痛宁胶囊制剂工艺及原料药超微粉碎研究
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摘要
目的:本课题研究的痛宁胶囊来源于临床经验方,具有祛风散寒,活血通络的效,用于治疗风寒头痛,瘀血阻滞脉络证。根据药材性质和临床用药特点,尝试应用超微粉碎技术对原药材进行处理后直接用于痛宁胶囊制备,并在实验中对白芷、川芎超微粉碎后的物理、化学等性质进行研究,拟总结出含有挥发性、热敏性成分中药材应用超微粉碎技术的适用性。
方法:(1)以两种香豆素含量及粉体粒径作为指标,筛选白芷饮片常温超微粉碎的最佳工艺,并对白芷超微粉体的物理、化学等性质进行初步的研究。
(2)对川芎分别尝试常温振动粉碎和低温振动粉碎处理,比较二者对热敏性成分和挥发性成分的影响,以阿魏酸和挥发油为指标筛选粉碎的最佳工艺,并对川芎超微粉体的物理、化学、溶出等性质进行初步的研究。
(3)细辛在提取挥发油后,以β-环糊精进行包合。
(4)将经筛选的白芷、川芎超微粉体与细辛环糊精包合物按比例混合,制成颗粒,干燥,分装,即得痛宁胶囊。
(5)质量标准研究部分采用TLC法对痛宁胶囊中各成分药进行了定性鉴别,并对欧前胡素进行了含量测定。
结果:(1)白芷应用常温振动粉碎15min后,其粒径和各项指标均为最佳。
(2)川芎常温振动粉碎挥发油损失比较严重,低温粉碎可以避免损失,热敏性成分含量亦无变化。
(3)拟定痛宁胶囊的质量标准,含量测定的方法学考察结果表明:精密度、稳定性、重现性以及加样回收率均符合要求,实验数据稳定可靠。
结论:白芷常温振动粉碎、川芎低温振动粉碎后其物理、化学性质稳定,并在溶出、热提取等方面较常规粉体优越。各粉体混合后制粒成型性良好。痛宁胶囊各项指标符合药典规定,质量工艺可控。
Objective:The Tongning Capsule comes from clinical experience prescription,with the effectiveness of dispel cold and promoting blood circulation to remove meridian obstruction,be used for the treatment of anemofrigid headache and gore retardation. according to herbal medicine property and clinical characteristics of nature,this study try to use the superfine comminution technique to deal with the original medicine,and directly use for the preparation of Tongning Capsule,to sum up the applicability of superfine powder which contain volatile and heat-sensitive components by studying physics,chemistry and other the nature characteristics of Angelica dahurica a nd Chuanxiong's superfine powder.
Methods:1) Choose the content of two kinds of coumarin and powder size pieces as target to select optimal ambient ternperature super fine crush technics of Angelica dahurica,and investigate physical and chemical characteristic of Angelica dahurica super fine powder preliminary in addition.2) Deal Chuanxiong at ambient temperature and low temperature vibration crush treatment separately,then compare their impact of the heat-sensitive and volatile components,use the content of ferulic acid and volatile oil as the target to select optimal superfine comminution technique, study physical,chemical and dissolution characteristic of Chuanxiong superfine powder preliminary in addition.3) The volatile of Breviscapus was included byβ-cyclodextrin.4) Tongning capsules were made after the process of the pro-rata mix of Angelica dahurica、Chuanxiong s uper fine powder and cyclodextrin inclusion compound of Breviscapus,made of particles,drying and packaging.5) The study on quality specification:By using TLC made qualitative analysis on each constitute of Tongning capsule;By using HPLC made quantitative analysis on imperatorin.
Results:1) The size and the target composition of Angelica dahurica are the best after 15 minutes ambient temperature vibrate crush.2) Compare with ambient temperature vibrate crush,low temperature can inhibit the bss of volatile oil in Chuanxiong and have no change of heat-sensitive ingredients.3) Set up the quality standards of Tongning capsule,methodological study shows that the precision,stability, reproducibility and recovery rate are in line with the requirements,experimental data is stable and reliable.
