CN115444825B - 芍药甘草汤冻干粉的制备方法 - Google Patents
芍药甘草汤冻干粉的制备方法 Download PDFInfo
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- CN115444825B CN115444825B CN202210636060.7A CN202210636060A CN115444825B CN 115444825 B CN115444825 B CN 115444825B CN 202210636060 A CN202210636060 A CN 202210636060A CN 115444825 B CN115444825 B CN 115444825B
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- Prior art keywords
- licorice
- freeze
- radix paeoniae
- dried powder
- paeoniae alba
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
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- A61K36/18—Magnoliophyta (angiosperms)
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- A—HUMAN NECESSITIES
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Abstract
本发明提供一种芍药甘草汤冻干粉的制备方法,属于中药制剂技术领域,所述制备方法是取白芍加至浓度为80~90wt%的乙醇水溶液中,调节pH值,浸泡后,加盖煎煮,得白芍药液;取甘草加至水中,调pH值,浸泡后,煎煮,过滤,得甘草药液;将白芍药液与甘草药液合并,浓缩后,经冷冻干燥,即得所述芍药甘草汤冻干粉。本发明所制芍药甘草汤中所含17种有效成分相对于经典名方中的煎煮方法均有所提高,能够有效提高芍药甘草汤的疗效。
Description
技术领域
本发明涉及中药冻干粉的制备,尤其涉及一种芍药甘草汤冻干粉的制备方法。
背景技术
芍药甘草汤为《古代经典名方目录》(第一批)中的第6首处方。原文出自《伤寒论》(汉·张仲景),原文描述为“伤寒脉浮,自汗出,小便数,心烦,微恶寒,脚挛急。……若厥愈足温者,更作芍药甘草汤与之,其脚即伸。”原文记载处方组成为“白芍药、甘草各四两,炙。以上二味,以水三升,煮取一升五合,去滓,分温再服。”根据文献及考证资料,研究确定现代应用剂量及炮制品为:白芍12g,水炙甘草12g。有柔肝舒筋、缓急止痛之功效。主治阴血、津液亏虚,筋脉失养而导致的筋脉、肌肉拘急、痉挛等病症,还可以很好的预防心脏病、治疗静脉曲张等。
原文记载煎煮方法为“以上二味,以水三升,煮取一升五合”,经考证按照汉代一升折合现代容积为200mL、一合折合现代容积为20mL计算,芍药甘草汤换算成现代制法为以上两味,加水600mL,煎煮至药液为300mL。但该法煎熬费时、服用不便,不利于质量控制和使用。
发明内容
针对上述问题,本发明提供一种芍药甘草汤冻干粉的制备方法。
为实现上述目的,本发明所采用的技术方案为:
一种芍药甘草汤冻干粉的制备方法,其特征在于,所述制备方法包括以下步骤:
取白芍加至浓度为80~90wt%的乙醇水溶液中,调节pH值至6.0~6.5,浸泡后,加盖煎煮,过滤,得白芍药液;
取甘草加至水中,调节pH值至7.2~7.5,浸泡后,煎煮,过滤,得甘草药液;
将白芍药液与甘草药液合并,浓缩后,经冷冻干燥,即得所述芍药甘草汤冻干粉。
进一步的,所述乙醇水溶液的用量为白芍的7~8重量倍;水的用量是甘草的8~10重量倍。
进一步的,所述白芍是采用文火煎煮1.5~2h;所述甘草是采用文火煎煮2~3h。
进一步的,所述白芍和甘草浸泡的时间均为0.5~1h。
进一步的,所述浓缩是在60~80℃、-0.08~-0.1MPa条件下进行减压浓缩。
进一步的,浓缩后且冷冻干燥前,所述浓缩液与白芍和甘草的总重量比为1.8~2.2:1。
