CN106729063B - 一种更年安片的制备方法 - Google Patents
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Abstract
本发明涉及一种更年安片制剂的制备方法，包括以下步骤：1)回流膏的制备：取首乌藤、制何首乌、钩藤、五味子、泽泻和牡丹皮，加4‑8倍量60％乙醇回流提取1‑3次，每次1‑3小时，浓缩得到回流膏；2)干浸膏粉的制备：取地黄、玄参、茯苓、熟地黄、仙茅和麦冬，加4‑8倍量的水煎煮1‑3次，每次1‑3小时，煎液浓缩成稠膏状，减压干燥，粉碎即得干浸膏粉；3)浮小麦等三味药材细粉的制备：分别取浮小麦、磁石、珍珠母干燥，粉碎成细粉，分别装袋，备用；4)将浮小麦等三味药材的细粉、干浸膏粉、回流膏混匀，制粒，干燥，压片，即得片剂。
Description
技术领域
本发明属于医药技术领域，具体涉及一种更年安片的制备方法,。
背景技术
更年安片处方是由十五味中药材组成，目前的制备工艺：浮小麦、磁石、珍珠母粉三味药材碎成细粉；地黄、熟地黄、玄参、茯苓、仙茅、麦冬六味药材加水煎煮，制得水煎浓缩液；其余首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮六味药材用60％乙醇渗漉提取，制得渗漉浓缩液；取上述两种浓缩液与浮小麦等三味细粉混匀，制成粗颗粒，干燥，粉碎，过筛，加入适量75％乙醇制颗粒，低温干燥，过筛，加入硬脂酸镁，混匀，压制成片，包糖衣或薄膜衣，即得。
更年安片具有滋阴清热，除烦安神。用于肾阴虚所致的绝经前后诸证，症见烦热出汗、眩晕耳鸣、手足心热、烦躁不安；更年期综合征见上述证候者。
现有技术制备的更年安片，主要存在着制何首乌，首乌藤两味药材有效成分大黄素提取转移率低，素片脆碎度低导致包衣时有少许掉边的问题，并且制备工艺复杂，因清膏量大制粒时需经两次制粒，才能制得更年安片颗粒，两次干燥过程对颗粒大黄素含量，五味子鉴别具有一定的损耗。
本发明人经过研究发现，上述制备方法，存在药物疗效不高，药材存在浪费等问题，所得片剂储存一定时间会裂片，而且有效成分降低。为此，申请人对现有的制备方法进行改进，提供一种更年安片的新的制备方法，该方法能够提高更年安片的疗效，提高更年安片有效成分含量，同时解决了稳定性和裂片问题。
本发明提供一种更年安片新的制备方法，将首乌藤、制何首乌、钩藤等六味药材采用回流提取方式，制得回流膏，以提高大黄素提取转移率；再将地黄、熟地黄、玄参等六味药材加水煎煮，煎液浓缩至一定相对密度，减压干燥，粉碎，制得干膏粉；最后将浮小麦等三味药材生药粉，与上述干膏、回流膏混匀，一起湿法制粒，低温干燥，过筛，加入硬脂酸镁，混匀，压制成片，包糖衣或薄膜衣，即得。
发明内容
本发明的目的在于提供一种更年安片的制备方法。通过该方法制备得到的片剂具有非常好质量。
本发明所述的更年安片的制备方法，包括以下步骤：
处方：
制备方法：
1)回流膏的制备：取首乌藤、制何首乌、钩藤、五味子、泽泻和牡丹皮，加4-8倍量60％乙醇回流提取1-3次，每次1-3小时，浓缩得到回流膏；
2)干浸膏粉的制备：取地黄、玄参、茯苓、熟地黄、仙茅和麦冬，加4-8倍量的水煎煮1-3次，每次1-3小时，煎液浓缩成稠膏状，减压干燥，粉碎即得干浸膏粉；
3)浮小麦等三味药材细粉的制备：分别取浮小麦、磁石、珍珠母干燥，粉碎成细粉，分别装袋，备用；
4)将浮小麦等三味药材细粉、干浸膏粉、回流膏混匀，制粒，干燥，压片，即得片剂。
其中，4-8倍量的乙醇是指：乙醇的用量为首乌藤、制何首乌、钩藤、五味子、泽泻和牡丹皮药材总药材重量的4-8倍，
其中，60％乙醇是指乙醇的浓度为60％。
优选的，本发明的制备方法，包括以下步骤：
