CN106074757A - 一种用于清热燥湿、泻火解毒的药物制剂的制备方法 - Google Patents
一种用于清热燥湿、泻火解毒的药物制剂的制备方法 Download PDFInfo
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Abstract
一种用于清热燥湿、泻火解毒的药物制剂的制备方法,涉及中药制剂制备的技术领域。该一清颗粒是由黄连、大黄和黄芩为原料,通过超微粉碎、超声波提取和喷雾干燥后,将中药提取物与药用辅料混合,制粒,分装而成。本发明的有益效果是:采用超微粉碎和超声波提取相结合,提取率高,有利于药材的充分利用,有效避免药材中热敏性成分的降解,且通过喷雾干燥,能够使中药提取物迅速干燥,使产品具有良好的分散性、流动性和溶解性,提高药品品质和疗效,该提取制备方法简便易行,适于工业化大生产。
Description
技术领域
本发明涉及中药制剂制备的技术领域,具体为一种用于清热燥湿、泻火解毒的药物制剂的制备方法。
背景技术
一清颗粒是由黄连、大黄和黄芩三味药材组方而成的中药制剂,具有清热燥湿、泻火解毒、化阏止血等功效,主要用于热毒所致的身热烦躁,目赤口疮,咽喉、牙龈肿痛,大便秘结等症及咽炎、扁桃体炎,牙龈炎见上述症候者,亦可用于热盛迫血妄行所致吐血、咯血、鼻血、内痔出血等症的治疗。处方中黄连和黄芩皆具有清热燥湿、泻火解毒等功效,大黄也具有泻火解毒、泻下攻积、清泄湿热和活血祛瘀等作用,该三味药合用,具有良好的清热燥湿、泻火解毒功效。目前,中国专利授权公告号为CN102145049B公开了“一清颗粒的制备方法”的发明专利,该专利通过将黄连和黄芩用水煎煮,大黄用乙醇回流提取的方式提取制备一清颗粒,动物实验表明该制剂具有一定的抗炎作用;中国专利授权公告号为CN103977097B公开了“一清颗粒的制备方法”的发明专利,该专利是先将黄连、大黄和黄芩三位药材分别加水煎煮提取,然后再分别制成颗粒,最后将三种颗粒混合分装而成,以便较好解决产品熔化性的问题。然而,这些发明专利的制备工艺仍是通过直接高温加热煎煮等传统的提取技术,制备工艺相对简单粗糙,易造成药材提取率低,热敏性功效成分受热易降解,影响产品的品质和疗效。
发明内容
本发明的目的是针对上述缺陷,提供一种提取效率高,产品品质好的用于清热燥湿、泻火解毒的药物制剂的制备方法。
本发明的目的是通过以下技术方案予以实现的。
一种用于清热燥湿、泻火解毒的药物制剂的制备方法,由下列重量份的中药原料制成,黄连165-495份、大黄500-1500份、黄芩250-750份,其特征在于采用以下步骤制备:
(1)采用超微粉碎技术分别将黄连、大黄和黄芩粉碎成细粉,备用;
(2)将步骤(1)粉碎的三味药材细粉加入8倍药材重量的水超声提取,提取后滤过,收集滤液;
(3)将步骤(2)中的滤液浓缩至相对密度为1.20-1.35的稠膏;
(4)将步骤(3)的稠膏通过喷雾干燥,成干浸膏粉;
(5)将步骤(4)的干浸膏粉加入各种辅料,混匀,制粒,干燥,分装,即得。
步骤(1)所述的超微粉碎是指将黄连、大黄和黄芩粉碎成粒径为8-20微米的细粉。
步骤(2)所述的超声提取次数为2次,每次1.5-2h,超声波功率为40-80kw,温度为室温。
步骤(4)所述的喷雾干燥的条件和工艺参数包括:入口温度140-350℃,出口温度80-90℃,雾化器转速15000-28000rpm,水分蒸发量120-160kg/h,传动功率15-30kw,加热功率36-72kw,干粉回收率大于95%。
步骤(5)所述的加入的辅料为蔗糖、淀粉、糊精、微晶纤维素、硬脂酸镁的一种或多种。
所述的清热燥湿、泻火解毒的药物制剂还可制成中药散剂、片剂或胶囊剂。
