CN115487225B - 一种槐米提取物的制备方法 - Google Patents
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Abstract
本发明涉及一种槐米提取物的制备方法,包括以下步骤:取槐米药材,加入沸水中后,用石灰乳调节PH,煎煮,滤过,合并滤液,用盐酸调节pH,静置,过滤,干燥,粉碎成细粉,即得。本发明通过改变槐米提取工艺提高芦丁转移率,提高芦丁含量稳定性。
Description
技术领域
本发明属于医药技术领域,涉及一种槐米提取物及其制备方法。
技术背景
槐米含芸香甙--芦丁、三萜皂甙、白桦脂醇、槐花二醇花瓣、葡萄糖、葡萄糖酸醛。槐花蕾中还含有槐花米甲素槐花米乙素和槐花米丙素甲素是和芸香苷(旧时称甙、现多称苷)不同的黄酮类化合物,乙素和丙素为甾醇类化合物。具有凉血止血,清肝泻火。用于便血、痔血、血痢、崩漏、吐血、衄血、肝热目赤、头痛眩晕。其产品心脉通胶囊在临床上已广泛应用于治疗心脑血管系统疾病,具有活血化瘀,通脉养心,降压降脂的功效,用于高血压、高脂血症等病症,产品临床疗效显著,质量稳定,安全性好。多年来,凭着安全可靠的疗效,为中医领域治疗心脑血管系统疾病的首选药物。
现有的槐米的提取方法为:槐米加入沸水中后,用石灰乳调节PH至8.5,再煎煮二次,滤过,合并滤液,用盐酸调节PH至4.0~5.0,静置24小时,滤取沉淀,干燥,粉碎成细粉,即得。
现有方法制备得到的芦丁转移率低,单位含量低,干燥困难等问题,使本品在有效期内极易不合格,导致产品芦丁含量不合格,从而影响疗效。
为了解决上述问题,提高药品的质量,发明人经过大量的实验,优选得到一种新的槐米提取物的制备方法。
发明内容
本发明的目的在于提供一种新的槐米提取物的制备方法。本发明通过改变槐米提取工艺提高芦丁转移率,提高芦丁含量稳定性。
本发明将槐米100-2000重量份,采用碱提酸沉法,针对加水量、煎煮时间、煎煮次数、pH值进行工艺研究,按上述参数进行工艺筛选,确定最佳提取工艺。本发明还对滤取方式,干燥方式、辅料加入量等参数进行筛选,确定最佳干燥工艺。
本发明的目的是这样实现的:通过对处方的工艺不断优化,将处方中的药材进行提取,采用碱提酸沉法,通过优化提取参数,使提取更充分。再用适当的滤取方式,干燥方式、辅料加入量,得到适当的提取物。
为此,本发明提供一种槐米提取物的制备方法,步骤如下:
将槐米加入10-30倍沸水中后,用石灰乳调节pH至8.0-9.0,再煎煮1-3次,每次1-4.5小时,滤过,合并滤液,用盐酸调节pH至4.0~5.0,静置温度1-15℃,静置24-72小时,用不同方式滤取沉淀,在湿的沉淀物中加的二氧化硅或淀粉,干燥,粉碎成细粉,即得。
其中,用不同方式滤取沉淀是指,用滤布滤取、离心滤取或组合式滤取技术滤取沉淀。
其中,滤布滤取为采用300-500目的滤布过滤;离心滤取为采用三足离心机过滤;组合式滤取为采用三足离心机+板框过滤机+管式离心机进行多级过滤。
其中,10-30倍沸水的单位为体积/重量比,例如:1g槐米加入10-30ml沸水中。
其中,在湿的槐米提取物沉淀中加1%-5%的二氧化硅或淀粉,例如在100克湿的槐米提取物沉淀中加1-5克的二氧化硅或淀粉。
其中,静置温度1-15℃,优选为静置温度1-15℃。
其中,干燥方式为热风循环烘箱干燥、真空减压干燥机干燥、冷冻干燥机干燥。
最优选的,本发明所述的槐米提取物的制备方法,步骤如下:
将槐米加入20倍沸水中后,用石灰乳调节pH至8.0,再煎煮三次,每次3小时,滤过,合并滤液,用盐酸调节pH至4.0,静置温度1-5℃,静置24小时,用组合式滤取技术滤取沉淀,在湿的槐米提取物沉淀中加3%-5%的二氧化硅,干燥,粉碎成细粉,即得。
其中,组合式滤取为采用三足离心机+板框过滤机+管式离心机进行多级过滤。
本发明的制备方法,是经过筛选获得的,筛选过程如下:
步骤1:槐米100-2000重量份,采用碱提酸沉法得滤液。根据检测结果(参照国家药品标准YBZ01122005-2009Z的检测方法,进行实验筛选。见表1
步骤1的提取进行工艺优化。以芦丁转移率为考察指标按4因素3水平进行正交实验,以含量转移率为参考指标,进行工艺优化,实验结果及方差分析见表2、表3.