进一步的,所述冷冻干燥是先在-30~-45℃预冻至少60min,再于-40~-70℃真空干燥至少12h。
进一步的,真空干燥的真空度<100Pa。
进一步的,所述白芍与甘草的重量比为1:1。
本发明的芍药甘草汤冻干粉的制备方法的有益效果为:
本发明通过检测芍药甘草汤中最主要的17种有效成分,利用白芍和甘草的不同特性,采用不同溶剂分别进行提取,能够有效增加最终所制芍药甘草汤冻干粉中17种有效成分的含量;
本发明通过考察自白芍中提取的没食子酸、异甘草苷、丹皮酚、芍药内酯苷、芍药苷、芍药内酯B、苯甲酸、柚皮素和苯甲酰芍药苷等有效成分及甘草中提取的芹糖甘草苷、甘草苷、芒柄花黄素、新甘草苷、3'-去氧苏木酮A、异甘草素、甘草素和甘草酸,选取更适合白芍和甘草的提取溶剂在不同提取条件下进行提取,有效增加这些有效成分的提取量;
本发明所制芍药甘草汤中所含17种有效成分相对于经典名方中的煎煮方法均有所提高,能够有效提高芍药甘草汤的疗效;
本发明通过选择合适的浓缩和冻干工艺,在尽量保证有效成分含量不降低的情况下,制成冻干粉,提高储存和服用便利性;
本发明生产工艺简便、溶剂使用量低,能够节约浓缩和冻干时间,降低生产成本。
附图说明
图1是本发明实施例1中芍药甘草汤冻干粉的高效液相色谱图;
图2是本发明对比例1中芍药甘草汤冻干粉的高效液相色谱图。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述。在下面的描述中阐述了很多具体细节以便于充分理解本发明,但是本发明还可以采用其他不同于在此描述的其它方式来实施,本领域技术人员可以在不违背本发明内涵的情况下做类似推广,因此本发明不受下面公开的具体实施例的限制。
实施例1一种芍药甘草汤冻干粉的制备方法
本实施例为一种芍药甘草汤冻干粉的制备方法,具体合成过程包括以下步骤:
1)取12g白芍,加入8倍浓度为85wt%的乙醇水溶液(96g),滴加少量10wt%的盐酸调节pH值至6.5,浸泡1h后,加盖文火煎煮1.5h,经200目尼龙筛常压过滤,得白芍药液;
2)取12g甘草,加入9倍水(108g),再滴加少量10wt%氢氧化钠水溶液调节pH值至7.4,浸泡1h后,无需加盖直接文火煎煮2.5h,再经200目尼龙筛常压过滤,得甘草药液;
3)将白芍药液与甘草药液合并,于70℃、-0.1MPa条件下进行减压浓缩,浓缩至所得浓缩液为48g时停止浓缩,移至冻干机中,于-35℃预冻60min,然后降温至-50℃,维持-50℃于真空度<100Pa条件下进行真空干燥12h,粉碎,即得7.47g芍药甘草汤冻干粉,标记为M1。所得芍药甘草汤冻干粉即为芍药甘草汤的干膏粉,干膏率为32.25%。
取芍药甘草汤冻干粉M1利用高效液相色谱进行17种有效成分的含量测定,所得色谱图见图1,具体测定方法如下:
b1)供试品溶液和对照品溶液的配制
b11)供试品溶液配制
精密称取0.1g芍药甘草汤冻干粉M1(即m芍=0.1g),置10mL量瓶中,加入0.5wt%的氢氧化钠水溶液溶解并稀释至刻度,在40kHz、300W的条件下超声100min,放冷,得溶解液;
精密移取1mL溶解液,置于5mL量瓶中,用乙醇稀释并定容至刻度,摇匀,即得供试品溶液;此时,0.1g芍药甘草汤冻干相当于能够制成的供试品溶液的体积为V试=50mL。
b12)对照品储备液配制
分别取没食子酸、异甘草苷、丹皮酚、芍药内酯苷、芍药苷、芍药内酯B、苯甲酸、柚皮素、苯甲酰芍药苷、芹糖甘草苷、甘草苷、芒柄花黄素、新甘草苷、3'-去氧苏木酮A、异甘草素、甘草素和甘草酸对照品适量,精密称定,用70wt%的乙醇水溶液溶解并稀释制成浓度分别为135.274μg/mL(没食子酸的浓度)、40.125μg/mL(异甘草苷的浓度)、0.415μg/mL(丹皮酚的浓度)、86.249μg/mL(芍药内酯苷的浓度)、318.615μg/mL(芍药苷的浓度)、431.743μg/mL(芹糖甘草苷的浓度)、95.893μg/mL(甘草苷的浓度)、6.124μg/mL(芍药内酯B的浓度)、4.320μg/mL(苯甲酸的浓度)、10.410μg/mL(柚皮素的浓度)、7.920μg/mL(芒柄花黄素的浓度)、6.420μg/mL(新甘草苷的浓度)、8.367μg/mL(3’-去氧苏木酮A的浓度)、7.427μg/mL(异甘草素的浓度)、18.124μg/mL(甘草素的浓度)、173.24μg/mL(苯甲酰芍药苷的浓度)和490.079μg/mL(甘草酸的浓度)的对照品储备液。
