CN106975051A - 解郁安神颗粒制备方法 - Google Patents
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Abstract
本发明涉及一种中药的制备方法,即解郁安神颗粒制备方法。配方中原料预处理、提取前浸泡、装塑料袋、加压破壁处理:将原料塑料袋放入超高压加压舱中,启动设备,关闭加压舱门,设定加压压力数值为50‑600Mpa,保持压力时间值为3‑10分钟。卸压:达到设定的保压时间后,在3秒钟时间内,快速卸掉压力,使压力为0Mpa。超高压处理后再浸泡:从超高压处理舱内取出塑料袋,将已经破壁的原料倒入不锈钢桶或浸泡箱中,料液比1:10‑1:30,加水浸泡6‑8小时,得浸泡液,按工艺制成颗粒;经试验,本发明降低成本,提高收率,平均收率19.5%,从而提高了疗效。
Description
技术领域
本发明涉及一种中药的制备方法,即解郁安神颗粒制备方法。
背景技术
在现有技术中,由于生活节奏的急剧加快及压力骤升,失眠现象已经越来越常见。失眠又称入睡和维持睡眠障碍(DlMS),是指无法入睡或无法保持睡眠状态,导致睡眠不足。解郁安神颗粒(国药准字Z20093537),具有舒肝解郁,安神定志的作用,可用于情志不舒,肝郁气滞等精神刺激所致的疾病。处方:柴胡80g、大枣60g、石菖蒲80g、姜半夏60g、炒白术60g、浮小麦200g、制远志80g、炙甘草60g、炒栀子80g、百合200g、胆南星80g、郁金80g、龙齿200g、炒酸枣仁100g、茯苓100g、当归60g。制法:以上16味药将处方中十六味药材投入多功能提取罐中,加水煎煮三次,第一次加入药材重量6倍量的饮用水,浸泡2小时,煎煮3小时(沸腾后开始计时),将药液经过滤器打入与提取罐相连的贮罐中;第二次加入药材重量5倍量的饮用水,煎煮2小时,第三次加入药材重5倍量的饮用水,煎煮2小时,煎煮液过滤,滤液合并,滤液用单效、双效外循环节能蒸发器浓缩,控制一效真空度-0.05~-0.06MPa,温度70℃~80℃;控制二效真空度-0.07~-0.08MPa,温度60℃~70℃。浓缩至相对密度1.35~1.40(50℃)的稠膏,加入蔗糖粉适量,制成颗粒,干燥即得,可用于情志不舒,肝郁气滞等精神刺激所致的疾病。但是该药成方时间早,工艺不尽合理,严重浪费能源,对环境造成污染,如何进一步减少能源浪费,高效环保是面临的新问题。
发明内容
本发明的目的是针对上述不足而提供一种优选工艺,降低成本,提高疗效的解郁安神颗粒制备方法。
本发明的技术解决方案是:解郁安神颗粒制备方法,其特征在于步骤如下:
(1)原料:柴胡80份、大枣60份、石菖蒲80份、姜半夏60份、炒白术60份、浮小麦200份、制远志80份、炙甘草60份、炒栀子80份、百合200份、胆南星80份、郁金80份、龙齿200份、炒酸枣仁100份、茯苓100份、当归60份。
(2)原料预处理:用粉碎机将原料粉碎成粉状,过0.38mm×0.38mm孔径筛子备用。
(3)提取前浸泡:将粉状原材料装入容器中,加入水浸泡,料液比为1:1-1:3,充分搅拌,浸泡4-8小时,使原料细胞充分吸水膨胀。
(4)装塑料袋:将经过充分浸泡膨胀的原料装入塑料袋中,排除塑料袋中的空气,封严塑料袋口。
(5)加压破壁处理:将原料塑料袋放入超高压加压舱中,启动设备,关闭加压舱门,设定加压压力数值为50-600Mpa,保持压力时间值为3-10分钟。
(6)卸压:达到设定的保压时间后,在3秒钟时间内,快速卸掉压力,使压力为0Mpa。
