后240min测定大鼠右后足容积,通过与造模前的足容积相比计算致炎后足肿程度,具体结果如下:
(2)采用醋酸致小鼠疼痛模型考察实施例1和实施例2制备的独活挥发油的止痛效果效果,具体方法为:取ICR小鼠,20g左右,ig给药3天,剂量为25mg/kg,末次给药后,分别ip给予0.2ml醋酸,观察记录注射醋酸后15min内的小鼠扭体次数,具体结果如下:
实施例4
采用不同孔径滤膜进行过滤分别制备独活止痛搽剂(除下表参数外其他制备方法同实施例1),高温高湿(45℃,相对湿度75%)储存3个月,采用GC-MS分别测定搽剂中的独活主要活性成分含量。
实施例1及对比例制备搽剂的主要成分含量(%)
本发明内容仅仅举例说明了要求保护的一些具体实施方案,其中一个或更多个技术方案中所记载的技术特征可以与任意的一个或多个技术方案相组合,这些经组合而得到的技术方案也在本申请保护范围内,就像这些经组合而得到的技术方案已经在本发明公开内容中具体记载一样。
Claims (1)
1. 一种独活止痛搽剂的制备方法,其包括如下步骤:
(1)取新鲜独活药材,粉碎成8目筛的粗粉,置多功能提取罐中,药材量为提取罐容积的1/4,加药材量1/10的水润湿60分钟;从罐底通入蒸汽,加热,保持蒸汽压力0.12- 0.15Mpa,温度为100-120℃,蒸馏8小时,
(2)从油水分离器中分别接收独活挥发油和母液;母液收集在带冷凝装置的不锈钢贮罐中,加入无机盐溶液,使成浓度为5%,开启制冷机组,用冷水循环保温,使母液温度保持在4℃,保温16小时;收集上面的油层置油水分离器中,分取挥发油即得;
(3)取独活挥发油10g,加玫瑰香精10g,搅拌混匀,加入70%乙醇300g,搅拌混匀,再用70%乙醇调整总量至1000ml;经过板框过滤,滤膜孔径10μm,再经过超滤,材质:中空纤维,孔径10000道尔顿分子量;超滤完后的药液灌装,即得。
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