b13)不同浓度的对照品标准系列溶液配制
分别精密量取1、2、4、5、8、10mL对照品储备液分别置于50、20、20、20、10、10mL量瓶中,用70wt%乙醇水溶液定容,作为不同浓度的对照品标准系列溶液,其中,不同化学成分的浓度见表1。
b2)高效液相色谱检测
b21)取不同浓度的对照品标准系列溶液在上述色谱条件下进行高效液相色谱检测,得相应化学成分对应浓度测定的峰面积,具体峰面积见表1。
表1不同浓度的对照品标准系列溶液实验结果一览表
其中,检测对照品标准溶液的高效液相色谱条件为:
色谱柱:YMC-Triart C18(5μm,4.6×250mm);
流动相:乙腈(A)-0.1wt%甲酸水溶液(B);
洗脱程序:0~5min,5%→13%流动相A,95%→87%流动相B;
5~15min,13%→23%流动相A,87%→77%流动相B;
15~40min,23%→50%流动相A,77%→50%流动相B;
40~55min,50%→100%流动相A,50%→0%流动相B;
55~55.01min,100%→5%流动相A,0%→95%流动相B;
55.01~65min,5%流动相A,95%流动相B。
流速:0.60mL/min;
柱温:35℃;
检测波长:230nm;
进样量:5μL。
再根据不同化学成分的浓度和相应化学成分对应浓度测定的峰面积,绘制不同化学成分对应的标准曲线,并以不同化学成分的浓度作为横坐标(即x,单位为μg/mL),以相应化学成分对应浓度测定的峰面积作为纵坐标(即y)。
利用不同浓度的对照品标准系列溶液绘制的标准曲线如下:
没食子酸对应的标准曲线为y=7893.9x+10.438,R2=1.000;
异甘草苷对应的标准曲线为y=95117x+8090.5,R2=0.9999;
丹皮酚对应的标准曲线为y=874711x-597.18,R2=1.000;
芍药内酯苷对应的标准曲线为y=4789x-1561.8,R2=0.9995;
芍药苷对应的标准曲线为y=12301x+21868,R2=0.9996;
芹糖甘草苷对应的标准曲线为y=8142.2x-3638.1,R2=0.9993;
甘草苷对应的标准曲线为y=19786x+11017,R2=0.9996;
芍药内酯B对应的标准曲线为y=47442x+629.14,R2=0.9996;
苯甲酸对应的标准曲线为y=106956x-899.14,R2=1.000;
柚皮素对应的标准曲线为y=40543x-1700.9,R2=0.9996;
芒柄花黄素对应的标准曲线为y=40417x-1051.9,R2=0.9994;
新甘草苷对应的标准曲线为y=61161x-1294,R2=0.9998;
3’-去氧苏木酮A对应的标准曲线为y=49390x+298.4,R2=0.9999;
异甘草素对应的标准曲线为y=28818x-272.07,R2=0.9998;
甘草素对应的标准曲线为y=16997x+371.77,R2=0.9998;
苯甲酰芍药苷对应的标准曲线为y=1684.4x-587.75,R2=0.9999;
甘草酸对应的标准曲线为y=5868.1x+14514,R2=0.9995。
b23)取供试品溶液在上述色谱条件下进行高效液相色谱检测,分别得供试品溶液中所含不同化学成分对应的峰面积,将相应化学成分的峰面积代入相应的标准曲线,即得供试品溶液中相应化学成分的浓度(C试-相应化学成分)。
再将供试品溶液中相应化学成分的浓度(C试-相应化学成分)乘以制备的供试品溶液总体积(V试=50mL)除以制备供试品溶液所用芍药甘草汤冻干粉的用量(m芍=0.1g),即得芍药甘草汤中相应化学成分的含量,也就是说芍药甘草汤中相应化学成分的含量=(C对-相应化学成分×V试)/m芍。
以甘草酸为例,即将甘草酸在上述色谱条件下测定的峰面积(A对-甘草酸=436727)代入甘草酸对应的标准曲线,计算得供试品溶液I中甘草酸的浓度(C试-甘草酸=71.95μg/mL);
芍药甘草汤中甘草酸的含量=(C对-甘草酸×VI-甘草酸)/m芍=65.134μg/mL×50mL/0.1g=29606.5μg/g=35.98mg/g。