(7)超高压处理后再浸泡:从超高压处理舱内取出塑料袋,将已经破壁的原料倒入不锈钢桶或浸泡箱中,料液比1:10-1:30,加水浸泡6-8小时,得浸泡液;
(8)过滤浸泡液,滤液合并,滤液用单效、双效外循环节能蒸发器浓缩,控制一效真空度-0.05~-0.06MPa,温度70℃~80℃;控制二效真空度-0.07~-0.08MPa,温度60℃~70℃;浓缩至相对密度1.35~1.40的稠膏(50℃);将稠膏装入洁净的干燥盘中,用真空干燥箱干燥,干燥温度50-60℃,真空度-0.04~-0.05MPa,干燥时间48小时;将干浸膏取出,装入洁净容器中,称重,将干浸膏用吸尘粉碎机粉碎,粉碎机筛网100目,粉碎后药粉装入洁净容器中,将批量称取的蔗糖粉、浸膏粉分5次倒入湿法制粒机内,先干混5分钟后,加入药粉重量20%的70%乙醇,湿混5分钟,将制好的软材加入颗粒机料斗内,筛网目数10目、65目,每次填料量不超过料斗容积的1/2;将制好的湿颗粒装于洁净的不锈钢盘中;开启热风循环蒸汽烘箱,设置温度为70~80℃,时间50分钟,取出干燥的颗粒;用振动筛分机进行整粒,振动筛筛网10目、65目;按批量,将颗粒加入到二维运动混合机中,开机混合60分钟后,将批混后颗粒装入容器中备用。
本发明的优点是:1、提取时间短:超高压提取的升压和保压阶段,超高的压力差使提取溶剂迅速渗透到固体药物组织内部,有效成分快速溶解在提取溶剂中。卸压阶段,超高的反向压力差为溶解在提取溶剂中的有效成分由固体组织内部向外的扩散提供了超高的传质动力,有效成分能够快速扩散到固体组织外,因此超高压提取能显著地缩短提取时间。以人参皂苷提取为例,超高压提取时间为5 min,而回流法、索氏提取法、超声法、超临界CO2萃取法、微波法提取时间依次为180、360、 40、180、15 min。在上述6种提取方法中超高压提取时间最短,微波提取时间与超高压提取时间最接近,但存在微波不均匀、工业化难等不足。2、溶剂消耗少:超高压提取是在一个完全封闭的条件下进行的,没有溶剂的挥发消耗,而且目标成分由固体组织向周围溶剂的扩散,不是单纯的靠浓度梯度提供传质动力,而是主要靠由压力差提供,因此超高压提取选择的固体原料与提取溶剂的比例较其他方法都要小,能明显地降低溶剂的消耗。3、提取效率高:超高压提取压力最高可达700 MPa,在这样高的压力下,可以显著地提高提取效率。以人参总皂苷的提取为例,回流、超声、超临界CO2萃取、超高压的提取得率分别是5.75%、5.89%、2.32%、7.33%。4、节能:高压提取在保压、卸压阶段,能量的转化和热量的对外交换相对来讲很小,因此这两个段消耗能量也很小;在升压阶段消耗的能量主要体现在抵抗流体形变的应力上(液体内部质点摩擦产生小部分热量,引起较小温升,消耗小部分能量),对流体的机械做功更体现在流体的压缩能量上。以溶剂水为例,从理论上分析,100 L水加热到90℃需要热量293×105 J,100 L水加压到400MPa耗能仅为18.84× 105J,在回流提取过程中,溶剂还需要不断地吸收能量,使提取溶剂维持在沸腾状态,大量能量消耗于液体的汽化,而且由电能转化为热能的效率要远低于转化为压缩能,因此高压提取消耗的能量相对较低,仅占热回流提取的1/15左右,实际运行时扣除各种因素的影响,至少节能80%以上。5、提取温度低:在绝热条件下,压力每提高100MPa,水的温度升高3℃左右。实际提取时,由于高压容器壁与周围环境有热交换,温度升高的程度远小于上述数值。因此可以说高压提取可以维持在接近常温的条件下进行。