CN110314214A - 一种经前安片及其质量检测方法 - Google Patents
一种经前安片及其质量检测方法 Download PDFInfo
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- CN110314214A CN110314214A CN201910740098.7A CN201910740098A CN110314214A CN 110314214 A CN110314214 A CN 110314214A CN 201910740098 A CN201910740098 A CN 201910740098A CN 110314214 A CN110314214 A CN 110314214A
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- radix
- fructus aurantii
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- premenstrual
- radix bupleuri
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Abstract
本发明属于药物提取技术，公开了一种经前安片，其由如下的原料制备而得：柴胡、枳壳、合欢皮、郁金、香附、青皮、橘核、当归、白芍、川芎、茯苓、大腹皮。本发明通过多次药方删减试验发现，删除部分原料，对药效并没有影响，可以节约企业成本，开发出新的药物品种。
Description
技术领域
本发明属于药物提取技术领域，具体涉及一种经前安片及其质量检测方法。
背景技术
经前期综合征(Premenstrual Syndrome，PMS)是指妇女在月经周期的后期表现出的一系列生理和情感方面的不适症状，症状与精神和内科疾病无关，并在卵泡期缓解，在月经来潮后自行恢复到没有任何症状状态。其主要表现有烦躁易怒、失眠、紧张、压抑以及头痛、乳房胀痛、颜面浮肿等一系列的症状，严重者可影响妇女的正常生活。从经前期综合征的临床症状看，该病是育龄妇女发病率较高的疾病之一。同时，经前期综合征是一种生理和社会心理等综合因素导致的一种妇女疾病。目前严重经前期综合征经前期症状的定义并不一致。但在最近的研究中，这一诊断标准已基本得到统一，并已用于诊断这一系列具有多种表现的严重的经前期症状(经前期烦躁不安精神障碍)---以至少5种症状为基础，同时包括4种核心心理症状之一(出自包含17种生理、心理症状的表格。这17种症状是：抑郁、无助和负罪感、焦虑/压力大、情绪不稳、易怒/持续愤怒、兴趣降低、注意力不集中、疲劳、食欲亢进、睡眠障碍、无自控力或易受打击、协助能力差、头痛、疼痛、水肿/体重增加、抽搐、乳房胀痛)并在经前期加重，月经后减轻或消失等。
经前安主要有柴胡、枳壳、合欢皮、郁金、香附、青皮、路路通、橘核、当归、白芍、川芎、茯苓、大腹皮、甘草等原料制备而成，是治疗经前期紧张症的有效药物；产品为薄膜衣片，除去包衣显棕褐色；气芳香，味苦、微辛。 功能主治：舒肝理气，活血通络。主要用于妇女经前期紧张症、中医辨证属于肝郁气滞者，症见经前情绪激动，烦燥易怒，情绪低落，忧郁，乳房胀痛，胸胁胀痛，少腹痛或头痛，或有不同程度水肿，经量或多或少，色暗，舌质暗，脉弦。 经前安片的批准日期是2010-3-26，生产单位是山东翔宇健康制药有限公司，是本发明的申请人。申请人前期的经前安相关发明专利“经前安片制备工艺及其检测方法”，通过添加原料药，提高了药效，但是存在组方复杂，原料成本较高等缺陷。申请人在药物制备过程中，多次尝试删减不同的原料组分，形成药效类似，但是组分相对较少的组分，可以减少企业原料成本。
发明内容
为了克服现有技术的缺陷，本发明提出一种经前安片及其质量检测方法，所述经前安片在保持类似药效的前提下，通过多次试验进行尝试，删减了部分原料药，以开发出新的医药品种。
本发明是通过如下技术方案来实现的：
一种经前安片，其由如下的原料制备而得：
柴胡、枳壳、合欢皮、郁金、 香附 、青皮、橘核、 当归、白芍、川芎、茯苓、大腹皮。
进一步地，其由如下重量的原料制备而得：