表1影响槐米提取物提取的4因素3水平表
表2关于提取因素筛选的正交实验表
表3影响含量提取转移率的因素的方差分析
(F临界值大于19,有显著性)
由上表可以看出:加水量是最显著的因素,其次是煎煮次数。结合能耗最优的要求,因此采用加水量20倍,煎煮次数3次,煎煮时间3小时,PH(石灰乳调)8.0为最佳提取工艺。
为了提高槐米提取物的单位含量,降低含量降解率,根据实验参数,优化相应的参数。
其优选过程如下:
步骤2:将按最优工艺制得的滤液,将所得滤液按以下实验方案进行实验,最终得槐米提取物干品。根据检测结果(参照国家药品标准YBZ01122005-2009Z的检测方法,进行实验筛选。见表4
步骤2的纯化工艺优化。以芦丁转移率为考察指标按4因素3水平进行正交实验,以含量转移率为参考指标,进行工艺优化,实验结果及方差分析见表5、表6.表4影响纯化工艺的4因素3水平表
备注:滤布滤取为采用300-500目的滤布过滤;离心滤取为采用三足离心机过滤;组合式滤取为采用三足离心机+板框过滤机+管式离心机进行多级过滤。
表5关于提取因素筛选的正交实验表
表6影响含量提取转移率的因素的方差分析
(F临界值大于19,有显著性)
由上表可以看出:静置温度是最显著的因素,其次是滤取方式和PH(盐酸调)。结合能耗最优的要求,因此采用静置温度1-5℃,滤取方式为组合式滤取,PH(盐酸调)4.0,静置时间24小时,为最佳纯化工艺。
综上:最佳提取纯化工艺:槐米加入20倍沸水中后,用石灰乳调节PH至8.0,再煎煮三次,滤过,合并滤液,用盐酸调节PH至4.0,静置24小时,用组合式滤取技术滤取沉淀。
在实验研究过程中,我们还发现槐米提取物沉淀在干燥过程中,存在“炸粒”现象,即将湿的槐米提取物采用常温干燥或减压干燥时,物料会不时的产生不规则的小泡,且这些小泡会不时的破裂,导致干燥容器内壁会残留大量的槐米残渣,影响产品总得率,并且导致设备清洁困难,影响设备运行,无法连续生产。
因此,为了解决“炸粒”现象,根据实验情况,优化相应的参数。
其优选过程如下表:
表7
从上述数据中可以看出,在湿的槐米提取物沉淀中加3%-5%二氧化硅,有利于干燥的进行,且解决了干燥过程中的“炸粒”现象,避免的物料损失,提高了物料总得率(7%左右),降低了员工的劳动强度,提高了设备的使用效率。
综上:槐米提取物的最佳工艺:槐米加入20倍沸水中后,用石灰乳调节PH至8.0,再煎煮三次,每次3小时,滤过,合并滤液,用盐酸调节pH至4.0,静置24小时,用组合式滤取技术滤取沉淀,在湿的槐米提取物沉淀中加3%-5%的二氧化硅,干燥,粉碎成细粉,即得。
选取最佳工艺制备的槐米提取物,按照以下方法制备成心脉通胶囊成品。
进行加速稳定性考察,考察条件为:温度40℃±2℃、相对湿度75%±5%的条件下放置6个月。在试验期间第0个月,第1个月,第2个月,第3个月,第6个月分别取样一次,进行检测。如表8
表8方案的加速稳定性数据
