CN108524863A - 一种蒙药复方协日嘎四味片的提取工艺 - Google Patents
一种蒙药复方协日嘎四味片的提取工艺 Download PDFInfo
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Abstract
本发明公开了一种蒙药复方协日嘎四味片的提取工艺，所述蒙药复方协日嘎四味片是由下述重量份的药材组成：姜黄100‑200、黄柏60‑120、栀子80‑160、蒺藜100‑200。根据处方中组成药物所含化学成分的性质，选定煎煮提取时的加水量，浸泡时间，煎煮时间，煎煮次数作为四个因素，同时为每个因素选取三个水平，以黄柏季胺类生物碱的煎出量及总煎出物为评价指标，采用正交试验进行设计，筛选出方中药物煎煮提取的最佳工艺条件。
Description
技术领域
本发明属于蒙药技术领域，特别涉及一种蒙药复方协日嘎四味片的提取工艺。
背景技术
协日嘎四味片是由姜黄、黄柏、栀子、蒺藜四味药材组成的蒙药复方制剂，具有利尿，泻湿热功能；主要用于小便闭止，尿频，尿急，尿中带血，膀胱刺痛。原方为煮散剂，收载于《中华人民共和国卫生部药品标准蒙药分册》(1998年版)。
蒙药煮散剂的应用，每次剂量为5.0g～7.5g，加水约200mL，煎煮至半干，滤取煎液口服，微苦，携带使用极不方便，故根据临床需要，为提高药效，稳定质量，方便患者，将其改为片剂。我们按照拟定的制备工艺路线，选定煎煮提取时的加水量，浸泡时间，煎煮时间，煎煮次数四个因素，为每个因素选取三个水平，以黄柏季胺类生物碱的煎出量及总煎出物为评价指标，采用L9(34)正交表进行试验设计，研究筛选了方中黄柏等药物的煎煮提取最佳工艺条件。如何将活性物质充分有效地提取，是复方协日嘎四味片制备的关键。
发明内容
本发明的内容是提供一种蒙药复方协日嘎四味片的提取工艺。
所述药物是由下述重量配比的蒙药材组成的：姜黄100-200、黄柏60-120、栀子80-160、蒺藜100-200。
其提取工艺如下：将姜黄、黄柏、栀子、蒺藜四味药材粉碎成粗粉，加入10倍量水，浸泡因素可忽略，煎煮提取3次，每次煮沸1小时，合并煎煮提取液，加热浓缩，浓缩至相对密度为1.05-1.10(40℃测)的清膏，将清膏喷雾干燥，加入适量药学意义上的辅料制成片剂。药材活性成分的提取是复方协日嘎四味片制备的关键，具体研究如下：
1试验设计 采用L9(34)正交表进行试验设计，见表1。
表1正交试验因素水平表
2供试品溶液的制备：根据表2正交试验设计要求，精密称取样品粗粉约33g，加A倍量水，浸泡D小时，煎煮C次，每次B小时，离心分离5min(3.5kr/min)，合并上清液于1000mL量瓶中加水至刻度，摇匀，即得。
3季胺类总生物碱的含量测定
3.1标准曲线的绘制 精密称取盐酸小檗碱对照品10～12mg，pH＝7～10的缓冲液使溶解，并稀释至100mL，准确吸取上述对照品溶液0mL、0.2mL、0.4mL、0.6mL、0.8mL、1.0mL分别置50mL比色管中，加pH＝7～10的缓冲液至1ml，再加0.007％的溴麝香草酚蓝溶液(pH＝7～10)9mL，摇匀，加入氯仿10mL，振摇2min后移入60mL分液漏斗中，静置分层。取氯仿层，以空白试剂氯仿萃取液为空白对照，在420nm波长处测定吸收度，并计算，得标准曲线工作方程为C＝170106A-0.177，r2＝0.9997。
3.2含量测定 精密吸取样品液1mL，置50mL比色管中，照上述标准曲线绘制项下的方法，依法进行配制并测定吸收度，计算含量。含量以盐酸小檗碱计，结果见表2。
4总煎出物的测定 精密吸取供试品溶液30mL，按照《中国药典》2010年版一部附录X A浸出物测定法测定，并计算，即得。结果见表2(n＝3)。
表2 正交试验设计与试验结果
