CN114073751A - 一种桂枝芍药知母汤的喷雾干燥工艺 - Google Patents
一种桂枝芍药知母汤的喷雾干燥工艺 Download PDFInfo
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Abstract
本发明公开了一种桂枝芍药知母汤的喷雾干燥工艺。所述工艺包括以下步骤:(1)取桂枝芍药知母汤的原料药桂枝、白芍、知母、防风、白术、麻黄、甘草、生姜、附子,加水提取,过滤,得提取液;(2)在提取液中加入辅料,进行喷雾干燥;所述辅料为β‑环糊精和乳糖的混合物,其中,β‑环糊精和乳糖的重量比为1:(1~9)。实验结果表明,通过添加上述特定比例的特定辅料,在本发明特定的工艺参数下对桂枝芍药知母汤浓缩液进行喷雾干燥,所得粉末的不仅含水量低,而且得粉率高,取得了意料不到的技术效果。采用本发明的喷雾干燥工艺,能够制得高产率、低含水量的桂枝芍药知母汤粉末试剂,应用前景广阔。
Description
技术领域
本发明属于制剂加工领域,具体涉及一种桂枝芍药知母汤的喷雾干燥工艺。
背景技术
类风湿性关节炎(RA)是一种以关节滑膜炎症为特征的慢性全身性自身免疫性疾病。滑膜炎反复发作,导致关节内软骨和软骨下骨组织的破坏,关节功能障碍,最终造成关节畸形和强直。
桂枝芍药知母汤出自《金匮要略·中风历节病脉证治》篇,由桂枝四两、白芍三两、甘草二两、麻黄二两、生姜五两、白术五两、知母四两、防风四两、附子二量提取制得,具有祛风除湿、温经散寒、滋阴清热之功效,主治风湿历节,是临床治疗类风湿性关节炎的常用方。
但是,桂枝芍药知母汤是汤剂,其存在不易携带,不易储存、质量不稳定等缺点。如果将桂枝芍药知母汤加工成粉末试剂,将有利于药物的携带、储存,以及提高药物的稳定性。
目前,将汤剂加工成粉末制剂的方法主要有冷冻干燥法、传统热风干燥法以及喷雾干燥法。其中,冷冻干燥法制得的产物虽然品质较好,但是过程耗时较长、能耗大、效率低、成本高,不适合量大的工业化生产,并且冻干后的产品极易吸潮,不便于长期保存;传统热风干燥法得到的产品颗粒较大,且品质不佳。由于上述缺点,极大的限制了冷冻干燥法、传统热风干燥法的应用。
喷雾干燥法不仅能够得到颗粒小、均匀的粉末,而且过程耗时短、能耗小、成本低,适合量大的工业化生产。但是,现有的喷雾干燥法在制粉时,粉末含水量高,粘壁现象严重,极大的降低了得粉率,极大地限制了其使用。
因此,研究出一种产品含水量低、得粉率高的桂枝芍药知母汤的喷雾干燥工艺具有非常重要的意义。
发明内容
本发明的目的在于提供一种桂枝芍药知母汤的喷雾干燥工艺。
本发明提供了一种桂枝芍药知母汤的喷雾干燥工艺,所述工艺包括以下步骤:
(1)取桂枝芍药知母汤的原料药桂枝、白芍、知母、防风、白术、麻黄、甘草、生姜、附子,加水提取,过滤,得提取液;
(2)在提取液中加入辅料,进行喷雾干燥;所述辅料为β-环糊精和乳糖的混合物,其中,β-环糊精和乳糖的重量比为1:(1~9)。
进一步地,步骤(2)中,所述β-环糊精和乳糖的重量比为1:5。
进一步地,步骤(2)中,所述辅料的加入量为干浸膏重量的10%~30%,优选为25%;其中,干浸膏为提取液干燥后所得产物。
进一步地,步骤(2)中,所述提取液为浓缩后所得的浓缩液,所述浓缩液的密度为1.05~1.20g/mL,优选为1.05~1.08g/mL。
进一步地,步骤(2)中,所述喷雾干燥的进风温度为160.00~200.00℃,优选为173.60~191.55℃,更优选为180.00~182.50℃。
进一步地,步骤(2)中,所述喷雾干燥的进样速率为15.0~30.0r/min,优选为17.0~22.5r/min。
进一步地,步骤(2)中,所述喷雾干燥的出风温度为80~85℃;风机频率为80~100Hz,通针时间为8~12s。
进一步地,步骤(1)中,所述桂枝、白芍、知母、防风、白术、麻黄、甘草、生姜、附子的重量份数之比为:桂枝12份、白芍9份、知母12份、防风12份、白术15份、麻黄6份、甘草6份、生姜15份、附子6份;所述附子为炮附片。
进一步地,步骤(1)中,所述水的重量为桂枝、白芍、知母、防风、白术、麻黄、甘草、生姜、附子总重量的10~20倍,优选为16倍。
进一步地,步骤(1)中,所述提取次数为1~5次,优选为3次;所述提取时间为每次0.5~2.0小时,优选为1小时。
