CN104435113A - 用于制备复方鱼腥草滴丸的黄芩提取物的制备方法 - Google Patents
用于制备复方鱼腥草滴丸的黄芩提取物的制备方法 Download PDFInfo
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Abstract
本发明公开了用于制备复方鱼腥草滴丸的黄芩提取物的制备方法。该制备方法包括以下步骤:(1)黄芩加水提取,得提取液;(2)提取液浓缩至浓缩液体积L为药材重量kg的6-20倍;(3)浓缩液用酸调节pH值至1.0~2.0,50℃-90℃保温,静置,过滤,得沉淀物;(4)沉淀物加水搅匀,50℃-90℃保温,静置,过滤,循环操作1-2次,沉淀物再加30%-70%的乙醇溶液搅匀,静置,过滤,循环操作1-2次,得沉淀物或再经干燥、粉碎,即为黄芩提取物。
Description
技术领域
本发明涉及中药领域,特别涉及一种黄芩提取物的制备方法。
背景技术
咽炎、扁桃体炎是上呼吸道感染常见的症状,中医属喉科之喉蛾、喉痹范畴,是外感风热引起的。西医则认为,咽炎、扁桃体炎是咽喉粘膜及其淋巴组织的炎症,病因主要是细菌、病毒感染、理化因素粉尘、烟酒等刺激,也可继发于全身性疾病或是其他疾病的前期症状,治疗大多采用抗生素类药物辅以含化片剂等方法,但疗效往往不理想,症状虽有减轻,但咽喉的肿痛、干痒等症常迁延难愈、不易根除,有的数月不愈,从而导致了抗生素滥用。
中医运用整体观念和辩证论治对外风热引起的咽喉疼痛、急性咽炎、扁桃体炎常采用清热解毒的办法。收载于《中华人民共和国药典》的复方鱼腥草片具有清热解毒的功效,用于外感风热引起的咽喉疼痛;急性咽炎、扁桃腺炎有风热证候者。申请人通过改变提取工艺,并将其制成速效制剂——滴丸剂,起效快,更加符合中医急症急治的治疗原则,并于2007年申请了发明专利“复方鱼腥草滴丸的制备方法(公开号:CN101040950A)”。由于滴丸载药量较小,需要对提取物进行精制,上述发明中黄芩提取物的精制方法有待改进,精制过程黄芩苷的损失较大,而黄芩苷是黄芩中的主要药效成分。
发明内容
本发明的目的在于提供一种用于制备复方鱼腥草滴丸的黄芩提取物的制备方法,本发明制备方法更加科学合理,制备得到的黄芩提取物黄芩苷损失小,更加有利于保证制剂的临床疗效。
本发明涉及的复方鱼腥草滴丸是由以下重量配比原料药制备而成:鱼腥草1000-1300份、黄芩250-350份、板蓝根250-350份、连翘100—150份、金银花100—150份。
本发明提供的黄芩提取物制备方法包括如下步骤:
(1)黄芩加水提取,得提取液;
(2)提取液浓缩至浓缩液体积L为药材重量kg的6-20倍;
(3)浓缩液用酸调节pH值至1.0~2.0,50℃-90℃保温,静置,过滤,得沉淀物Ⅰ;
(4)沉淀物Ⅰ加水搅匀,50℃-90℃保温,静置,过滤,循环操作1-2次,得沉淀物Ⅱ;
(5)沉淀物Ⅱ加30%-70%的乙醇溶液搅匀,静置,过滤,循环操作1-2次,得沉淀物或再经干燥、粉碎,即为黄芩提取物。
本发明提供的黄芩提取物制备方法包括如下步骤:
(1)黄芩加8-12倍量水提取2-3次,得提取液;
(2)提取液浓缩至浓缩液体积L为药材重量kg的8-12倍;
(3)浓缩液用酸调节pH值至1.5~2.0,70℃-80℃保温,静置,过滤,得沉淀物Ⅰ;
(4)沉淀物Ⅰ加水搅匀,70℃-80℃保温,静置,过滤,循环操作1-2次,循环操作1-2次,得沉淀物Ⅱ;
(5)沉淀物Ⅱ加30%-70%的乙醇溶液搅匀,静置,过滤,循环操作1-2次,得沉淀物或再经干燥、粉碎,即为黄芩提取物。
采用本发明黄芩提取物制备复方鱼腥草滴丸的方法如下:
(1)鱼腥草、板蓝根、连翘、金银花混合或单独提取挥发油;
(2)步骤(1)提取挥发油后的药渣加水提取,提取液过滤,滤液浓缩至在60℃时相对密度为1.10~1.30,加乙醇使含醇量达到60%—85%,静置,过滤,滤液回收乙醇并浓缩成流浸膏,备用;
