CN107126480B - 一种治疗颈椎病的中药胶囊剂及其质量控制方法 - Google Patents
一种治疗颈椎病的中药胶囊剂及其质量控制方法 Download PDFInfo
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Abstract
本发明公开了一种治疗颈椎病的中药胶囊剂,其特征在于由熟地黄、制何首乌、牛膝、杜仲、鹿衔草、骨碎补、葛根、三七、威灵仙、甘草等十味药物组成;本发明公开了该中药胶囊剂的制备方法及其质量控制方法;该胶囊剂适用于肾虚血瘀所致的颈椎病,症见颈项胀痛麻木、活动不利、头晕耳鸣等,治疗总有效率在85%以上。
Description
技术领域
本发明涉及一种治疗颈椎病的中药胶囊剂,属于中药制药领域。
背景技术
颈椎病又称颈椎综合征,是颈椎骨关节炎、增生性颈椎炎、颈神经根综合征、颈椎间盘脱出症的总称,是一种以退行性病理改变为基础的疾患。主要由于颈椎长期劳损、骨质增生,或椎间盘脱出、韧带增厚,致使颈椎脊髓、神经根或椎动脉受压,出现一系列功能障碍的临床综合征。颈椎病的常见症状有颈痛、头晕、四肢麻木无力,严重的可以合并大小便障碍。
著名颈椎病专家、中山大学附属第一医院康复科主任赖在文教授日前在中国康复医学会第七次全国颈椎病学术会议上介绍说,在他接诊的颈椎病人当中,40岁以下患者人数过半,其中年龄最小的只有两岁。颈椎病本是中老年人的常见病,但是近年来呈现发病率不断上升和发病年龄不断提前的趋势。调查显示,全国大约有7%~10%的人患颈椎病。而且,颈椎病发病出现低龄化趋势,其中中小学生的颈椎病发病率急速上升。
本发明公开了一种治疗颈椎病的中药良药,适用于肾虚血瘀所致的颈椎病,症见颈项胀痛麻木、活动不利、头晕耳鸣等,治疗总效率在85%以上。
发明内容
本发明公开了一种治疗颈椎病的中药良药,其特征在于其处方由熟地黄、制何首乌、牛膝、杜仲、鹿衔草、骨碎补、葛根、三七、威灵仙、甘草等十味药物组成。其中熟地黄补血滋阴、益精填髓,主治肝肾阴虚,腰膝酸软,眩晕耳鸣;制首乌补益精血、乌须发、强筋骨、补肝肾;杜仲补肝肾,强筋骨,安胎,配伍牛膝,补肝肾及强筋骨之力增强,常用于治肝肾不足的腰腿疼痛及两足无力等症;鹿衔草能补虚、益肾、祛风除湿、活血、补肾强骨;骨碎补:补肾强骨、续伤止痛;葛根解表退热、生津止渴、止泻,治疗项背板滞酸痛;三七活血化瘀、消肿定痛,为伤科之要药,且能补虚强壮;威灵仙祛风除湿,通络止痛;甘草解毒而调和诸药;诸药合用共奏补肾强筋、养血活血、通络、祛风止痛之功效;适用于肾虚血瘀所致的颈椎病,症见颈项胀痛麻木、活动不利、头晕耳鸣等。
本发明还公开了制备该中药胶囊剂所需药味的配比:
熟地黄180g~200g 制何首乌180g~200g 牛膝80g~90g 杜仲100g~110g鹿衔草80g~90g 骨碎补100g~110g 葛根100g~110g 三七30g~50g 威灵仙80g~90g 甘草30g~50g。
本发明发公开了该中药胶囊剂的制备工艺:
1)取处方量三七粉碎成细粉;
2)取熟地黄、何首乌等九味药材,加六倍量水浸泡1小时,煎煮三次,第一次2小时,第二次2小时,第三次1小时,过滤,合并提取液,浓缩至相对密度1.25~1.30(80℃)的浸膏;
3)将上述细粉与浸膏混合均匀,75℃以下减压干燥,粉碎,过80目筛;将上述原料粉与适量淀粉混合均匀,加入95%酒精制颗粒,过20目筛,80℃以下干燥(控制颗粒含水份在5.0%以下);
4)将上述颗粒与适量硬脂酸镁混和均匀,装入胶囊制成胶囊剂即得。
本发明还公开了该胶囊剂的质量控制方法:
【鉴别】