这对于天然产物中的热敏性成分、易挥发性成分的提取是极为有利的;同时由于高压提取使用的是流体静压力,压力传递是在瞬间完成的,容器内任何方向和位置的压力相等,因此超高压提取对物料的作用是均匀一致的,这就避免了像微波提取、热回流提取过程中的局部受热不均,造成目标成分的结构变化和损失从而保证了有效成分具有更高的生物活性。6、由于超高压提取技术破坏了植物的细胞壁、细胞膜,使细胞内的有效成分会充分的释放到提取介质中。提取能耗低、时间短、速度快。一般情况下,使用超高压设备出来一次提取物,只需要7-8分钟即可完成一次提取过程,能耗低,时间非常短,降低了提取成本。7、经试验,本发明可以提高收率,平均收率19.5%(现有技术15.33%),从而提高了疗效。
下面将结合实施例对本发明的实施方式作进一步详细描述。
具体实施方式
实施例1
解郁安神颗粒制备方法,其特征在于步骤如下:
配方:柴胡80份、大枣60份、石菖蒲80份、姜半夏60份、炒白术60份、浮小麦200份、制远志80份、炙甘草60份、炒栀子80份、百合200份、胆南星80份、郁金80份、龙齿200份、炒酸枣仁100份、茯苓100份、当归60份。
步骤组成:
原料预处理:植物原料需做预处理,即用粉碎机将植物原料粉碎成粉状,过0.38mm×0.38mm孔径筛子备用。
提取前浸泡:将粉状植物原材料装入容器中,加入水浸泡,料液比为1:1-1:3,充分搅拌,浸泡4-8小时,使植物细胞充分吸水膨胀。
装塑料袋:将经过充分浸泡膨胀的原料装入塑料袋中,排除塑料袋中的空气,封严塑料袋口。塑料袋的大小根据超高压设备的处理舱大小灵活决定。
加压破壁处理:将装好充分浸泡膨胀的原料的塑料袋放入超高压加压舱中,启动设备,关闭加压舱门,设定加压压力数值为50-600Mpa,保持压力时间值为3-10分钟。
卸压:达到设定的保压时间后,在3秒钟时间内,快速卸掉压力,使压力为0Mpa。
超高压处理后再浸泡:从超高压处理舱内取出塑料袋,将已经破壁的植物原料倒入不锈钢大桶或大型浸泡箱中,料液比1:10-1:30,并按所提取植物实际需要的料液比减去已加入到溶剂的比例份额(1:1-1:3)加入水在浸泡,浸泡6-8小时即可。也可以将上述再浸泡工艺过程加入到溶剂分成若干等份,每次加入一份,浸泡1-1.5小时滤出溶液,在加入另一份溶剂浸泡,直至加入完全部溶剂。浸泡过程中每隔20分钟需要充分搅动一次。
实施例2
解郁安神颗粒
配方:柴胡80份、大枣60份、石菖蒲80份、姜半夏60份、炒白术60份、浮小麦200份、制远志80份、炙甘草60份、炒栀子80份、百合200份、胆南星80份、郁金80份、龙齿200份、炒酸枣仁100份、茯苓100份、当归60份。
首先原料预处理,提取前浸泡,装塑料袋(或瓶)加压破壁出来卸压,超高压处理后再浸泡。预处理即用粉碎机将植物原材料粉碎成粉状,过筛。装入容器中,加入水(或酒精)浸泡,充分浸泡膨胀的植物原料装入塑料袋(或瓶)中,排除空气,封严。塑料袋放入超高压加压舱中,加压为50-600Mpa,时间为3-10分钟后,快速卸掉压力。将已经破壁的植物原料倒入容器中,料液比加大至1:10-1:30,并按所提取植物实际需要的料液比减去加入的溶剂的比例份额1:1-1:3加入水(或酒精)在浸泡6-8小时。将经过浸泡过的浸泡液过滤,滤液合并,滤液用单效、双效外循环节能蒸发器浓缩,控制一效真空度-0.05~-0.06MPa,温度70℃~80℃;控制二效真空度-0.07~-0.08MPa,温度60℃~70℃。浓缩至相对密度1.35~1.40(50℃)的稠膏。将稠膏装入洁净的干燥盘中,用真空干燥箱干燥,干燥温度50-60℃,真空度-0.04~-0.05MPa,干燥时间48小时。