本实施例中,芍药甘草汤M1中含有没食子酸2.074mg/g、异甘草苷3.321mg/g、丹皮酚0.0058mg/g、芍药内酯苷1.369mg/g、芍药苷52.71mg/g、芍药内酯B 0.1023mg/g、苯甲酸0.0676mg/g、柚皮素0.1529mg/g、苯甲酰芍药苷5.524mg/g、芹糖甘草苷28.64mg/g、甘草苷26.19mg/g、芒柄花黄素0.1217mg/g、新甘草苷0.1034mg/g、3'-去氧苏木酮A0.1426mg/g、异甘草素0.2312mg/g、甘草素0.2628mg/g和甘草酸47.98mg/g。
相当于,本实施例制备芍药甘草汤M1中的成分分析具体见下表:
表2芍药甘草汤中有效成分结果一览表
有效成分 | 有效成分含量(mg/g) | 各有效成分总量 | 提取效率(%) |
没食子酸 | 2.074 | 16.05276 | 0.134 |
异甘草苷 | 3.321 | 25.70454 | 0.214 |
丹皮酚 | 0.0058 | 0.044892 | 0.0004 |
芍药内酯苷 | 1.369 | 10.59606 | 0.0883 |
芍药苷 | 52.71 | 407.9754 | 0.34 |
芹糖甘草苷 | 28.64 | 221.6736 | 1.85 |
甘草苷 | 26.19 | 202.7106 | 1.69 |
芍药内酯B | 0.1023 | 0.791802 | 0.0066 |
苯甲酸 | 0.0676 | 0.523224 | 0.0044 |
柚皮素 | 0.1529 | 1.183446 | 0.0099 |
芒柄花黄素 | 0.1217 | 0.941958 | 0.0078 |
新甘草苷 | 0.1034 | 0.800316 | 0.0067 |
3'-去氧苏木酮A | 0.1426 | 1.103724 | 0.0092 |
异甘草素 | 0.2312 | 1.789488 | 0.0149 |
甘草素 | 0.2628 | 2.034072 | 0.017 |
苯甲酰芍药苷 | 5.524 | 42.75576 | 0.356 |
甘草酸 | 47.98 | 371.3652 | 2.32 |
实施例2~6芍药甘草汤冻干粉的制备方法
实施例2~6分别为一种芍药甘草汤冻干粉的制备方法,它们的步骤与实施例1基本相同,不同之处仅在于原料用量及工艺参数的不同,具体详见表3:
表3实施例2~5中各项工艺参数一览表
实施例2~6其它部分的内容,与实施例1相同。
实验例1含量的测定
对比例1~6为实施例1中芍药甘草汤冻干粉的制备过程的对比试验,且白芍和甘草均与实施例1取自同一批药材,区别仅在于:
对比例1中按照《伤寒论》中记载的“白芍药、甘草各四两,炙。以上二味,以水三升,煮取一升五合,去滓,分温再服”制备白芍和甘草的混合药液,再利用实施例1中的方法浓缩、冷冻干燥,制得5.04芍药甘草汤冻干粉,标记为DM1,干膏率21.00%,芍药甘草汤冻干粉DM1中含有没食子酸1.614mg/g、异甘草苷0.8241mg/g、丹皮酚0.0045mg/g、芍药内酯苷0.8632mg/g、芍药苷41.44mg/g、芍药内酯B 0.0678mg/g、苯甲酸0.0459mg/g、柚皮素0.1042mg/g、苯甲酰芍药苷3.512mg/g、芹糖甘草苷24.12mg/g、甘草苷19.69mg/g、芒柄花黄素0.0798mg/g、新甘草苷0.0657mg/g、3'-去氧苏木酮A 0.0869mg/g、异甘草素0.1534mg/g、甘草素0.1856mg/g和甘草酸29.63mg/g。
没食子酸1.614mg/g、异甘草苷0.8241mg/g、丹皮酚0.0045mg/g、芍药内酯苷0.8632mg/g、芍药苷41.44mg/g、芍药内酯B 0.0678mg/g、苯甲酸0.0459mg/g、柚皮素0.1042mg/g、苯甲酰芍药苷3.512mg/g、芹糖甘草苷24.12mg/g、甘草苷19.69mg/g、芒柄花黄素0.0798mg/g、新甘草苷0.0657mg/g、3'-去氧苏木酮A 0.0869mg/g、异甘草素0.1534mg/g、甘草素0.1856mg/g和甘草酸29.61mg/g。