1)取本品内容物4g,加乙醇20ml,回流提取40min,静置;取上清液10ml,加盐酸1ml,回流提取1h,浓缩至约5ml,加水10ml,用石油醚(60-90℃)20ml提取,提取液蒸干,残渣加乙醇2ml溶解,作供试品溶液;另取齐墩果酸加乙醇制成每1ml含1mg的溶液,作对照品溶液;吸取供试品溶液10-20μl,对照品溶液10μl,分别点于同一硅胶G薄层板上,以氯仿-甲醇(40:1)溶液展开,取出晾干,喷以磷钼酸试液,110℃供约10min;供试品色谱中,在与对照品色谱中相应的位置上,显相同的蓝色斑点;
2)取本品内容物3.5g,加乙酸乙酯100ml,超声处理30分钟,滤过,滤液然干, 残渣加甲醇l ml使溶解,作为供试品溶液。另取葛根素对照品,加甲醇制成每l ml含1mg的溶液,作为对照品溶液。照薄层色谱法(中国药典2015年版四部通则0502)试验,吸取上述溶液各10ul,分别点于同一以羧甲基纤维素钠为黏合剂的硅胶GF254薄层板上,以三氯甲烷-甲醇-水(7:2.5:0.25)为展开 剂,展开,取出,晾干,置紫外光灯(254nm)下检视。供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的斑点;
3)取本品内容物2. 3g,加甲醇50nl,超声处理30分钟,滤过,滤液蒸干,残渣加甲醇1ml 使溶解,作为供试品溶液。另取大黄素对照品,加甲醇制成每1ml含1mg的溶液,作为对照品溶液。照薄层色谱法(中国药典2015年版四部通则0502)试验。吸取上述供试品溶液10ul、对照品溶液5ul,分别点于同一以羧甲基纤维素钠为黏合剂的硅胶G薄层板上,以石油醚 (30~60℃)-甲酸乙酯-甲酸(15:5:1)的上层溶液为展开剂,展开,取出,晾干。供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的黄色斑点;置紫外光灯(365nm)下检视,显相同颜色的荧光斑点;
4)取本品内容物3g,加乙醇30nl,超声处理30分钟,滤过,滤液蒸干,残渣加水20ml使溶解,移至分液漏斗中,用0.4%氢氧化钠溶液饱和的正丁醇30ml,振摇提取(轻摇防止乳化),分取正丁醇液,蒸干,残渣加乙醇1ml使溶解,作为供试品溶液。另取人参皂苷Rg1对照品,加乙醇制成每1ml含1mg的溶液,作为对照品溶液。照薄层色谱法(中国药典2015年版四部通则0502)试验,吸取上述溶液各10ul,分别点于同一硅胶G薄层板上,以三氯甲烷-甲醇-水 (13:7:2)的下层溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇液,在105℃加热至斑点清晰。供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的斑点;
【检査】
应符合胶囊剂项下有关的各项规定(中囯药典2015年版四部通则0103);
【含量测定】
照高效液相色谱法(中国药典2015年版四部通则0512)测定;
色谱条件与系统适用性试验 以十八烷基硅烷键合硅胶为填充剂:以乙腈-水(26:74)为流动相;蒸发光散射检测器,理论板数按黄芪甲苷峰计算应不低于3000;
对照品溶液的制备:精密称取人参皂苷Rg1对照品,加甲醇制成每1ml含0.22mg的溶液即得;
供试品溶液的制备:取装量差异项下的内容物,研细,混匀,取1g,精密称定,精密加入水饱和的正丁醇50ml,密塞,称定重量,放置过夜,超声(功率300W,频率25Khz)处理1小时,放冷,再称定重量,用水饱和的正丁醇补足重量,滤过。精密量取续滤液25ml,用正丁醉饱和的氨试液洗涤2次,每次25ml,洗涤液再用水饱和的正丁醇振摇提取2次,每次20ml,合并正丁醇液,蒸干,残渣加甲醇溶解并转移至5ml量瓶中,加甲醇至刻度,摇匀,即得;