现有工艺是指:将槐米加入5倍量沸水中后,用石灰乳调节PH至8.5,再煎煮二次,滤过,合并滤液,用盐酸调节PH至4.5,室温静置24小时,用300目滤布滤取沉淀,减压干燥,粉碎成细粉,即得。
从上述所有数据分析得出:采用最佳工艺制备的样品比标准工艺的芦丁的稳定性好,所得产品抗引湿能力强、稳定性强,疗效稳定;整体工艺易于操作,适于推广应用。
为更好的体现本发明的先进性,本发明采用对比研究的形式,与其它槐米提取物样品进行对比研究。见表9。
表9对比实验情况
从上述所有数据分析得出:采用最佳工艺制备的样品比其它方法所得的样品,单位含量要高,样品稳定性好,所得产品抗引湿能力强、稳定性强,疗效稳定;整体工艺易于操作,适于推广应用。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1:一种槐米提取物的制备方法
槐米320份,加入20倍沸水中后,用石灰乳调节PH至8.0,再煎煮三次,每次3小时,滤过,合并滤液,用盐酸调节pH至4.0,在2℃环境下静置24小时,用组合式滤取技术滤取沉淀。在湿的槐米提取物沉淀中加3%的二氧化硅,搅匀,用热风循环烘箱干燥,粉碎成80目细粉,即得。
实施例2:一种槐米提取物的制备方法
槐米520份,加入20倍沸水中后,用石灰乳调节PH至8.0,再煎煮三次,每次3小时滤过,合并滤液,用盐酸调节pH至4.0,在2℃环境下静置24小时,用组合式滤取技术滤取沉淀。在湿的槐米提取物沉淀中加4%的二氧化硅,搅匀,用真空减压干燥机干燥,粉碎成100目细粉,即得。
实施例3:一种槐米提取物的制备方法
槐米1500份,加入20倍沸水中后,用石灰乳调节pH至8.5,再煎煮2次,每次1.5小时滤过,合并滤液,用盐酸调节PH至4.5,在5℃环境下静置24小时,用三足离心机过滤滤取沉淀。在湿的槐米提取物沉淀中加5%的二氧化硅,搅匀,用真空减压干燥机干燥,粉碎成60目细粉,即得。
实施例4:一种槐米提取物的制备方法
槐米1100份,加入20倍沸水中后,用石灰乳调节PH至9.0,再煎煮2次,每次4.5小时滤过,合并滤液,用盐酸调节pH至5.0,在4℃环境下静置48小时,用滤布过滤滤取沉淀。用冷冻干燥机干燥,粉碎成120目细粉,即得。
实施例5:一种槐米提取物的制备方法
槐米1800份,加入30倍沸水中后,用石灰乳调节PH至8.5,再煎煮1次,每次4.5小时滤过,合并滤液,用盐酸调节pH至4.5,在12℃环境下静置72小时,用三足离心机过滤滤取沉淀。在湿的槐米提取物沉淀中加3%的淀粉,搅匀,用热风循环烘箱干燥,粉碎成80目细粉,即得。
Claims (1)
1.一种槐米提取物的制备方法,其特征在于,包括以下步骤:
将槐米加入20倍沸水中后,用石灰乳调节pH至8.0,再煎煮三次,每次3小时,滤过,合并滤液,用盐酸调节pH至4.0,静置温度1-5℃,静置24小时,用组合式滤取技术滤取沉淀,在湿的槐米提取物沉淀中加3%-5%的二氧化硅,干燥,粉碎成细粉,即得。
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