对比例2中步骤1)仅将85wt%的乙醇水溶液更换为100%乙醇,所得6.86g芍药甘草汤冻干粉,标记为DM2,干膏率28.58%,芍药甘草汤冻干粉DM2中含有没食子酸2.121mg/g、异甘草苷3.314mg/g、丹皮酚0.0062mg/g、芍药内酯苷0.657mg/g、芍药苷34.24mg/g、芍药内酯B 0.8793mg/g、苯甲酸0.0423mg/g、柚皮素0.1293mg/g、苯甲酰芍药苷4.912mg/g、芹糖甘草苷28.38mg/g、甘草苷26.27mg/g、芒柄花黄素0.1224mg/g、新甘草苷0.1021mg/g、3'-去氧苏木酮A 0.1409mg/g、异甘草素0.2321mg/g、甘草素0.2619mg/g和甘草酸47.93mg/g;可以看出,出自白芍的部分有效成分含量明显降低。
对比例3中步骤1)仅将85wt%的乙醇水溶液更换为60wt%的乙醇水溶液,所得6.58g芍药甘草汤冻干粉,标记为DM3,干膏率27.38%,芍药甘草汤冻干粉DM3中含有没食子酸1.0123mg/g、异甘草苷3.327mg/g、丹皮酚0.0041mg/g、芍药内酯苷0.8264mg/g、芍药苷38.71mg/g、芍药内酯B0.9153mg/g、苯甲酸0.0375mg/g、柚皮素0.1497mg/g、苯甲酰芍药苷2.524mg/g、芹糖甘草苷28.72mg/g、甘草苷25.98mg/g、芒柄花黄素0.1231mg/g、新甘草苷0.1042mg/g、3'-去氧苏木酮A0.1410mg/g、异甘草素0.2306mg/g、甘草素0.2617mg/g和甘草酸48.04mg/g;可以看出,出自白芍中的部分有效成分含量明显降低。
对比例4中步骤1)不调节pH值,直接加乙醇水溶液浸泡,所得6.72g芍药甘草汤冻干粉,标记为DM4,干膏率28.00%,芍药甘草汤冻干粉DM4中含有没食子酸1.845mg/g、异甘草苷3.321mg/g、丹皮酚0.0047mg/g、芍药内酯苷1.126mg/g、芍药苷32.69mg/g、芍药内酯B0.0824mg/g、苯甲酸0.0563mg/g、柚皮素0.1392mg/g、苯甲酰芍药苷4.524mg/g、芹糖甘草苷28.69mg/g、甘草苷25.94mg/g、芒柄花黄素0.1236mg/g、新甘草苷0.1029mg/g、3'-去氧苏木酮A 0.1419mg/g、异甘草素0.2324mg/g、甘草素0.2626mg/g和甘草酸47.85mg/g;可以看出,出自白芍中的部分有效成分含量明显降低。
对比例5中步骤1)仅不加盖进行文火煎煮,所得7.09g芍药甘草汤冻干粉,标记为DM5,干膏率29.54%,芍药甘草汤冻干粉DM5中含有没食子酸2.076mg/g、异甘草苷3.325mg/g、丹皮酚0.0007mg/g、芍药内酯苷1.321mg/g、芍药苷49.69mg/g、芍药内酯B 0.1034mg/g、苯甲酸0.0667mg/g、柚皮素0.1534mg/g、苯甲酰芍药苷5.521mg/g、芹糖甘草苷28.72mg/g、甘草苷26.21mg/g、芒柄花黄素0.1214mg/g、新甘草苷0.1039mg/g、3'-去氧苏木酮A0.1424mg/g、异甘草素0.2316mg/g、甘草素0.2625mg/g和甘草酸47.91mg/g;可以看出,出自白芍中的丹皮酚等有效成分含量明显降低。
对比例6中步骤2)中不调节pH值,直接加水浸泡,所得6.96g芍药甘草汤冻干粉,标记为DM6,干膏率29.00%,芍药甘草汤冻干粉DM6中含有没食子酸2.076mg/g、异甘草苷2.672mg/g、丹皮酚0.0057mg/g、芍药内酯苷1.364mg/g、芍药苷52.68mg/g、芍药内酯B0.1026mg/g、苯甲酸0.0678mg/g、柚皮素0.1524mg/g、苯甲酰芍药苷5.531mg/g、芹糖甘草苷22.92mg/g、甘草苷20.71mg/g、芒柄花黄素0.0954mg/g、新甘草苷0.0623mg/g、3'-去氧苏木酮A 0.0324mg/g、异甘草素0.1059mg/g、甘草素0.1379mg/g和甘草酸26.15mg/g;可以看出,出自甘草中的部分有效成分含量明显降低。
显然,所描述的实施例仅仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