1)回流膏的制备：取首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮材加6倍量的浓度60％的乙醇回流提取2次，第一次2小时，第二次1.5小时；回流液回收乙醇至无醇味，减压浓缩至相对密度1.18-1.20(80℃测)的回流膏；
2)干浸膏粉的制备：取地黄、玄参、茯苓、熟地黄、仙茅、麦冬加7倍量的水煎煮2次，第一次3小时，第二次2小时，过滤，滤液浓缩成稠膏状，减压干燥，粉碎即得干浸膏粉；
3)浮小麦等三味药材细粉的制备：分别取浮小麦、磁石、珍珠母干燥，粉碎成细粉，分别装袋，备用；
4)将浮小麦等三味药材细粉、干浸膏粉混匀，加入回流膏，加适量纯化水，制得软材，制粒，干燥，压片，即得片剂。
本发明的制备方法是经过大量实验筛选后得到的，通过以下实验数据说明本发明的有益效果：
批号：150301指的是本发明实施例1制备得到的回流膏
批号：150302指的是按照现有方法制备得到的渗漉膏
批号：150302的制备方法如下：
取首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮材加入6倍量60％乙醇进行渗漉，浸渍48小时，以3ml/kg.min的速度缓缓渗漉，收集渗漉液，回收乙醇，浓缩成稠膏，即得。
1.1对新方法及原工艺所得样品进行质量对比
1.1.1清膏样品对比
注：首乌藤药材大黄素含量为0.04％，投料量为105g,制何首乌药材大黄素含量为0.17％，投料量为52.5,试制量为1000片，规格为0.42g/s。
1.1.2待包装样品质量对比
1.2对新方法及原工艺所得样品进行加速6个月稳定性考察试验结果批号：150301
| 检测项目 | 0月 | 1月 | 2月 | 3月 | 6月 |
| 崩解时限(分钟) | 13 | 12 | 15 | 14 | 17 |
| 鉴别 | 均符合规定 | 均符合规定 | 均符合规定 | 均符合规定 | 均符合规定 |
| 大黄素(mg/s) | 0.0738 | 0.0726 | 0.0668 | 0.0636 | 0.0585 |
批号：150302
在制备工艺上，本发明的制备方法，相对于现有的更年安片制备方法，主要改进在于：采用回流法替代渗漉法，水煎膏减压干燥制干浸膏。正是这两点改进，使得本发明产生了意想不到的效果：
①用改进的提取方法制成的回流膏，大黄素提取转移率比原工艺提高了30％；
②采用干浸膏一步制粒，降低大黄素及五味子甲素因两次制粒而损耗的影响；
③取回流膏湿法制粒，增加了软材粘性，使素片脆碎度(≤1％)，避免了包衣时出现掉边的问题，产品质量大幅度提高。
本发明相对于现有技术而言，大大提高产品的稳定性和质量，减少药物的副作用，同时还提高有效成分的含量，本发明还简化工艺流程，降低成产成本，适合大规模生产。
具体实施方式
通过以下具体实施例对本发明作进一步的说明，但不作为限制。
实施例1片剂
处方：制成1000片
制法：
⑴回流膏的制备：取首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮材加6倍量60％乙醇回流提取二次，第一次2小时，第二次1.5小时；回流液回收乙醇至无醇味，减压浓缩至相对密度1.18-1.20(80℃测)，减压干燥，粉碎，即得回流膏；
⑵干浸膏粉的制备：取地黄、玄参、茯苓、熟地黄、仙茅、麦冬加7倍量水煎煮二次，第一次3小时，第二次2小时，过滤，滤液浓缩至适量，即得干浸膏粉；
⑶浮小麦等三味药材细粉的制备：分别取浮小麦、磁石、珍珠母干燥，粉碎成细粉，分别装袋，备用；
⑷将浮小麦等三味药材生药粉、干浸膏粉混匀，加入回流膏，加适量纯化水，制得软材，制粒，干燥，过筛，加入硬脂酸镁，混匀，压制成1000片，包糖衣或薄膜衣，即得。