Conclusion:The physics and chemistry characteristic of Angelica dahurica and Chuanxiong stability which were deal with ambient temperature vibration crush andlow-temperature vibrate crush respectively;and they are superior than conventional powder in dissolution and thermal extraction aspect.The powder mixture has good formability.Tongning capsule is accord with the Chinese Pharmacopoeia requirements,quality and crafts control.
方法:(1)以两种香豆素含量及粉体粒径作为指标,筛选白芷饮片常温超微粉碎的最佳工艺,并对白芷超微粉体的物理、化学等性质进行初步的研究。
(2)对川芎分别尝试常温振动粉碎和低温振动粉碎处理,比较二者对热敏性成分和挥发性成分的影响,以阿魏酸和挥发油为指标筛选粉碎的最佳工艺,并对川芎超微粉体的物理、化学、溶出等性质进行初步的研究。
(3)细辛在提取挥发油后,以β-环糊精进行包合。
(4)将经筛选的白芷、川芎超微粉体与细辛环糊精包合物按比例混合,制成颗粒,干燥,分装,即得痛宁胶囊。
(5)质量标准研究部分采用TLC法对痛宁胶囊中各成分药进行了定性鉴别,并对欧前胡素进行了含量测定。
结果:(1)白芷应用常温振动粉碎15min后,其粒径和各项指标均为最佳。
(2)川芎常温振动粉碎挥发油损失比较严重,低温粉碎可以避免损失,热敏性成分含量亦无变化。
(3)拟定痛宁胶囊的质量标准,含量测定的方法学考察结果表明:精密度、稳定性、重现性以及加样回收率均符合要求,实验数据稳定可靠。
结论:白芷常温振动粉碎、川芎低温振动粉碎后其物理、化学性质稳定,并在溶出、热提取等方面较常规粉体优越。各粉体混合后制粒成型性良好。痛宁胶囊各项指标符合药典规定,质量工艺可控。
Objective:The Tongning Capsule comes from clinical experience prescription,with the effectiveness of dispel cold and promoting blood circulation to remove meridian obstruction,be used for the treatment of anemofrigid headache and gore retardation. according to herbal medicine property and clinical characteristics of nature,this study try to use the superfine comminution technique to deal with the original medicine,and directly use for the preparation of Tongning Capsule,to sum up the applicability of superfine powder which contain volatile and heat-sensitive components by studying physics,chemistry and other the nature characteristics of Angelica dahurica a nd Chuanxiong's superfine powder.
Methods:1) Choose the content of two kinds of coumarin and powder size pieces as target to select optimal ambient ternperature super fine crush technics of Angelica dahurica,and investigate physical and chemical characteristic of Angelica dahurica super fine powder preliminary in addition.2) Deal Chuanxiong at ambient temperature and low temperature vibration crush treatment separately,then compare their impact of the heat-sensitive and volatile components,use the content of ferulic acid and volatile oil as the target to select optimal superfine comminution technique, study physical,chemical and dissolution characteristic of Chuanxiong superfine powder preliminary in addition.3) The volatile of Breviscapus was included byβ-cyclodextrin.4) Tongning capsules were made after the process of the pro-rata mix of Angelica dahurica、Chuanxiong s uper fine powder and cyclodextrin inclusion compound of Breviscapus,made of particles,drying and packaging.5) The study on quality specification:By using TLC made qualitative analysis on each constitute of Tongning capsule;By using HPLC made quantitative analysis on imperatorin.
Results:1) The size and the target composition of Angelica dahurica are the best after 15 minutes ambient temperature vibrate crush.2) Compare with ambient temperature vibrate crush,low temperature can inhibit the bss of volatile oil in Chuanxiong and have no change of heat-sensitive ingredients.3) Set up the quality standards of Tongning capsule,methodological study shows that the precision,stability, reproducibility and recovery rate are in line with the requirements,experimental data is stable and reliable.
Conclusion:The physics and chemistry characteristic of Angelica dahurica and Chuanxiong stability which were deal with ambient temperature vibration crush andlow-temperature vibrate crush respectively;and they are superior than conventional powder in dissolution and thermal extraction aspect.The powder mixture has good formability.Tongning capsule is accord with the Chinese Pharmacopoeia requirements,quality and crafts control.
引文
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