“固含量”是液体烘干后剩余部分占液体总量的质量百分数。
“干浸膏”是指用适宜的溶媒浸出药材的有效成分后,将浸出液蒸去全部溶媒后所得的稠膏状、块状或粉状的体系。
本发明中,“X%干浸膏量”是指物质重量为浓缩液干燥后所得浸膏重量的X%。比如,“25%干浸膏量”的辅料是指辅料重量为浓缩液干燥后所得浸膏重量的25%。
实验结果表明,通过添加本发明特定比例(25%干浸膏量)的特定辅料(β-环糊精和乳糖重量比为1:5组成的混合物),在本发明特定的工艺参数下(进风温度为160~200℃,进样速率为15~30r/min,料液密度为1.05~1.20g/mL)对桂枝芍药知母汤浓缩液进行喷雾干燥,所得粉末的不仅含水量低,而且得粉率高。
特别的,当控制进风温度为173.6~191.55℃,进样速率为17~22.5r/min,料液密度为1.05~1.08g/mL时,喷雾干燥所得粉末的含水量低至3.55%以下,得粉率高达68.03%~71.58%。更特别的,当控制进风温度为180~182.5℃,进样速率为17~22.5r/min,料液密度为1.05~1.08g/mL时,喷雾干燥所得粉末的含水量低至3.04%以下,得粉率高达68.15%~71.58%。
采用本发明的喷雾干燥工艺,能够制得高产率、低含水量的桂枝芍药知母汤粉末试剂,应用前景广阔。
显然,根据本发明的上述内容,按照本领域的普通技术知识和惯用手段,在不脱离本发明上述基本技术思想前提下,还可以做出其它多种形式的修改、替换或变更。
以下通过实施例形式的具体实施方式,对本发明的上述内容再作进一步的详细说明。但不应将此理解为本发明上述主题的范围仅限于以下的实例。凡基于本发明上述内容所实现的技术均属于本发明的范围。
具体实施方式
本发明所用原料与设备均为已知产品,通过购买市售产品所得。
实施例1、辅料的筛选
按处方取桂枝12g、白芍9g、知母12g、防风12g、白术15g、麻黄6g、甘草6g、生姜15g、炮附片6g,加16倍量水,提取3次,每次1h,合并滤液,即得。
然后将所得滤液浓缩,得浓缩液。所得浓缩液在25℃下的密度为1.087g/mL。
(1)单一辅料种类的筛选
取上述浓缩液分别加入30%干浸膏量的单一辅料进行喷雾干燥(进风温度180℃,出风温度设定80~85℃,进样速率15r/min,风机设定90Hz,通针设定10s),喷雾干燥结果见表1。
30%干浸膏量是指加入的辅料重量为浓缩液干燥后所得浸膏重量的30%。
得粉率(M):M=m1/m。其中,m1为收集瓶得粉质量,m为浓缩液固含量。
表1单一辅料种类筛选结果
结果显示,无辅料加入时,得粉率很低,且易堵塞喷头;加入β-环糊精或乳糖后的得粉率较高。
(2)混合辅料种类的筛选
取上述浓缩液分别加入30%干浸膏量的混合辅料进行喷雾干燥(喷雾干燥条件与上述“(1)单一辅料的筛选”中相同,喷雾干燥结果见表2。
表2混合辅料种类筛选结果
结果显示,当β-环糊精和乳糖重量比为1:5时,将其作为混合辅料加入浓缩液进行喷雾干燥,得粉率最高。
(3)辅料加入量的筛选
取上述浓缩液分别加入表3所示重量的混合辅料(β-环糊精和乳糖重量比为1:5组成的混合物)进行喷雾干燥(喷雾干燥条件与上述“(1)单一辅料的筛选”中相同,喷雾干燥结果见表3。
表3辅料用量筛选
由以上结果可见,以加入混合辅料(β-环糊精和乳糖重量比为1:5组成的混合物)进行喷雾干燥时,当辅料的重量为干浸膏重量的10%~30%时,能够有效改善黏壁现象;当辅料的重量为干浸膏重量的25%时,喷雾干燥后的得粉率最高。
实施例2、喷雾干燥工艺的筛选
1、实验方法
按照实施例1的方法制得桂枝芍药知母汤,然后进行不同程度的浓缩,得不同密度的浓缩液(如表4所示)。
取上述浓缩液,加入25%干浸膏量的混合辅料(β-环糊精和乳糖重量比为1:5组成的混合物)进行喷雾干燥,喷雾干燥条件为:进风温度(如表4所示),出风温度设定80~85℃,进样速率(如表4所示),风机设定90Hz,通针设定10s。
2、数据处理
测试喷雾干燥后所得粉末的得粉率(M)和含水量:
(1)得粉率:M=m1/m。其中,m1为收集瓶得粉质量,m为浓缩液固含量。
(2)含水量=(供试品原重-供试品烘干后重量)/供试品原重×100%。
