CN106692316A - 一种双香排石颗粒的制备方法 - Google Patents

一种双香排石颗粒的制备方法 Download PDF

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CN106692316A
CN106692316A CN201611197798.9A CN201611197798A CN106692316A CN 106692316 A CN106692316 A CN 106692316A CN 201611197798 A CN201611197798 A CN 201611197798A CN 106692316 A CN106692316 A CN 106692316A
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文万江
郭伟
杨明
何平清
惠刚
余宣
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Jiangxi Jinshuibao Pharmaceutical Co.,Ltd.
Jiangxi Jimin Kexin Pharmaceutical Co Ltd
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Abstract

本发明涉及一种双香排石颗粒的制备方法,步骤如下:1)取徐长卿、肉桂和土木香粗碎,加入上述药材量1‑3倍的水,蒸馏0.5‑2.5小时,收集挥发油,备用,同时收集上述药材的煎煮液,药渣再加入3‑6倍水煎煮1‑3小时,过滤,得药液与上述煎煮液合并,2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草,加上述药材量6‑10倍的水,煎煮1‑3次,每次1‑3小时,合并煎液,静置,滤过,得滤液,将此处滤液与步骤1的药液合并浓缩得到清膏,加入适量辅料,混匀,制成颗粒干燥,在颗粒上喷入步骤1所得的挥发油,即得。