柴胡 400g 枳壳 400g 合欢皮 320g 郁金 320g
香附 320g 青皮 240g 橘核 240g 当归 320g
白芍 320g 川芎 240g 茯苓 240g 大腹皮 240g 。
进一步地，所述经前安片的制备方法包括如下步骤：
步骤1）将柴胡和枳壳在粉碎机中粉碎，过100目筛，然后铺成3mm厚度的平层，置于紫外线下照射45min，收集粉末置于容器中，再添加两倍重量的70%（v/v）的乙醇，加热至40℃，然后300rpm搅拌提取，提取时间为90min；静置12小时，过滤，收集滤液，然后低温旋转蒸发回收乙醇，再冷冻干燥，即得柴胡枳壳提取物；
步骤2）将郁金、香附、青皮、当归以及川芎混合，用蒸馏法提取挥发油，药渣备用，挥发油用β-环糊精制成包合物，备用；将上述药渣加8倍重量水煎煮2次，第一次1小时，第二次0.5小时，合并煎液，滤过，收集滤液A；将剩余原料混合，加水煎煮2次，第一次加10倍重量水煎煮2小时，第二次加8倍重量水煎煮1小时，合并煎煮液，滤过，收集滤液B；合并滤液A和滤液B，减压浓缩至密度为1.20-1.25g/mL的浸膏，放冷，加入乙醇，使含醇量为55%（v/v），静置24小时，滤过，沉淀用55%（v/v）乙醇洗涤，滤过，合并滤液，回收乙醇减压浓缩至密度为1.20-1.25g/mL的浸膏，喷雾干燥，加入包合物和柴胡枳壳提取物，混匀，制成颗粒，干燥，加辅料羧甲基淀粉，硬脂酸镁适量，混匀，压成1000片，包薄膜衣，即得。
优选地，所述步骤1）中，紫外线的强度为2000uW/cm2。
优选地，所述步骤1）中，提取过程中采用微波辅助提取，微波功率为500W。
与现有技术相比，本发明的特点主要包括但是不限于以下几个方面：
本发明动物试验提示本发明的制剂具备较好的镇痛镇静功能，柴胡和枳壳原料使用量减少，并且效果优于现有的经前安片，可进行进一步临床试验研究；本发明制备方法简单可行，对不同的中药成分采用不同技术进行处理，提高了各原料有效成分的浸出，增加了药效，减少了原料浪费；柴胡皂苷和柴胡多糖是柴胡中的主要有效成分，提取通常采用水提醇沉法，提取分离时柴胡皂苷易发生化学变化，而且导致柴胡多糖成分浸出率低；枳壳提取时，采用煎煮的方式，容易导致酮类物质的分解；本发明采用较小的粒径能够提高柴胡枳壳有效组分的浸出率，采用紫外照射配合微波醇提的方式可获得更高的提取率，避免了成分的流失和原料浪费；本发明通过多次药方删减试验发现，删除了路路通和甘草，对药效并没有影响，可以节约企业成本，开发出新的药物品种，但是后续的其他动物学试验仍然需要研究删减路路通和甘草带来的影响。
具体实施方式
为了使本技术领域的人员更好地理解本申请中的技术方案，下面将结合本申请具体实施例，对本发明进行更加清楚、完整地描述，显然，所描述的实施例仅仅是本申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都应当属于本发明保护的范围。
实施例1
一种经前安片，其由如下重量的原料制备而得：
柴胡 400g 枳壳 400g 合欢皮 320g 郁金 320g
香附 320g 青皮 240g 橘核 240g 当归 320g
白芍 320g 川芎 240g 茯苓 240g 大腹皮 240g 。
上述药物制剂的制备方法包括如下步骤：
将柴胡和枳壳在粉碎机中粉碎，过100目筛，然后铺成3mm厚度的平层，置于强度为2000uW/cm2的紫外线下照射45min，收集粉末置于容器中，再添加两倍重量的70%（v/v）的乙醇，加热至40℃，然后300rpm搅拌提取，提取过程中控制微波功率为500W，提取时间为90min；静置12小时，过滤，收集滤液，然后低温旋转蒸发回收乙醇，再冷冻干燥，即得柴胡枳壳提取物；吸光度法检测柴胡多糖总得率为6.61%，HPLC法测得柴胡皂苷总得率为5.39%，枳壳新橙皮苷和柚皮苷的总得率为13.2%；