测定法:分别精密吸取对照品溶液15、20、25 ul及供试品溶液20 ul,注入高效液相色谱仪,测定,即得;
本品每粒含三七以人参皂苷Rg1 (C42H72O14)计,不得少于0.30mg。
实施案例
实施案例1:采用本发明所述处方配比和制备方法制备批号为01、02、03的三批中药胶囊,其成品率稳定可控,其制备过程如下:
1)取处方量三七粉碎成细粉备用;
2)取熟地黄、何首乌等九味药材,加六倍量水浸泡1小时,煎煮三次,第一次2小时,第二次2小时,第三次1小时,过滤,合并提取液,浓缩至相对密度1.25~1.30(80℃)的浸膏;
3)将上述细粉与浸膏混合均匀,75℃以下减压干燥,粉碎,过80目筛;将上述原料粉与适量淀粉混合均匀,加入95%酒精制颗粒,过20目筛,80℃以下干燥(控制颗粒含水份在5.0%以下);
4)将上述颗粒与适量硬脂酸镁混和均匀,装入胶囊制成胶囊剂1000粒即得;
实施案例2:采用本发明所述质量控制方法对实施案例一中三批胶囊进行检验,结果三批胶囊质量均一可控,其检验结果如下:
批号 | 鉴别1 | 鉴别2 | 鉴别3 | 鉴别4 | 水分 | 装量差异 | 崩解时限 | 微生物限度 | 含量测定 |
01 | 检出与齐墩果酸对照品相对应的斑点 | 检出与葛根素对照品相对应的斑点 | 检出与大黄素对照品相对应的斑点 | 检出与人参皂苷Rg1对照品相对应的斑点 | 5.0% | 符合规定 | 14min | 符合规定 | 0.54mg |
02 | 检出与齐墩果酸对照品相对应的斑点 | 检出与葛根素对照品相对应的斑点 | 检出与大黄素对照品相对应的斑点 | 检出与人参皂苷Rg1对照品相对应的斑点 | 4.9% | 符合规定 | 15min | 符合规定 | 0.50mg |
03 | 检出与齐墩果酸对照品相对应的斑点 | 检出与葛根素对照品相对应的斑点 | 检出与大黄素对照品相对应的斑点 | 检出与人参皂苷Rg1对照品相对应的斑点 | 4.9% | 符合规定 | 12min | 符合规定 | 0.52mg |
Claims (2)
1.一种治疗颈椎病的中药胶囊剂的质量检测方法,其特征在于:其处方由熟地黄、制何首乌、牛膝、杜仲、鹿衔草、骨碎补、葛根、三七、威灵仙、甘草等十味药物组成;
其制备工艺如下:1)取处方量三七粉碎成细粉;
2)取熟地黄、何首乌等九味药材,加六倍量水浸泡1小时,煎煮三次,第一次2小时,第二次2小时,第三次1小时,过滤,合并提取液,浓缩至80℃时相对密度1.25~1.30的浸膏;
3)将上述细粉与浸膏混合均匀,75℃以下减压干燥,粉碎,过80目筛;将上述原料粉与适量淀粉混合均匀,加入95%酒精制颗粒,过20目筛,80℃以下干燥控制颗粒含水份在5.0%以下;
4)将上述颗粒与适量硬脂酸镁混合均匀,装入胶囊制成胶囊剂即得;
其药物配比如下:熟地黄180g~200g制何首乌180g~200g牛膝80g~90g杜仲100g~110g鹿衔草80g~90g骨碎补100g~110g葛根100g~110g三七30g~50g威灵仙80g~90g甘草30g~50g;
其质量检测方法如下:
【鉴别】
1)取本品内容物4g,加乙醇20ml,回流提取40min,静置;取上清液10ml,加盐酸1ml,回流提取1h,浓缩至约5ml,加水10ml,用60-90℃石油醚20ml提取,提取液蒸干,残渣加乙醇2ml溶解,作供试品溶液;另取齐墩果酸加乙醇制成每1ml含1mg的溶液,作对照品溶液;吸取供试品溶液10-20μl,对照品溶液10μl,分别点于同一硅胶G薄层板上,以氯仿-甲醇,40:1的溶液展开,取出晾干,喷以磷钼酸试液,110℃供约10min;供试品色谱中,在与对照品色谱中相应的位置上,显相同的蓝色斑点;
