CN116159095B - 当归六黄汤冻干粉的制备方法 - Google Patents
当归六黄汤冻干粉的制备方法 Download PDFInfo
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- CN116159095B CN116159095B CN202310054873.XA CN202310054873A CN116159095B CN 116159095 B CN116159095 B CN 116159095B CN 202310054873 A CN202310054873 A CN 202310054873A CN 116159095 B CN116159095 B CN 116159095B
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- angelica
- decoction
- radix
- yellow
- extraction
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Classifications
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Abstract
本发明提供一种当归六黄汤冻干粉的制备方法,属于中药制剂技术领域,所述制备方法是将当归以乙醇水溶液超声提取,生地黄、熟地黄和黄芪以乙醇水溶液渗漉提取,黄芩以乙酸水溶液煎煮提取,黄柏和黄连以磷酸盐缓冲液煎煮提取,各步提取所得溶液混匀后,各步提取所得药液与环糊精依特定顺序混匀后,减压浓缩、冻干,即得所述当归六黄汤冻干粉。本发明依据中药材特性分类进行提取,有效防止各味中药材中的有效成分在溶出过程中发生反应形成不溶性复合物,提高不同有效成分的提取率,进而提高出膏率。
Description
技术领域
本发明涉及中药冻干粉的制备,尤其涉及一种当归六黄汤冻干粉的制备方法。
背景技术
当归六黄汤出自金·李东垣编撰的《兰室秘藏》,主治阴虛火旺之盗汗证。后世医家以本方为基础加上各自见解,并根据临床具体症状辩证论治,进行加减化裁,临床应用颇广,涉及现代医学的各个系统疾病,如病毒性心肌炎、肺结核、痢疾、甲状腺功能亢进、糖尿病、肾病综合征、精神分裂症、自身免疫系统疾病、皮肤病、慢性口腔溃疡、围绝经期综合征、人工流产后阴道出血、心律失常以及慢性前列腺炎等方面。
金·李东垣《兰室秘藏》中记载“当归、生地黄、熟地黄、黄芩、黄连、黄柏各等分,黄芪加倍。上为粗末,每服五钱,水两盏,煎至一盏,食前服,小儿减半服之”。然而,该法在煎制过程中,由于成分复杂,部分成分可能在配伍煎煮时发生反应,导致有效成分提取率降低。有研究发现黄芩苷、汉黄芩苷、阿魏酸等在煎煮过程中,都能与小檗碱形成不溶性复合物,这些不溶性复合物会随药渣过滤一并去除,导致所得产品中有效成分含量降低。同时,当归、黄芩和黄芪中主要成分之一为酸性化合物,而黄连和黄柏的主要成分之一则为生物碱,依据化学反应规律,在煎煮过程中这些酸性成分和碱性成分也会发生反应,导致配伍前后化学成分发生明显变化形成不溶性复合物,随药渣过滤去除,进一步导致所得产品中有效成分含量降低。
发明内容
针对上述问题,本发明提供一种当归六黄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:
一种当归六黄汤冻干粉的制备方法,包括以下步骤:
1)取当归采用乙醇水溶液浸渍后,超声提取,得当归提取液;
取生地黄、熟地黄和黄芪,采用乙醇水溶液浸渍后,渗漉提取,得三黄提取液;
取黄芩经提取挥发油后,得黄芩挥发油和黄芩药渣;
黄芩药渣经乙酸水溶液浸泡后,煎煮,得黄芩煎煮液;
黄柏和黄连经提取挥发油后,得二黄挥发油和二黄药渣;
二黄药渣经磷酸盐缓冲液浸泡后,煎煮,得二黄煎煮液;
2)取二黄煎煮液加入环糊精混匀后,加入黄芩煎煮液和三黄提取液,再加入黄芩挥发油和二黄挥发油,最后加入当归提取液,混匀,减压浓缩至无醇味,冻干,即得所述当归六黄汤冻干粉。
进一步的,在步骤1)所述当归提取液提取过程中,所用乙醇水溶液的浓度为90~92wt%、pH为4.5~5.5。