本发明的有益效果是:采用超微粉碎和超声波提取相结合,提取率高,有利于药材的充分利用,有效避免药材中热敏性成分的降解,且通过喷雾干燥,能够使中药提取物迅速干燥,使产品具有良好的分散性、流动性和溶解性,提高药品品质和疗效,该提取制备方法简便易行,适于工业化大生产,在大生产过程中能够节约中药材资源和生产成本。
具体实施方式
以下通过具体实施例对本发明作进一步说明,应该理解的是,这些实施例仅用于说明本发明,并不限制本发明的范围。
实施例1
处方组成:黄连165kg、大黄500kg、黄芩250kg,糊精250kg、蔗糖160kg,共制成120000袋一清颗粒(7.5g/袋)。
采用以下步骤制备:采用超微粉碎技术分别将黄连、大黄和黄芩粉碎成粒径为10微米的细粉,备用;将粉碎的黄连、大黄和黄芩细粉加入8倍药材重量的水超声提取2次,每次1.5h(超声波功率40kw,温度为室温),提取后滤过,收集滤液;将滤液浓缩至相对密度为1.35的稠膏;将稠膏通过喷雾干燥(喷雾干燥的工艺参数为:入口温度160℃,出口温度80℃,雾化器转速15000rpm,水分蒸发量120kg/h,传动功率15kw,加热功率36kw),得干膏粉,加入糊精和蔗糖,混匀,制粒,干燥,分装,即得一清颗粒。
鉴别:(1)取本品8g,加甲醇50ml,浸渍2小时,并时时振摇,滤过,滤液置水浴上蒸干,残渣加水10ml使溶解,再加盐酸1ml,置水浴上加热30分钟,立即冷却,用氯仿20ml分2次提取,合并氯仿提取液,浓缩至约1ml,作为供试品溶液。另取大黄素对照品,加氯仿制成每1ml含0.5mg的溶液,作为对照品溶液。照薄层色谱法(《中国药典》2015年版)试验,吸取上述两种溶液各10μl,分别点于同一以羧甲基纤维素纳为粘合剂的硅胶G薄层板上,以石油醚(60~90℃)-甲酸乙酯-甲酸(15:5:1)的上层液为展开剂,展开,取出, 晾干,置氨气中熏。供试品色谱中,在与对照品色谱相应的位置上,显相同的红色斑点。
(2)取本品8g,加甲醇50ml,浸渍2小时,并时时振摇,滤过,滤液置水浴上浓缩至约1ml,作为供试品溶液。另取盐酸小檗碱对照品,加甲醇制成每1ml含0.5mg的溶液,作为对照品溶液。照薄层色谱法(《中国药典》2015年版)试验,吸取上述两种溶液各10μl,分别点于同一以羧甲基纤维素钠为粘合剂的硅胶G薄层板上,以醋酸乙酯-丁酮-甲酸-水(10:6:1:1)为展开,取出,晾干,置紫外灯(365nm)下检视。供试品色谱中,在与对照品色谱相应的位置上,显相同的黄色荧光斑点。
含量测定:照高效液相色谱法(《中华人民共和国药典》2015年版)测定。
色谱条件与系统适用性试验 用十八烷基硅烷键合硅胶为填充剂,甲醇-0.2mol/L磷酸二氢钠缓冲液(磷酸调pH2.7)(42:58)为流动相;检测波长275nm;理论板数按黄芩苷峰计算不低于5000。对照品溶液的制备 精密称取在105℃干燥至恒重的黄芩甙对照品12.5mg,置250ml量瓶中,用少量甲醇溶解,用重蒸馏水稀释至刻度,摇匀,即得(每1ml中含黄芩苷50μg)。供试品溶液的制备 取本品22.5g,混匀,研细,取约0.75g,精密称定,置100ml量瓶中,加甲醇10ml,超声处理10分钟,用重蒸馏水稀释至刻度,取此液离心10分钟(15000r/min),分取上清液,取得。测定法 分别精密吸取对照品溶液与供试品溶液液各10μl,注入液相色谱仪,测定,计算,即得。本品每1g含黄芩苷(C21H18O11)不得少于3.0mg。
实施例2
处方组成:黄连330kg、大黄1000kg、黄芩500kg,糊精500kg、蔗糖250kg,共制成250000袋一清颗粒(7.5g/袋)。