(3)将黄芩提取物加入到上述流浸膏中,加入挥发油,混匀,制成滴丸,即得;
其中,步骤(1)中提取挥发油的方法可以采用水蒸气蒸馏;
其中,步骤(3)制滴丸所用基质选自脂溶性基质和水溶性基质中的一种或几种,脂溶性基质选自:硬脂酸、单硬脂酸甘油酯、虫蜡、蜂蜡、石蜡、氢化植物油、半合成脂肪酸酯;水溶性基质选自聚乙二醇、聚氧乙烯单硬脂酸脂、泊洛沙姆、硬脂酸钠、甘油明胶;木糖醇与淀粉复合物,赤藓糖醇;优选的基质为重量比为3∶1的聚乙二醇6000和聚乙二醇4000混合物;药物成分与基质的重量比为1∶1-6,优选1∶3。
下面通过一些实验例对本发明作进一步说明。
实验例1黄芩提取液浓缩比例考察
将黄芩提取液等分成三份,第一份浓缩至浓缩液的体积(L)为药材重量(kg)的5倍,第二份浓缩至浓缩液的体积(L)为药材重量(kg)的10倍,第三份浓缩至浓缩液的体积(L)为药材重量(kg)的17倍,三份样品浓缩后用稀盐酸调节pH值至1.8,70℃-80℃保温1小时,静置24小时,过滤,测定沉淀物中黄芩苷的量,以原药材中黄芩苷量为参照,计算黄芩苷的转移率。
结果:第一份样品黄芩苷的转移率67.17%,第二份样品黄芩苷的转移率为75.52%,第三份样品黄芩苷的转移率为69.32%。由此可见,黄芩提取液浓缩至适当的比例再进行酸沉,可以提高黄芩苷的转移率。
实验例2黄芩提取液酸沉得到的沉淀物处理方法的考察
将黄芩提取液浓缩至浓缩液的体积(L)为药材重量(kg)的10倍,用稀盐酸调节pH值至1.8,70℃-80℃保温1小时,平均分成3份,分别静置24小时,过滤,第一份沉淀物加水搅匀,加水量(L)为药材重量(kg)的10倍,70℃-80℃保温1小时,静置24小时,过滤,沉淀物加50%乙醇搅匀,50%乙醇用量(L)为药材重量(kg)的4倍,静置24小时,过滤,得黄芩提取物;第二份沉淀物依次用50%乙醇、水洗,50%乙醇和水的用量(L)均为药材重量(kg)的4倍,得黄芩提取物;第三份沉淀物按现行生产工艺,依次用95%乙醇、水洗,95%乙醇和水的用量(L)为药材重量(kg)的2倍和4倍,得黄芩提取物;将三份黄芩提取物减压干燥,分别测定黄芩苷的含量,并以原药材中黄芩苷量为参照,计算黄芩苷的转移率,结果见表1.
表1 黄芩提取液酸沉得到的沉淀物处理方法的考察结果
由表1结果可知,第一份黄芩提取物重量与采用现行生产工艺得到的黄芩提取物(第三份黄芩提取物)相近,不会影响滴丸的成型,但第一份黄芩提取物的黄芩苷含量要明显高于现行生产工艺。
实验例3滴丸成型工艺研究
1、基质的选择:常用的基质有:聚乙二醇(PEG4000,PEG 6000)、甘油明胶、硬脂酸、虫蜡、氢化植物油等。本试验中选用熔点低同时具有分散力和较大内集力的PEG-4000和用于调整滴丸硬度、耐热性和流动性的PEG-6000进行成型处方的设计和筛选。
2、冷凝剂的确定:水溶性基质要选脂溶性的冷却剂。分别选择液状石蜡、二甲基硅油、花生油为冷凝剂:以药物成分:基质PEG-6000为1:2和1:3;以滴头口径(内/外,mm)2.0/5.0,药液温度70℃,冷凝剂温度-5℃为实验条件:以沉降速度、硬度、圆整度为观察指标。结果表明,滴丸在液体石蜡中沉降速度适中,圆整度好,硬度好,故选择液状石蜡为冷凝剂。
3、成型处方筛选:先将不同配比的PEG-4000和PEG-6000基质处方作基质,熔融,再将混合均匀的药物成分分别加入到熔融的基质中,并不断搅拌加热使之混合均匀,保持在一定温度(80℃)下,以液状石蜡为冷凝剂进行滴制。以组成处方PEG-6000:PEG-4000=3:1为基质制成的滴丸粘结情况较佳,圆整度、硬度能符合滴丸剂的要求。