Description

一种双香排石颗粒的制备方法
技术领域
本发明属于医药技术领域,涉及一种双香排石颗粒的制备方法。
背景技术
泌尿系结石是泌尿系的常见病。结石可见于肾、膀胱、输尿管和尿道的任何部位。但以肾与输尿管结石为常见。临床表现因结石所在部位不同而有异。肾与输尿管结石的典型表现为肾绞痛与血尿,在结石引起绞痛发作以前,病人没有任何感觉,由于某种诱因,如剧烈运动、劳动、长途乘车等,突然出现一侧腰部剧烈的绞痛,并向下腹及会阴部放射,伴有腹胀、恶心、呕吐、程度不同的血尿;膀胱结石主要表现是排尿困难和排尿疼痛,双香排石颗粒功效:利水,通淋,排石,解毒。用于石淋及排除泌尿结石。
双香排石颗粒是由乳香(制)、土木香、肉桂、连钱草、车前子、木通、徐长卿、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草组合成的中药制剂,具有利水,通淋,排石,解毒功能,用于石淋及排除泌尿结石。
目前,双香排石颗粒的制备方法,除肉桂外,其余乳香等十二味加水煎煮二次,第一次3小时,第二次加进肉桂,煎煮2小时,合并煎液,静置,滤过,取滤液浓缩至相对密度1.31~1.34(80~85℃)的清膏。取清膏1份,蔗糖2份,糊精0.5份及适量乙醇,混匀,制成颗粒,干燥,即得。
现有的制备方法存在的问题有:药物疗效不高,药材浪费等问题,所得颗粒储存一定时间会粉碎,而且有效成分降低。为此,申请人对现有的制备方法进行改进,提供一种双香排石颗粒新的制备方法,该方法能够提高双香排石颗粒的疗效,提高双香排石颗粒有效成分含量,同时解决了稳定性和颗粒粉碎的问题。
发明内容
本发明的目的在于提供一种双香排石颗粒的制备方法。
本发明所述的双香排石颗粒的制备方法,由以下中药原料药制备而成:
优选的,本发明所述的双香排石颗粒的制备方法,由以中药原料药制备而成:
制备工艺:
1)取徐长卿、肉桂和土木香粗碎,加入上述药材量1-3倍的水,蒸馏0.5-2.5小时,收集挥发油,备用,同时收集上述药材的煎煮液,药渣再加入3-6倍水煎煮1-3小时,过滤,得药液与上述煎煮液合并,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草,加上述药材量6-10倍的水,煎煮1-3次,每次1-3小时,合并煎液,静置,滤过,得滤液,将此处滤液与步骤1的药液合并浓缩得到清膏,加入适量辅料,混匀,制成颗粒干燥,在颗粒上喷入步骤1所得的挥发油,即得。
优选的,本发明所述的双香排石颗粒的制备方法,包括以下步骤:
方案1:
1)取徐长卿、肉桂和土木香粗碎,加入药材量2.5倍水,蒸馏2小时,收集挥发油,备用,同时收集上述药材的煎煮液,药渣再加入5倍水煎煮2小时,过滤,得药液与上述煎煮液合并,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草,加上述药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,将此处滤液与步骤1所得药液合并浓缩至相对密度1.31~1.34(80~85℃)的清膏,取清膏,加入适量辅料,混匀,制成颗粒干燥,颗粒喷入步骤1所得的挥发油,即得。
方案2:
1)取徐长卿、肉桂和土木香粗碎,加入7倍量75%乙醇,回流2次,每次1.5小时,收集回流液,减压回收乙醇,浓缩至相对密度1.25~1.28(80~85℃)的清膏,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草,加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,浓缩至相对密度1.31~1.34(80~85℃)的清膏,将1)与2)清膏混合,取混合清膏1000g,蔗糖1900g,糊精450g混匀,制成软材,制粒,干燥,整粒,颗粒喷入挥发油,即得。
方案3:
1)取徐长卿、肉桂和土木香粗碎,用75%乙醇100L作溶剂,浸渍72小时后,以每千克每分钟1~3ml的速度渗漉,然后继续补入剩余75%乙醇120L渗漉,收集渗漉液,渗漉液减压回收乙醇,得浓缩回流液备用,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,将此处滤液与1)药液合并浓缩至相对密度1.31~1.34(80~85℃)的清膏,将1)清膏与2)清膏混合,取混合清膏1000g,蔗糖1900g,糊精450g混匀,制成软材,制粒,干燥,整粒,颗粒喷入挥发油即得。
本发明分别对桂皮醛、丹皮酚、土木香内酯和异土木香内酯进行测定,结果如下:
实验结果显示,通过方案2制备得到的药物,有效成分含量最高,因此选择该方法为最优选的制备工艺。
本发明的制备方法是经过大量实验筛选后得到的,通过以下实验进一步说明本发明的有益效果。
方案1:
(1)挥发油提取 取徐长卿、肉桂和木香3味药材提取挥发油,其水溶液滤过后另器收集,药液用200目滤布过滤,备用。
A、蒸馏时间优化
蒸馏时间(小时) 加入药材煎煮的水量(倍) 挥发油的量(L)
0.5 1 0.3
1 1 0.4
2 1 0.5
2.5 1 0.5
实验结果显示,从上表可以看出蒸馏时间2小时较为合理。
B、药材煎煮加入水量优化
蒸馏时间(小时) 加入药材煎煮的水量(倍) 挥发油的量(L)
2 0 0.35
2 1 0.46
2 2.5 0.56
2 3 0.53
实验结果显示,加入药材煎煮的水量(倍)2.5倍的水较为合理。
方案2:
(2)溶剂的筛选
取徐长卿、肉桂和木香用溶剂提取,考察油浸物;颗粒溶化性以黑点进行记分,较差为0,较好为10
从上表可以看出加入7倍量75%乙醇提取比较好。
方案3:
(3)提取方式优化(溶剂数量为药材的7倍)
上表中75%乙醇渗滤时间24小时,表示浸渍24小时后,进行渗滤。
本发明还包括双香排石颗粒的挥发油的制备方法,优化方案如下:
方案1:取徐长卿、肉桂和木香粗碎,加入药材2倍水,蒸馏2小时,收集挥发油,备用,同时收集药材中煎煮液,药渣再加入5倍水煎煮2小时,过滤,得药液与上述煎煮液合并。
方案2:取徐长卿、肉桂和木香粗碎,加入7倍75%乙醇,回流2次,每次1.5小时,收集回流液,减压回收乙醇,得浓缩回流液备用。
方案3:取徐长卿、肉桂和木香粗碎,用75%乙醇100L作溶剂,浸渍72小时后,以每千克每分钟1~3ml的速度渗漉,然后继续补入剩余75%乙醇120L渗漉,收集渗漉液。渗漉液减压回收乙醇,得浓缩回流液备用。
本发明的制备方法是经过大量实验筛选后得到的,以下通过实验数据说明本发明的有益效果:
实验1、有效成分的含量测定
和现有药物相比,药物中有效成分的含量测定
实验2、第6个月加速稳定性试验中有效成分的含量测定,
本发明相对于现有技术而言,大大提高产品的稳定性和质量,减少药物的副作用,同时还提高有效成分的含量,本发明还简化工艺流程,降低成产成本,适合大规模生产。
具体实施方式
通过以下具体实施例对本发明做进一步的说明,但不作为限制。
实施例1:
按下述配比称取原料:
A:取徐长卿、肉桂和木香粗碎,加入药材2倍水,蒸馏2小时,收集挥发油,备用,同时收集药材中煎煮液,药渣再加入5倍水煎煮2小时,过滤,得药液与上述煎煮液合并。
B:乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,将此处滤液与A处药液合并浓缩至相对密度1.31~1.34(80~85℃)的清膏。取清膏1份,蔗糖2份,糊精0.5份及适量乙醇,混匀,制成颗粒干燥,颗粒喷入A处挥发油,即得。
实施例2:
按下述配比称取原料:
A:取徐长卿、肉桂和木香粗碎,加入7倍75%乙醇,回流2次,每次1.5小时,收集回流液,减压回收乙醇,浓缩至相对密度1.25~1.28(80~85℃)。
B:乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,浓缩至相对密度1.31~1.34(80~85℃)的清膏。将A与B清膏混合,取混合清膏1000g,蔗糖1900g,糊精450g混匀,制成软材,制粒,干燥,整粒,颗粒喷入挥发油即得。
实施例3:
按下述配比称取原料:
A:取徐长卿、肉桂和木香粗碎,用75%乙醇100L作溶剂,浸渍72小时后,以每千克每分钟1~3ml的速度渗漉,然后继续补入剩余75%乙醇120L渗漉,收集渗漉液。渗漉液减压回收乙醇,得浓缩回流液备用。
B:乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,将此处滤液与A处药液合并浓缩至相对密度1.31~1.34(80~85℃)的清膏。将A与B清膏混合,取混合清膏1000g,蔗糖1900g,糊精450g混匀,制成软材,制粒,干燥,整粒,颗粒喷入挥发油即得。
实施例4:
按下述配比称取原料:
A:取徐长卿、肉桂和木香粗碎,用75%乙醇1000L作溶剂,浸渍72小时后,以每千克每分钟1~3ml的速度渗漉,然后继续补入剩余75%乙醇1200L渗漉,收集渗漉液。渗漉液减压回收乙醇,得浓缩回流液备用。
B:乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,将此处滤液与A处药液合并浓缩至相对密度1.15~1.20(热测)的清膏。将A与B清膏混合,将蔗糖粉19000g和糊精4500g加入一部制粒机内,加热,喷入混合膏,制粒,干燥,整粒,颗粒喷入挥发油,即得。
实施例5、本发明与现有方法的差异