Claims (9)
1.一种芍药甘草汤冻干粉的制备方法,其特征在于,所述制备方法包括以下步骤:
取白芍加至浓度为80~90wt%的乙醇水溶液中,调节pH值至6.0~6.5,浸泡后,加盖煎煮,过滤,得白芍药液;
取甘草加至水中,调节pH值至7.2~7.5,浸泡后,煎煮,过滤,得甘草药液;
将白芍药液与甘草药液合并,浓缩后,经冷冻干燥,即得所述芍药甘草汤冻干粉。
2.根据权利要求1所述的芍药甘草汤冻干粉的制备方法,其特征在于,所述乙醇水溶液的用量为白芍的7~8重量倍;水的用量是甘草的8~10重量倍。
3.根据权利要求1或2所述的芍药甘草汤冻干粉的制备方法,其特征在于,所述白芍是采用文火煎煮1.5~2h;所述甘草是采用文火煎煮2~3h。
4.根据权利要求1或2所述的芍药甘草汤冻干粉的制备方法,其特征在于,所述白芍和甘草浸泡的时间均为0.5~1h。
5.根据权利要求1或2所述的芍药甘草汤冻干粉的制备方法,其特征在于,所述浓缩是在60~80℃、-0.08~-0.1MPa条件下进行减压浓缩。
6.根据权利要求1或2所述的芍药甘草汤冻干粉的制备方法,其特征在于,浓缩后且冷冻干燥前,所述浓缩液与白芍和甘草的总重量比为1.8~2.2:1。
7.根据权利要求1或2所述的芍药甘草汤冻干粉的制备方法,其特征在于,所述冷冻干燥是先在-30~-45℃预冻至少60min,再于-40~-70℃真空干燥至少12h。
8.根据权利要求7所述的芍药甘草汤冻干粉的制备方法,其特征在于,真空干燥的真空度<100Pa。
9.根据权利要求1或2所述的芍药甘草汤冻干粉的制备方法,其特征在于,所述白芍与甘草的重量比为1:1。
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102204951A (zh) * | 2011-05-24 | 2011-10-05 | 药都制药集团股份有限公司 | 从甘草中提取有效成分的方法 |
CN112773831A (zh) * | 2020-12-21 | 2021-05-11 | 贵州景诚制药有限公司 | 一种芍药甘草药物组合物的制备方法及其检测方法 |
CN113230316A (zh) * | 2021-06-04 | 2021-08-10 | 郑州大学 | 芍药甘草汤制剂在防治肿瘤疾病中的应用 |
CN113820422A (zh) * | 2021-09-24 | 2021-12-21 | 宁波立华制药有限公司 | 一种白芍总苷指纹图谱检测方法 |
CN114376952A (zh) * | 2021-12-31 | 2022-04-22 | 浙江大学 | 一种芍药花提取物及其制备方法和应用 |
-
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102204951A (zh) * | 2011-05-24 | 2011-10-05 | 药都制药集团股份有限公司 | 从甘草中提取有效成分的方法 |
CN112773831A (zh) * | 2020-12-21 | 2021-05-11 | 贵州景诚制药有限公司 | 一种芍药甘草药物组合物的制备方法及其检测方法 |
CN113230316A (zh) * | 2021-06-04 | 2021-08-10 | 郑州大学 | 芍药甘草汤制剂在防治肿瘤疾病中的应用 |
CN113820422A (zh) * | 2021-09-24 | 2021-12-21 | 宁波立华制药有限公司 | 一种白芍总苷指纹图谱检测方法 |
CN114376952A (zh) * | 2021-12-31 | 2022-04-22 | 浙江大学 | 一种芍药花提取物及其制备方法和应用 |
Non-Patent Citations (2)
Title |
---|
不同评价指标对芍药甘草汤提取工艺优化的影响;杜平等;中成药;第40卷(第10期);第2188-2193页 * |
芍药甘草汤HPLC指纹图谱的建立和7种成分含量测定;何利等;中药材;第42卷(第08期);第1837-1841页 * |
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