2)取本品内容物3.5g,加乙酸乙酯100ml,超声处理30分钟,滤过,滤液然干.残渣加甲醇l ml使溶解,作为供试品溶液;另取葛根素对照品,加甲醇制成每l ml含1mg的溶液,作为对照品溶液;照中国药典2015年版四部通则0502薄层色谱法试验,吸取上述溶液各10ul,分别点于同一以羧甲基纤维素钠为黏合剂的硅胶GF254薄层板上,以三氯甲烷-甲醇-水,7:2.5:0.25的溶液为展幵剂,展开,取出,晾干,置紫外光灯254nm下检视;供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的斑点;
3)取本品内容物2.3g,加甲醇50nl,超声处理30分钟,滤过,滤液蒸干,残渣加甲醇1ml使溶解,作为供试品溶液;另取大黄素对照品,加甲醇制成每1ml含1mg的溶液,作为对照品溶液;照中国药典2015年版四部通则0502薄层色谱法试验;吸取上述供试品溶液10ul、对照品溶液5ul,分别点于同一以羧甲基纤维素钠为黏合剂的硅胶G薄层板上,以30~60℃的石油醚-甲酸乙酯-甲酸,15:5:1的上层溶液为展开剂,展开,取出,晾干,供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的黄色斑点;置紫外光灯365nm下检视,显相同颜色的荧光斑点;
4)取本品内容物3g,加乙醇30nl,超声处理30分钟,滤过,滤液蒸干,残渣加水20ml使溶解,移至分液漏斗中,用0.4%氢氧化钠溶液饱和的正丁醇30ml,振摇提取,轻摇防止乳化,分取正丁醇液,蒸干,残渣加乙醇1ml使溶解,作为供试品溶液;另取人参皂苷Rg1对照品,加乙醇制成每1ml含1mg的溶液,作为对照品溶液;照中国药典2015年版四部通则0502薄层色谱法试验,吸取上述溶液各10ul,分别点于同一硅胶G薄层板上,以三氯甲烷-甲醇-水,13:7:2的下层溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇液,在105℃加热至斑点清晰,供试品色谱中,在与对照品色谱相应的位置上,显相同颜色的斑点;【检査】
应符合中囯药典2015年版四部通则0103胶囊剂项下有关的各项规定;
【含量测定】
照中国药典2015年版四部通则0512高效液相色谱法测定
色谱条件与系统适用性试验:以十八烷基硅烷键合硅胶为填充剂:以乙腈-水,26:74的溶液为流动相;蒸发光散射检测器;理论板数按黄芪甲苷峰计算应不低于3000;
对照品溶液的制备:精密称取人参皂苷Rg1对照品,加甲醇制成每1ml含0.22mg的溶液,即得;
供试品溶液的制备:取装量差异项下的内容物,研细,混匀,取1g,精密称定,精密加入水饱和的正丁醇50ml,密塞,称定重量,放置过夜,功率300W、频率25Khz,超声处理1小时,放冷,再称定重量,用水饱和的正丁醇补足重量,滤过;精密量取续滤液25ml,用正丁醉饱和的氨试液洗涤2次,每次25ml,洗涤液再用水饱和的正丁醇振摇提取2次,每次20ml,合并正丁醇液,蒸干,残渣加甲醇溶解并转移至5ml量瓶中,加甲醇至刻度,摇匀,即得;
测定法:分别精密吸取对照品溶液15、20、25ul及供试品溶液20ul,注入高效液相色谱仪,测定,即得;
本品每粒含三七以人参皂苷Rg1即C42H72O14计,不得少于0.30mg。
2.如权利要求1所述中药胶囊剂的质量检测方法,其特征在于:所用辅料为淀粉和硬脂酸镁。
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