注：水煎提取工艺正交试验的两个评价指标，采用综合评分进行数据分析。总生物碱和总煎出物的权重系数分别为0.8、0.2。总生物碱评分＝总生物碱量/最大总生物碱量×0.8×100(1)；总煎出物评分＝总煎出物量/最大总煎出物量×0.2×100(2)；综合得分＝(1)+(2)。
5方差分析
将正交试验评价指标综合得分进行方差分析，结果见表3。
表3 正交试验的方差分析
F1-0.10(2，2)＝9.00 F1-0.05(2，2)＝19.00 F1-0.01(2，2)＝99.00
协日嘎四味片的煎煮提取工艺参数评价指标，以黄柏季胺类总生物碱的煎出率高为佳，总煎出物则以适中为度。从表2的正交试验结果表中可以直观看出，7号样品方案A3B1C3D2为较佳组合，综合得分最高。表3方差分析结果表明，C因素对提取效果影响极显著(P＜0.01)，故须以提取3次(C3)为最好；A因素影响显著(P＜0.05)，故加水量应以药材的10倍量(A3)为佳；B因素影响不显著(P＞0.01)，故可以采用7号方案的B1水平，每次煮沸时间以1h为宜；D因素影响甚微(故在方差分析中以SSD作误差估计用)，即浸泡因素可忽略，不必浸泡(D1)。所以，最佳组合应为A3B1C3D1方案。
具体实施方式
实施例1
姜黄150、黄柏90、栀子120、蒺藜150
称取上述重量份配比的药材粗粉3份，每份约33g，照优选出的A3B1C3D1方案进行煎煮提取，即加入10倍量水，浸泡因素可忽略，煎煮提取3次，每次煮沸1小时，合并煎煮提取液，加热浓缩，浓缩至相对密度为1.07(40℃测)的清膏，将清膏喷雾干燥，加入适量药学意义上的辅料制成片剂。结果见表4。
表4 试验结果
试验结果与正交试验结果基本相近，表明，该工艺方案合理，稳定可行。
实施例2
姜黄100、黄柏60、栀子80、蒺藜100
称取上述重量份配比的药材粗粉约33g，照优选出的A3B1C3D1方案进行煎煮提取，即加入10倍量水，浸泡因素可忽略，煎煮提取3次，每次煮沸1小时，合并煎煮提取液，加热浓缩，浓缩至相对密度为1.10(40℃测)的清膏，将清膏喷雾干燥。经检测，提取物中总生物碱的含量为1.40mg/g，总煎出物的重量比为22.5％。
实施例3
姜黄200、黄柏120、栀子160、蒺藜200
称取上述重量份配比的药材粗粉约33g，照优选出的A3B1C3D1方案进行煎煮提取，即加入10倍量水，浸泡因素可忽略，煎煮提取3次，每次煮沸1小时，合并煎煮提取液，加热浓缩，浓缩至相对密度为1.05(40℃测)的清膏，将清膏喷雾干燥。经检测，提取物中总生物碱的含量为1.44mg/g，总煎出物的重量比为22.7％。
上述实施例中的试验结果与正交试验结果基本相近，表明，该工艺方案合理，稳定可行。
Claims (3)
1.一种蒙药复方协日嘎四味片的提取工艺，其特征在于，所述药物是由下述重量份的蒙药材组成：姜黄100-200、黄柏60-120、栀子80-160、蒺藜100-200。
2.如权利要求1所述的一种蒙药复方协日嘎四味片的提取工艺，其特征在于，提取工艺如下：将姜黄、黄柏、栀子、蒺藜四味药材按重量配比混合粉碎成粗粉，加入10倍量水，浸泡因素可忽略，煎煮提取3次，每次煮沸1小时，合并煎煮提取液，加热浓缩，浓缩至相对密度为1.02-1.15(40℃测)的清膏，将清膏喷雾干燥，加入适量药学意义上的辅料制成片剂。
3.如权利要求2所述的一种蒙药复方协日嘎四味片的提取工艺，其特征在于，所述清膏的密度优选为1.05-1.10(40℃测)。
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| CN114177264A (zh) * | 2021-12-23 | 2022-03-15 | 赤峰学院 | 用于治疗糖尿病及肾炎的中药组合物及其制备方法、应用 |
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