根据实验可知喷雾干燥后,附着在干燥塔上的喷干粉颜色偏深,有焦屑,均一性差,而收集瓶上的喷干粉细腻、均匀,故实验中只考察收集瓶的喷干粉。实验结果期望收集瓶的得粉率越高越好,并且喷干粉的水分量在一定范围内越低越好,因为含水量高,易结块,不利于存贮。工艺目标要求含水量不得超过5.0%。
3、实验结果
不同工艺下的喷雾干燥效果如表4所示。其中,A为进风温度,B为进样速率,D为浓缩液密度。
表4喷雾干燥工艺筛选实验设计与结果
可以看出,在本发明特定的辅料下(25%干浸膏量的混合辅料(β-环糊精和乳糖重量比为1:5组成的混合物))进行喷雾干燥,当控制进风温度为160~200℃,进样速率为15~30r/min,浓缩液密度为1.05~1.20g/mL时,喷雾干燥所得粉末的含水量都在5.0%以下,满足工艺目标要求;而且,在保持低含水量的同时还具有较高的得粉率。
进一步的,当控制进风温度为173.6~191.55℃,进样速率为17~22.5r/min,浓缩液密度为1.05~1.08g/mL时,喷雾干燥所得粉末的含水量低至3.55%以下,得粉率高达68.03%~71.58%。
更进一步的,当控制进风温度为180~182.5℃,进样速率为17~22.5r/min,浓缩液密度为1.05~1.08g/mL时,喷雾干燥所得粉末的含水量低至3.04%以下,得粉率高达68.15%~71.58%。
上述实验表明,以本发明特定的辅料(25%干浸膏量的混合辅料(β-环糊精和乳糖重量比为1:5组成的混合物))进行喷雾干燥,在本发明特定的喷雾干燥工艺下,能够使所得桂枝芍药知母汤粉末同时满足含水量低、得粉率高的要求。
综上,本发明提供了一种桂枝芍药知母汤的喷雾干燥工艺。实验结果表明,通过添加特定比例(25%干浸膏量)的特定辅料(β-环糊精和乳糖重量比为1:5组成的混合物),在本发明特定的工艺参数下对桂枝芍药知母汤浓缩液进行喷雾干燥,所得粉末的含水量低,得粉率高,取得了意料不到的技术效果。采用本发明的喷雾干燥工艺,能够制得高产率、低含水量的桂枝芍药知母汤粉末试剂,应用前景广阔。
Claims (10)
1.一种桂枝芍药知母汤的喷雾干燥工艺,其特征在于:所述工艺包括以下步骤:
(1)取桂枝芍药知母汤的原料药桂枝、白芍、知母、防风、白术、麻黄、甘草、生姜、附子,加水提取,过滤,得提取液;
(2)在提取液中加入辅料,进行喷雾干燥;所述辅料为β-环糊精和乳糖的混合物,其中,β-环糊精和乳糖的重量比为1:(1~9)。
2.根据权利要求1所述的工艺,其特征在于:步骤(2)中,所述β-环糊精和乳糖的重量比为1:5。
3.根据权利要求1或2所述的工艺,其特征在于:步骤(2)中,所述辅料的加入量为干浸膏重量的10%~30%,优选为25%;其中,干浸膏为提取液干燥后所得产物。
4.根据权利要求1~3任一项所述的工艺,其特征在于:步骤(2)中,所述提取液为浓缩后所得的浓缩液,所述浓缩液的密度为1.05~1.20g/mL,优选为1.05~1.08g/mL。
5.根据权利要求4所述的工艺,其特征在于:步骤(2)中,所述喷雾干燥的进风温度为160.00~200.00℃,优选为173.60~191.55℃,更优选为180.00~182.50℃。
6.根据权利要求5所述的工艺,其特征在于:步骤(2)中,所述喷雾干燥的进样速率为15.0~30.0r/min,优选为17.0~22.5r/min。
7.根据权利要求6所述的工艺,其特征在于:步骤(2)中,所述喷雾干燥的出风温度为80~85℃;风机频率为80~100Hz,通针时间为8~12s。
8.根据权利要求1~7任一项所述的工艺,其特征在于:步骤(1)中,所述桂枝、白芍、知母、防风、白术、麻黄、甘草、生姜、附子的重量份数之比为:桂枝12份、白芍9份、知母12份、防风12份、白术15份、麻黄6份、甘草6份、生姜15份、附子6份;所述附子为炮附片。
9.根据权利要求8所述的工艺,其特征在于:步骤(1)中,所述水的重量为桂枝、白芍、知母、防风、白术、麻黄、甘草、生姜、附子总重量的10~20倍,优选为16倍。
10.根据权利要求9所述的工艺,其特征在于:步骤(1)中,所述提取次数为1~5次,优选为3次;所述提取时间为每次0.5~2.0小时,优选为1小时。
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