将干浸膏取出,装入洁净容器中,称重,将干浸膏用吸尘粉碎机粉碎,粉碎机筛网100目,粉碎后药粉装入洁净容器中,将批量称取的蔗糖粉、浸膏粉分5次倒入湿法制粒机内,先干混5分钟后,加入药粉重量20%的70%乙醇,湿混5分钟,将制好的软材加入颗粒机料斗内,筛网目数10目、65目,每次填料量不超过料斗容积的1/2。将制好的湿颗粒装于洁净的不锈钢盘中。开启热风循环蒸汽烘箱,设置温度为70~80℃,时间50分钟,取出干燥的颗粒。用振动筛分机进行整粒,振动筛筛网10目、65目。按批量,将颗粒加入到二维运动混合机中,开机混合60分钟后,将批混后颗粒装入容器中备用。
实验例1
提取物手率对比表
多功能提取 | 超高压提取 | |
第一次 | 15.2% | 18.9% |
第二次 | 15.5% | 20.2% |
第三次 | 15.3% | 19.4% |
平均收率 | 15.33% | 19.5% |
从列表中可知,本发明可以提高收率,平均收率19.5%(现有技术15.33%),从而提高了疗效。
上面描述,只是本发明的具体实施方式,各种举例说明不对本发明的实质内容构成限制。
Claims (1)
1.解郁安神颗粒制备方法,其特征在于步骤如下:
(1)原料:柴胡80份、大枣60份、石菖蒲80份、姜半夏60份、炒白术60份、浮小麦200份、制远志80份、炙甘草60份、炒栀子80份、百合200份、胆南星80份、郁金80份、龙齿200份、炒酸枣仁100份、茯苓100份、当归60份;
(2)原料预处理:用粉碎机将原料粉碎成粉状,过0.38mm×0.38mm孔径筛子备用;
(3)提取前浸泡:将粉状原材料装入容器中,加入水浸泡,料液比为1:1-1:3,充分搅拌,浸泡4-8小时,使原料细胞充分吸水膨胀;
(4)装塑料袋:将经过充分浸泡膨胀的原料装入塑料袋中,排除塑料袋中的空气,封严塑料袋口;
(5)加压破壁处理:将原料塑料袋放入加压舱中,启动设备,关闭加压舱门,设定加压压力数值为50-600Mpa,保持压力时间值为3-10分钟;
(6)卸压:达到设定的保压时间后,在3秒钟时间内,快速卸掉压力,使压力为0Mpa;
(7)超高压处理后再浸泡:从超高压处理舱内取出塑料袋,将已经破壁的原料倒入不锈钢桶或浸泡箱中,料液比1:10-1:30,加水浸泡6-8小时,得浸泡液;
(8)过滤浸泡液,滤液合并,滤液用单效、双效外循环节能蒸发器浓缩,控制一效真空度-0.05~-0.06MPa,温度70℃~80℃;控制二效真空度-0.07~-0.08MPa,温度60℃~70℃;50℃浓缩至相对密度1.35~1.40的稠膏;将稠膏装入洁净的干燥盘中,用真空干燥箱干燥,干燥温度50-60℃,真空度-0.04~-0.05MPa,干燥时间48小时;将干浸膏取出,装入洁净容器中,称重,将干浸膏用吸尘粉碎机粉碎,粉碎机筛网100目,粉碎后药粉装入洁净容器中,将批量称取的蔗糖粉、浸膏粉分5次倒入湿法制粒机内,先干混5分钟后,加入药粉重量20%的70%乙醇,湿混5分钟,将制好的软材加入颗粒机料斗内,筛网目数10目、65目,每次填料量不超过料斗容积的1/2;将制好的湿颗粒装于洁净的不锈钢盘中;开启热风循环蒸汽烘箱,设置温度为70~80℃,时间50分钟,取出干燥的颗粒;用振动筛分机进行整粒,振动筛筛网10目、65目;按批量,将颗粒加入到二维运动混合机中,开机混合60分钟后,将批混后颗粒装入容器中备用。
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