将郁金、香附、青皮、当归以及川芎混合，用蒸馏法提取挥发油，药渣备用，挥发油用β-环糊精制成包合物，备用；将上述药渣加8倍重量水煎煮2次，第一次1小时，第二次0.5小时，合并煎液，滤过，收集滤液A；将剩余原料（合欢皮、橘核、白芍、茯苓、大腹皮）混合，加水煎煮2次，第一次加10倍重量水煎煮2小时，第二次加8倍重量水煎煮1小时，合并煎煮液，滤过，收集滤液B；合并滤液A和滤液B，减压浓缩至密度为1.20-1.25g/mL的浸膏，放冷，加入乙醇，使含醇量为55%（v/v），静置24小时，滤过，沉淀用55%（v/v）乙醇洗涤，滤过，合并滤液，回收乙醇减压浓缩至密度为1.20-1.25g/mL的浸膏，喷雾干燥，加入挥发油β-环糊精包合物和柴胡枳壳提取物，混匀，制成颗粒，干燥，加辅料羧甲基淀粉，硬脂酸镁适量，混匀，压成1000片，包薄膜衣，即得。
上述制备方法制备的片剂为薄膜衣片，除去包衣显棕褐色；气芳香，味苦、微辛。
【规格】 每片重0.37g（薄膜衣片）
【贮藏】 密闭，置阴凉干燥处。
质量检测：本品每片含枳壳、青皮以柚皮苷（C27H32O14）计，不得少于8.0mg。
对比例1
一种经前安片，其由如下重量的原料制备而得：
柴胡 320g 枳壳 320g 合欢皮 320g 郁金 320g
香附 320g 青皮 240g 路路通 280g 橘核 240g
当归 320g 白芍 320g 川芎 240g 茯苓 240g
大腹皮 240g 甘草 120g；
上述药物制剂的制备方法包括如下步骤：
将柴胡和枳壳在粉碎机中粉碎，过100目筛，然后铺成3mm厚度的平层，置于强度为2000uW/cm2的紫外线下照射45min，收集粉末置于容器中，再添加两倍重量的70%（v/v）的乙醇，加热至40℃，然后300rpm搅拌提取，提取过程中控制微波功率为500W，提取时间为90min；静置12小时，过滤，收集滤液，然后低温旋转蒸发回收乙醇，再冷冻干燥，即得柴胡枳壳提取物；吸光度法检测柴胡多糖总得率为6.61%，HPLC法测得柴胡皂苷总得率为5.39%，枳壳新橙皮苷和柚皮苷的总得率为13.2%；
将郁金、香附、青皮、当归以及川芎混合，用蒸馏法提取挥发油，药渣备用，挥发油用β-环糊精制成包合物，备用；将上述药渣加8倍重量水煎煮2次，第一次1小时，第二次0.5小时，合并煎液，滤过，收集滤液A；将剩余原料（合欢皮、路路通、橘核、白芍、茯苓、大腹皮、甘草）混合，加水煎煮2次，第一次加10倍重量水煎煮2小时，第二次加8倍重量水煎煮1小时，合并煎煮液，滤过，收集滤液B；合并滤液A和滤液B，减压浓缩至密度为1.20-1.25g/mL的浸膏，放冷，加入乙醇，使含醇量为55%（v/v），静置24小时，滤过，沉淀用55%（v/v）乙醇洗涤，滤过，合并滤液，回收乙醇减压浓缩至密度为1.20-1.25g/mL的浸膏，喷雾干燥，加入挥发油β-环糊精包合物和柴胡枳壳提取物，混匀，制成颗粒，干燥，加辅料羧甲基淀粉，硬脂酸镁适量，混匀，压成1000片，包薄膜衣，即得。
上述制备方法制备的片剂为薄膜衣片，除去包衣显棕褐色；气芳香，味苦、微辛。
【规格】 每片重0.37g（薄膜衣片）
【贮藏】 密闭，置阴凉干燥处。
实施例2
一、镇痛试验：
选择雌性昆明小鼠80只，体重范围为20.1±1.8g，健康无病，本公司实验动物中心饲养。随机分为4组，分别为生理盐水组、实施例1组、对比例1组、对照组(经前安片，0.37g/片，山东翔宇健康制药有限公司)；每天给药两次，每次剂量为200mg/kg(实施例1组、对比例1组和对照组分别给予药物，生理盐水组给予同等重量的生理盐水)，连续灌胃给药3天，于末次灌胃给药1小时后，腹腔注射0.6％冰乙酸0.2ml/只，观察30min内小鼠扭体次数，结果见表1。
表1
| 组别 | 小鼠数目 | 30min内扭体次数 |
| 生理盐水组 | 20 | 33.4±12.1 |
| 对照组 | 20 | 8.7±1.9** |
| 实施例1组 | 20 | 7.6±1.5**# |
| 对比例1组 | 20 | 7.4±1.7**# |
*：与生理盐水组比较P<0.05，**：与生理盐水组比较P<0.01，#：与对照组比较P<0.05。
二、镇静试验：
选择雌性昆明小鼠80只，体重范围为20.3±2.2g，健康无病，本公司实验动物中心饲养。随机分为4组，分别为生理盐水组、实施例1组、对比例1、对照组(经前安片，0.37g/片，山东翔宇健康制药有限公司)；每天给药两次，每次剂量为200mg/kg(实施例1组、对比例1组和对照组分别给予药物，生理盐水组给予同等重量的生理盐水)，连续灌胃给药3天，于末次灌胃给药30min后，分别对小鼠腹腔注射戊巴比妥钠50mg/kg。以翻转反射消失及恢复为睡眠指标，记录小鼠注射后的睡眠时间。具体结果见表2：