Claims (5)

1.一种双香排石颗粒的制备方法,其特征在于,由以下原料药加工制成:
制备工艺:
1)取徐长卿、肉桂和土木香粗碎,加入上述药材量1-3倍的水,蒸馏0.5-2.5小时,收集挥发油,备用,同时收集上述药材的煎煮液,药渣再加入3-6倍水煎煮1-3小时,过滤,得药液与上述煎煮液合并,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草,加上述药材量6-10倍的水,煎煮1-3次,每次1-3小时,合并煎液,静置,滤过,得滤液,将此处滤液与步骤1的药液合并浓缩得到清膏,加入适量辅料,混匀,制成颗粒干燥,在颗粒上喷入步骤1所得的挥发油,即得。
2.根据权利要求1所述的制备方法,其特征在于,由以下原料药加工制成:
3.根据权利要求1所述的制备方法,其特征在于,包括以下步骤:
1)取徐长卿、肉桂和土木香粗碎,加入药材量2.5倍水,蒸馏2小时,收集挥发油,备用,同时收集上述药材的煎煮液,药渣再加入5倍水煎煮2小时,过滤,得药液与上述煎煮液合并,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草,加上述药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,将此处滤液与步骤1所得药液合并浓缩至相对密度1.31~1.34(80~85℃)的清膏,取清膏,加入适量辅料,混匀,制成颗粒干燥,颗粒喷入步骤1所得的挥发油,即得。
4.根据权利要求1所述的制备方法,其特征在于,包括以下步骤:
1)取徐长卿、肉桂和土木香粗碎,加入7倍量75%乙醇,回流2次,每次1.5小时,收集回流液,减压回收乙醇,浓缩至相对密度1.25~1.28(80~85℃)的清膏,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草,加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,浓缩至相对密度1.31~1.34(80~85℃)的清膏,将1)与2)清膏混合,取混合清膏1000g,蔗糖1900g,糊精450g混匀,制成软材,制粒,干燥,整粒,颗粒喷入挥发油,即得。
5.根据权利要求1所述的制备方法,其特征在于,包括以下步骤:
1)取徐长卿、肉桂和土木香粗碎,用75%乙醇100L作溶剂,浸渍72小时后,以每千克每分钟1~3ml的速度渗漉,然后继续补入剩余75%乙醇120L渗漉,收集渗漉液,渗漉液减压回收乙醇,得浓缩回流液备用,
2)乳香(制)、连钱草、车前子、木通、石韦、瞿麦、忍冬藤、滑石、冬葵子、甘草加药材量8倍的水,煎煮二次,第一次3小时,第二次煎煮2小时,合并煎液,静置,滤过,得滤液,将此处滤液与1)药液合并浓缩至相对密度1.31~1.34(80~85℃)的清膏,将1)清膏与2)清膏混合,取混合清膏1000g,蔗糖1900g,糊精450g混匀,制成软材,制粒,干燥,整粒,颗粒喷入挥发油即得。
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