进一步的,在步骤1)所述三黄提取液提取过程中,所用乙醇水溶液的浓度为50~55wt%、pH为5.0~5.5。
进一步的,在步骤1)所述黄芩煎煮液煎煮过程中,所用的乙酸水溶液的pH为3.30~3.38。
进一步的,在步骤1)所述二黄煎煮液煎煮过程中,所用磷酸盐缓冲液的pH为5.8~6.0。
进一步的,在步骤1)所述当归提取液提取过程中,超声提取的温度为40~45℃、频率为30~35Hz、时间为25~35min。
进一步的,在步骤1)所述三黄提取液提取过程中,浸渍的时间为24~28h。
进一步的,所述当归、生地黄、熟地黄、黄芪、黄芩、黄柏、黄连与环糊精的重量比为1:1:1:1:1:1:1:0.07~0.08。
进一步的,在步骤1)所述当归提取液提取过程中,所用乙醇水溶液的用量为当归重量的6~8倍;
所述三黄提取液提取过程中,浸渍所用乙醇水溶液的用量为生地黄、熟地黄和黄芪三味药材总重量的6~8倍;
所述黄芩煎煮液煎煮过程中,所用乙酸水溶液的用量为黄芩重量的5~6倍;
所述二黄煎煮液煎煮过程中,所用磷酸盐缓冲液的用量为黄柏和黄连总重量的5~6倍。
进一步的,在步骤1)所述当归提取液提取过程中,所用乙醇水溶液中含有HCl;
所述三黄提取液提取过程中,所用乙醇水溶液中含有HCl;
所述黄芩药渣利用乙酸水溶液浸泡的时间为1~2h,煎煮的时间为1~1.5h;
所述二黄药渣利用磷酸水溶液浸泡的时间为1~2h,煎煮的时间为1~1.5h。
本发明的当归六黄汤冻干粉的制备方法的有益效果为:
本发明依据中药材特性分类进行提取,有效避免各味中药材中的有效成分在溶出过程中发生反应形成不溶性复合物(比如黄芩苷、汉黄芩苷、阿魏酸在直接提取过程中会与小檗碱形成不溶性复合物,进而影响提取率),从而提高不同有效成分的提取率,进而提高出膏率;
本发明采用特定pH和浓度的乙醇水溶液对当归在特定温度下进行超声提取,即能很好提取出挥发油、阿魏酸、绿原酸、环烯萜醚类等有效成分,又能抑制阿魏酸、绿原酸等成分受温度和pH值影响分解;
本发明采用特定pH和浓度的乙醇水溶液对生地黄、熟地黄和黄芪进行渗漉提取,能够充分提取出小檗碱、环烯醚萜甙类、环烯醚匝类、毛蕊异黄酮葡萄糖苷、毛蕊花糖苷等有效成分,并能够抑制毛蕊异黄酮葡萄糖苷、毛蕊花糖苷受温度、pH等影响分解;
本发明通过对黄芩经提取挥发油后,再单独采用特定pH的乙酸水溶液进行煎煮,能够充分提取黄芩中黄芩苷、汉黄芩苷、黄芩素、汉黄芩素等有效成分;
本发明通过对黄柏和黄连提取挥发油后,采用特定pH的磷酸盐缓冲液进行煎煮,能够有效提取出小檗碱、黄连碱、表小檗碱、木兰花碱、黄柏碱等有效成分;
本发明通过在黄柏和黄连煎煮所得二黄煎煮液中加入β-环糊精后,再加入其它提取所得药液及挥发油,能够抑制呈现不同酸碱特性的有效成分之间相互反应形成沉淀,同时β-环糊精还能够包裹挥发油,提高所含挥发油的稳定性,防止挥发油在后续浓缩和冻干过程中挥发。
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1一种当归六黄汤冻干粉的制备方法
本实施例为一种当归六黄汤冻干粉的制备方法,具体合成过程包括以下步骤:
1)有效成分提取
11)取10kg当归采用70kg含HCl且pH=5.0、浓度为92wt%的乙醇水溶液浸渍1.5h后,在40℃、35Hz条件下超声提取30min,得当归提取液;
12)取10kg生地黄、10kg熟地黄和20kg黄芪混合,采用280kg含HCl且pH=5.2、浓度为52wt%的乙醇水溶液浸渍24h后,按2mL/min/kg的速度进行渗漉提取,得三黄提取液;
13)取10kg黄芩经水蒸气提取挥发油后,得黄芩挥发油和黄芩药渣;
所得黄芩药渣采用70kg的pH=3.35的乙酸水溶液浸泡1.5h后,煎煮1h,得黄芩煎煮液;
14)以10L浓度为0.2mol/L的磷酸氢二钠与90L浓度为0.2mol/L的磷酸二氢钠混合,制得pH=5.9的磷酸盐缓冲液;
取10kg黄柏与10kg黄连混合,经水蒸气提取挥发油后,得二黄挥发油和二黄药渣;
所得二黄药渣经100kg的pH=5.9的磷酸盐缓冲液浸泡1.5h后,煎煮1h,得二黄煎煮液;
2)冻干粉制备