表2
| 组别 | 小鼠数目 | 睡眠时间（min） |
| 生理盐水组 | 20 | 59.1±20.3 |
| 对照组 | 20 | 78.7±19.2* |
| 实施例1组 | 20 | 82.9±15.6* |
| 对比例1组 | 20 | 84.1±16.3* |
*：与生理盐水组比较P<0.05，**：与生理盐水组比较P<0.01，#：与对照组比较P<0.05。
结论：通过小鼠镇静试验和阵痛实验发现，对照组、实施例1组和对比例1组均比生理盐水组有明显的改善，与对照组（现有经前安片）相比，实施例1组和对比例1组有所提高，但是实施例1组和对比例1组没有明显差异，说明实施例1组删除了路路通和甘草，对药效并没有影响，可以节约企业成本，开发出新的药物品种。
以上列举的仅是本发明的最佳具体实施例。显然，本发明不限于以上实施例，还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。
Claims (5)
1.一种经前安片，其由如下的原料制备而得：
柴胡、枳壳、合欢皮、郁金、 香附 、青皮、橘核、 当归、白芍、川芎、茯苓、大腹皮。
2.根据权利要求1所述的经前安片，其由如下重量的原料制备而得：
柴胡 400g 枳壳 400g 合欢皮 320g 郁金 320g
香附 320g 青皮 240g 橘核 240g 当归 320g
白芍 320g 川芎 240g 茯苓 240g 大腹皮 240g 。
3.根据权利要求1或2所述的经前安片，所述经前安片的制备方法包括如下步骤：
步骤1）将柴胡和枳壳在粉碎机中粉碎，过100目筛，然后铺成3mm厚度的平层，置于紫外线下照射45min，收集粉末置于容器中，再添加两倍重量的70%（v/v）的乙醇，加热至40℃，然后300rpm搅拌提取，提取时间为90min；静置12小时，过滤，收集滤液，然后低温旋转蒸发回收乙醇，再冷冻干燥，即得柴胡枳壳提取物；
步骤2）将郁金、香附、青皮、当归以及川芎混合，用蒸馏法提取挥发油，药渣备用，挥发油用β-环糊精制成包合物，备用；将上述药渣加8倍重量水煎煮2次，第一次1小时，第二次0.5小时，合并煎液，滤过，收集滤液A；将剩余原料混合，加水煎煮2次，第一次加10倍重量水煎煮2小时，第二次加8倍重量水煎煮1小时，合并煎煮液，滤过，收集滤液B；合并滤液A和滤液B，减压浓缩至密度为1.20-1.25g/mL的浸膏，放冷，加入乙醇，使含醇量为55%（v/v），静置24小时，滤过，沉淀用55%（v/v）乙醇洗涤，滤过，合并滤液，回收乙醇减压浓缩至密度为1.20-1.25g/mL的浸膏，喷雾干燥，加入包合物和柴胡枳壳提取物，混匀，制成颗粒，干燥，加辅料羧甲基淀粉，硬脂酸镁适量，混匀，压成1000片，包薄膜衣，即得。
4.根据权利要求3所述的经前安片，所述步骤1）中，紫外线的强度为2000uW/cm2。
5.根据权利要求3所述的经前安片，所述步骤1）中，提取过程中采用微波辅助提取，微波功率为500W。
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| CN106729405A (zh) * | 2016-12-27 | 2017-05-31 | 翔宇药业股份有限公司 | 用于治疗经前期综合征的药物制剂及其制备方法 |
| CN106729406A (zh) * | 2016-12-27 | 2017-05-31 | 翔宇药业股份有限公司 | 经前安制剂的制备方法 |
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| CN106729405A (zh) * | 2016-12-27 | 2017-05-31 | 翔宇药业股份有限公司 | 用于治疗经前期综合征的药物制剂及其制备方法 |
| CN106729406A (zh) * | 2016-12-27 | 2017-05-31 | 翔宇药业股份有限公司 | 经前安制剂的制备方法 |
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