采用以下步骤制备:采用超微粉碎技术分别将黄连、大黄和黄芩粉碎成粒径为15微米的细粉,备用;将粉碎的黄连、大黄和黄芩细粉加入8倍药材重量的水超声提取2次,每次2h(超声波功率60kw,温度为室温),提取后滤过,收集滤液;将滤液浓缩至相对密度为1.30的稠膏;将稠膏通过喷雾干燥(喷雾干燥的工艺参数为:入口温度240℃,出口温度85℃,雾化器转速22000rpm,水分蒸发量140kg/h,传动功率20kw,加热功率48kw),得干膏粉,加入糊精和蔗糖,混匀,制粒,干燥,分装,即得一清颗粒。
实施例3
处方组成:黄连495kg、大黄1500kg、黄芩750kg,淀粉700kg、蔗糖420kg,共制成330000袋一清颗粒(7.5g/袋)。
采用以下步骤制备:采用超微粉碎技术分别将黄连、大黄和黄芩粉碎成粒径为20微米的细粉,备用;将粉碎的黄连、大黄和黄芩细粉加入8倍药材重量的水超声提取2次,每次2h(超声波功率80kw,温度为室温),提取后滤过,收集滤液;将滤液浓缩至相对密度为1.25的稠膏;将稠膏通过喷雾干燥(喷雾干燥的工艺参数为:入口温度350℃,出口温度90℃,雾化器转速28000rpm,水分蒸发量160kg/h,传动功率20kw,加热功率72kw),得干膏粉,加入淀粉和蔗糖,混匀,制粒,干燥,分装,即得一清颗粒。
实施例4
处方组成:黄连330kg、大黄1000kg、黄芩500kg,淀粉300kg、微晶纤维素200kg,硬脂酸镁80kg,共制成3700000片一清片剂(0.5g/片)。
采用以下步骤制备:采用超微粉碎技术分别将黄连、大黄和黄芩粉碎成粒径为15微米的细粉,备用;将粉碎的黄连、大黄和黄芩细粉加入8倍药材重量的水超声提取2次,每次2h(超声波功率60kw,温度为室温),提取后滤过,收集滤液;将滤液浓缩至相对密度为1.30的稠膏;将稠膏通过喷雾干燥(喷雾干燥的工艺参数为:入口温度240℃,出口温度85℃,雾化器转速25000rpm,水分蒸发量150kg/h,传动功率20kw,加热功率48kw),得干膏粉,加入淀粉和微晶纤维素,混匀,制粒,加硬脂酸镁,压片,即得一清片。
Claims (6)
1.一种用于清热燥湿、泻火解毒的药物制剂的制备方法,由下列重量份的中药原料制成,黄连165-495份、大黄500-1500份、黄芩250-750份,其特征在于采用以下步骤制备:
采用超微粉碎技术分别将黄连、大黄和黄芩粉碎成细粉,备用;
将步骤(1)粉碎的三味药材细粉加入8倍药材重量的水超声提取,提取后滤过,收集滤液;
将步骤(2)中的滤液浓缩至相对密度为1.20-1.35的稠膏;
将步骤(3)的稠膏通过喷雾干燥,成干浸膏粉;
将步骤(4)的干浸膏粉加入各种辅料,混匀,制粒,干燥,分装,即得。
2.根据权利要求1所述的一种用于清热燥湿、泻火解毒的药物制剂的制备方法,其特征在于:步骤(1)所述的超微粉碎是指将黄连、大黄和黄芩粉碎成粒径为8-20微米的细粉。
3.根据权利要求1所述的一种用于清热燥湿、泻火解毒的药物制剂的制备方法,其特征在于:步骤(2)所述的超声提取次数为2次,每次1.5-2h,超声波功率为40-80kw,温度为室温。
4.根据权利要求1所述的一种用于清热燥湿、泻火解毒的药物制剂的制备方法,其特征在于:步骤(4)所述的喷雾干燥的条件和工艺参数包括:入口温度140-350℃,出口温度80-90℃,雾化器转速11700-28000rpm,水分蒸发量120-160kg/h,传动功率15-30kw,加热功率36-72kw,干粉回收率大于95%。
5.根据权利要求1所述的一种用于清热燥湿、泻火解毒的药物制剂的制备方法,其特征在于:步骤(5)所述的加入的辅料为蔗糖、淀粉、糊精、微晶纤维素、硬脂酸镁的一种或多种。
6.根据权利要求1所述的一种用于清热燥湿、泻火解毒的药物制剂的制备方法,其特征在于:所述的清热燥湿、泻火解毒的药物制剂还可制成中药散剂、片剂或胶囊剂。
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