实施例2片剂
制成1000片
制法：
⑴回流膏的制备：取首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮材，加入浓度为60％乙醇回流提取二次，第一次2小时，第二次1.5小时；回流液回收乙醇至无醇味，减压浓缩至适量，即得回流膏；
⑵浸膏的制备：取地黄、玄参、茯苓、熟地黄、仙茅、麦冬加加7倍量水煎煮二次，第一次3小时，第二次2小时，过滤，滤液浓缩至适量，即得浸膏；
⑶浮小麦等三味药材细粉的制备：取浮小麦、磁石、珍珠母除杂，粉碎成细粉，即得；
⑷将浮小麦等三味药材生药粉、浸膏混匀，制成粗颗粒，干燥，粉碎，过筛加入回流膏，加适量纯化水，制得软材，制粒，干燥，过筛，加入硬脂酸镁，混匀，压制成1000片，包糖衣或薄膜衣，即得。
实施例3
制法：
⑴回流膏的制备：取首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮材加6倍量60％乙醇回流提取二次，第一次2小时，第二次1.5小时；回流液回收乙醇至无醇味，减压浓缩至相对密度1.18-1.20(80℃测)，即得回流膏；
⑵干浸膏粉的制备：取地黄、玄参、茯苓、熟地黄、仙茅、麦冬加加7倍量水煎煮二次，第一次3小时，第二次2小时，过滤，滤液浓缩成稠膏状，减压干燥，粉碎即得干浸膏粉；
⑶浮小麦等三味药材细粉的制备：取浮小麦、磁石、珍珠母除杂，粉碎成细粉，即得；
⑷将浮小麦等三味药材生药粉、干浸膏粉混匀，加入回流膏，加适量纯化水，制得软材，制粒，干燥，过筛，加入硬脂酸镁，混匀，压制成1000片压片，即得片剂。
试验例1、本发明制备条件的筛选过程
对首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮五味药材回流工艺参数
进行优化，本方案主要对乙醇浓度、提取时间、提取次数进行筛选，以大黄
素提取转移率为考核指标。具体实施情况见表1：
表1回流提取工艺路线筛选
根据实验结果表明:首乌藤等五味药材加8倍量60％乙醇回流提取3次，第一次2小时，第二次1.5小时，第三次1小时，清膏大黄素提取转移率最高，但因大生产工艺的可行性需对提取时间及乙醇耗量综合考虑，所以最终优选出：加6倍量60％乙醇回流提取2次，第一次2小时，第二次1.5小时为最佳工艺参数，所得清膏含量能满足产品质量要求。
Claims (1)
1.一种更年安片的制备方法，其特征在于，包括以下步骤：
处方：
地黄：52.5g 泽泻：52.5g 麦冬：52.5g 熟地黄：52.5g 玄参：52.5g 茯苓：105g
仙茅：105g 磁石: 52.5g 牡丹皮: 34.5g 珍珠母: 105g 五味子:52.5 首乌藤:105g
制何首乌: 52.5g 浮小麦: 105g 钩藤:105g
60%乙醇：2412g 硬脂酸镁：2.25g
制备方法：
1）回流膏的制备：取首乌藤、制何首乌、钩藤、五味子、泽泻、牡丹皮加6倍量60%乙醇回流提取二次，第一次2小时，第二次1.5小时；回流液回收乙醇至无醇味，80℃测定，减压浓缩至相对密度1.18-1.20，减压干燥，粉碎，即得回流膏；
2）干浸膏粉的制备：取地黄、玄参、茯苓、熟地黄、仙茅、麦冬加7倍量水煎煮二次，第一次3小时，第二次2小时，过滤，滤液浓缩至适量，即得干浸膏粉；
3）细粉的制备：分别取浮小麦、磁石、珍珠母干燥，粉碎成细粉，分别装袋，备用；
4）将细粉、干浸膏粉混匀，加入回流膏，加适量纯化水，制得软材，制粒，干燥，过筛，加入硬脂酸镁，混匀，压制成1000片，包糖衣或薄膜衣，即得。
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