4、滴丸成型工艺条件优选:在滴丸的制备工艺中,基质种类、中药提取物与基质的混合比例、滴制温度、滴头口径、冷却剂温度等是滴丸成型的重要因素,在单因素筛选的基础上,以PEG-6000:PEG-4000=3:1为基质,液状石蜡为冷凝剂,滴头口径(内/外,mm)定为2.0/5.0。以重量差异、溶散时限、外观质量(硬度,色泽均匀度,圆整度,粘丸,拖尾)为评价指标,对药物成分与基质比例、滴制温度、冷却剂温度等因素进行正交试验优选。结果表明:滴丸最佳成型工艺为:滴制温度为75℃,冷却剂温度为-5℃,中药提取物:基质=1:3(g/g)。滴丸成型率平均为96.07%。
实验例4对二甲苯诱导的小鼠耳肿胀的影响
取小鼠30只,随机分为3组,每组10只,即空白对照组(等容积)、实施例1复方鱼腥草滴丸组(1.7g·kg-1)、对比例1复方鱼腥草滴丸组(1.7g·kg-1)。Ig给药,连续7d,于末次给药后1h,在小鼠左耳两面粉以100%二甲苯,右耳为对照,4h后处死小鼠,沿耳廊基线煎下两耳,用6mm直径打孔器制备小鼠耳片,用电子秤称湿重,以两耳重量之差作为肿胀度(炎症指标)。结果见表2。
表2 复方鱼腥草制剂对二甲苯诱导的小鼠耳肿胀的影响
组别 | 剂量(g·kg-1) | 耳肿胀度(△mg) |
空白对照组 | — | 9.27±1.85 |
实施例1复方鱼腥草滴丸组 | 1.7 | 5.58±2.13** |
对比例1复方鱼腥草滴丸组 | 1.7 | 7.01±2.17* |
与空白对照组相比,**P<0.01;*P<0.05.
具体实施方式
下述实施例用于说明本发明,但不用来限制本发明的范围。
实施例1滴丸剂
鱼腥草1166g 黄芩300g 板蓝根300g
连翘116g 金银花116g
上述药材按如下方法制成1000g滴丸:
上述五味药材,鱼腥草、板蓝根、连翘、金银花四味合并,加12倍量水,蒸馏提取挥发油2小时,收集挥发油备用;过滤,收取滤液,药渣再加10倍量水煎煮2次,每次1小时,过滤,收集滤液,合并三次滤液,浓缩至相对密度约为1.15(60℃),加乙醇使含醇量达70%,放置过夜,过滤,滤液回收乙醇后并浓缩成清膏。黄芩加10倍量水煎煮3次,每次1小时,合并滤液,浓缩至体积为药材重量的10倍,用稀盐酸调pH1.8~2.0,70-80℃保温1小时,静置24小时,过滤,沉淀物加10倍药材量的水搅拌均匀,70-80℃保温1小时,静置24小时,过滤,沉淀物加4倍药材量的50%乙醇搅拌均匀,静置24小时,过滤,真空干燥,粉碎,得黄芩提取物粉,加入清膏中混匀浓缩至流浸膏,加入挥发油,混匀,与熔融的聚乙二醇6000-聚乙二醇4000混合物混合均匀,由上至下,滴入液状石蜡中,将成型的滴丸沥尽并擦除液状石蜡,制成1000g,即得。
实施例2滴丸剂
鱼腥草1166g 黄芩300g 板蓝根300g
连翘116g 金银花116g
上述药材按如下方法制成1000g滴丸:
上述五味药材,鱼腥草、板蓝根、连翘、金银花四味合并,加12倍量水,蒸馏提取挥发油2小时,收集挥发油备用;过滤,收取滤液,药渣再加10倍量水煎煮2次,每次1小时,过滤,收集滤液,合并三次滤液,浓缩至相对密度约为1.15(60℃),加乙醇使含醇量达70%,放置过夜,过滤,滤液回收乙醇后并浓缩成流浸膏。黄芩加10倍量水煎煮3次,每次1小时,合并滤液,浓缩至体积为药材重量的10倍,用稀盐酸调pH1.8~2.0,70-80℃保温1小时,静置24小时,过滤,沉淀物加10倍药材量的水搅拌均匀,70-80℃保温1小时,静置24小时,过滤,沉淀物加4倍药材量的50%乙醇搅拌均匀,静置24小时,过滤,得黄芩提取物,加入流浸膏中,并加入挥发油,用胶体磨混匀,与熔融的聚乙二醇6000-聚乙二醇4000混合物混合均匀,由上至下,滴入液状石蜡中,将成型的滴丸沥尽并擦除液状石蜡,制1000g,即得。
对比例1滴丸剂
鱼腥草1166g 黄芩300g 板蓝根300g
连翘116g 金银花116g
上述药材按如下方法制成1000g滴丸:
上述五味药材,鱼腥草、连翘、金银花三味药材加12倍量水,蒸馏提取挥发油2小时,收集挥发油备用;过滤,滤液另器收集备用;药渣与板蓝根一起再加12倍量水煎煮2次,每次2小时,过滤,收集滤液,合并三次滤液,浓缩至相对密度约为1.15(60℃),加乙醇使含醇量达70%,放置过液,过滤,滤液回收乙醇并浓缩成清膏。黄芩加10倍量水煎煮2次,每次1小时,合并滤液,浓缩至体积为药材重量的10倍,用稀盐酸调pH1.8~2.0,70-80℃保温1小时,静置24小时,过滤,沉淀用乙醇洗、水洗至PH5~6,真空干燥,粉碎,得黄芩提取物粉,加入清膏中混匀浓缩成流浸膏,加入挥发油,混匀,与熔融的聚乙二醇6000-聚乙二醇4000混合物混合均匀,由上至下,滴入液状石蜡中,将成型的滴丸沥尽并擦除液状石蜡,制1000g,即得。
Claims (8)
1.用于制备复方鱼腥草滴丸的黄芩提取物的制备方法,所述复方鱼腥草滴丸由下列重量份药材制成:鱼腥草1000-1300份、黄芩250-350份、板蓝根250-350份、连翘100—150份、金银花100—150份,其特征在于该制备方法包括以下步骤:
(1)黄芩加水提取,得提取液;
(2)提取液浓缩至浓缩液体积L为药材重量kg的6-20倍;
(3)浓缩液用酸调节pH值至1.0~2.0,50℃-90℃保温,静置,过滤,得沉淀物Ⅰ;
(4)沉淀物Ⅰ加水搅匀,50℃-90℃保温,静置,过滤,循环操作1-2次,得沉淀物Ⅱ;
(5)沉淀物Ⅱ加30%-70%的乙醇溶液搅匀,静置,过滤,循环操作1-2次,得沉淀物或再经干燥、粉碎,即为黄芩提取物。
2.根据权利要求1所述的制备方法,其特征在于该制备方法包括以下步骤:
(1)黄芩加8-12倍量水提取2-3次,得提取液;
(2)提取液浓缩至浓缩液体积L为药材重量kg的8-12倍;
(3)浓缩液用酸调节pH值至1.5~2.0,70℃-80℃保温,静置,过滤,得沉淀物Ⅰ;
(4)沉淀物Ⅰ加水搅匀,70℃-80℃保温,静置,过滤,循环操作1-2次,循环操作1-2次,得沉淀物Ⅱ;
(5)沉淀物Ⅱ加30%-70%的乙醇溶液搅匀,静置,过滤,循环操作1-2次,得沉淀物或再经干燥、粉碎,即为黄芩提取物。
3.根据权利要求1或2所述的制备方法,其特征在于所述复方鱼腥草滴丸的制备方法如下:
(1)鱼腥草、板蓝根、连翘、金银花混合或单独提取挥发油;
(2)步骤(1)提取挥发油后的药渣加水提取,提取液过滤,滤液浓缩至在60℃时相对密度为1.10~1.30,加乙醇使含醇量达到60%—85%,静置,过滤,滤液回收乙醇并浓缩成流浸膏,备用;
(3)将黄芩提取物加入到上述流浸膏中,加入挥发油,混匀,制成滴丸,即得。
4.根据权利要求3所述的制备方法,其特征在于:步骤(1)提取挥发油的方法为水蒸汽蒸馏。
5.根据权利要求3所述的制备方法,其特征在于:步骤(3)制滴丸所用基质选自脂溶性基质和水溶性基质中的一种或几种,其中脂溶性基质选自:硬脂酸、单硬脂酸甘油酯、虫蜡、蜂蜡、石蜡、氢化植物油、半合成脂肪酸酯;水溶性基质选自聚乙二醇、聚氧乙烯单硬脂酸脂、泊洛沙姆、硬脂酸钠、甘油明胶;木糖醇与淀粉复合物,赤藓糖醇。
6.根据权利要求5所述的制备方法,其特征在于步骤(3)制滴丸药物成分与基质的重量比为1∶1-6。
7.根据权利要求6所述的制备方法,其特征在于步骤(4)制滴丸药物成分与基质重量比为1∶3。
8.根据权利要求7所述的制备方法,其特征在于所述基质为重量比为3∶1 的聚乙二醇6000和聚乙二醇4000混合物。
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CN103494928A (zh) * | 2013-09-29 | 2014-01-08 | 江西天施康中药股份有限公司 | 一种复方鱼腥草制剂的制备方法 |
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