取二黄煎煮液加入0.75kg的β-环糊精搅拌均匀(β-环糊精完全溶解),再依次加入黄芩煎煮液、三黄提取液再次搅拌均匀,然后滴加黄芩挥发油和二黄挥发油,边滴加边搅拌至混匀,最后加入当归提取液搅拌混匀,所得药液经减压浓缩至无醇味后,冻干,即得40.52kg当归六黄汤冻干粉,标记为M1,出膏率为56.81%。
当归六黄汤冻干粉M1中含有黄芩苷17.65mg/g、小檗碱21.03mg/g、黄柏碱1.24mg/g、阿魏酸0.61mg/g、表小檗碱2.53mg/g、黄连碱3.87mg/g、巴马汀2.92mg/g。
其中,出膏率(%)=干膏量/投药量×100%;
干膏量=当归六黄汤冻干粉重量-辅料重量,辅料为β-环糊精。
其中,黄芩苷、小檗碱、黄柏碱、阿魏酸的含量依据《当归六黄汤UPLC指纹图谱的建立及4种成分的含量测定》(曾杉等,广东药科大学学报,2022,38(02))进行测定;
表小檗碱、黄连碱、巴马汀的含量依据《当归六黄汤合煎与单煎质量表征及其抗阴虚甲亢作用研究》(闫妍,硕士学位论文,长春中医药大学,2022年3月)。
实施例2~6当归六黄汤冻干粉的制备方法
实施例2~6分别为一种当归六黄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1:
表1实施例2~6中各项工艺参数一览表
其中,pH=5.8的磷酸盐缓冲液是以8L浓度为0.2mol/L的磷酸氢二钠与92L浓度为0.2mol/L的磷酸二氢钠混合制得;
pH=5.9的磷酸盐缓冲液是以10L浓度为0.2mol/L的磷酸氢二钠与90L浓度为0.2mol/L的磷酸二氢钠混合制得;
pH=6.0的磷酸盐缓冲液是以12.3L浓度为0.2mol/L的磷酸氢二钠与87.7L浓度为0.2mol/L的磷酸二氢钠混合制得;
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1~12为实施例1中当归六黄汤冻干粉的制备过程的对比试验,且当归、生地黄、熟地黄、黄芪、黄芩、黄柏、黄连均与实施例1取自同一批药材,区别仅在于:
对比例1的步骤2)中,不添加β-环糊精,直接混匀冻干,得37.68kg当归六黄汤冻干粉,标记为DM1,出膏率为52.76%。当归六黄汤冻干粉DM1中含有黄芩苷17.62mg/g、小檗碱21.00mg/g、黄柏碱1.23mg/g、阿魏酸0.60mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,在各提取工艺不变的前提下,测定的各有效成分含量变化不大,但当归六黄汤冻干粉总量明显降低。这可能是由于制备冻干粉过程中,浓缩和冻干过程导致部分挥发油挥发。
对比例2的步骤11)中仅将乙醇水溶液的浓度更换为80wt%,得37.72g当归六黄汤冻干粉,标记为DM2,干膏率52.81%。当归六黄汤冻干粉DM2中含有黄芩苷17.62mg/g、小檗碱20.99mg/g、黄柏碱1.23mg/g、阿魏酸0.49mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量和阿魏酸含量均有所降低,可能是由于当归提取过程中有效成分无法完全提取出(本领域技术人员均知道,当归中含有阿魏酸)。
对比例3的步骤11)中仅将92wt%乙醇水溶液更换为100%乙醇,得38.12g当归六黄汤冻干粉,标记为DM3,干膏率53.39%。当归六黄汤冻干粉DM3中含有黄芩苷17.62mg/g、小檗碱21.00mg/g、黄柏碱1.23mg/g、阿魏酸0.52mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量和阿魏酸含量依然有所降低,可能是由于当归提取过程中有效成分无法完全提取出(本领域技术人员均知道,当归中含有阿魏酸)。
对比例4的步骤11)中仅将乙醇水溶液的pH更换为6.5,得38.23g当归六黄汤冻干粉,标记为DM4,干膏率53.54%。当归六黄汤冻干粉DM4中含有黄芩苷17.62mg/g、小檗碱21.01mg/g、黄柏碱1.23mg/g、阿魏酸0.54mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量和阿魏酸含量均有所降低,可能是由于当归提取过程中有效成分无法完全提取出(本领域技术人员均知道,当归中含有阿魏酸)。
对比例5的步骤11)中仅将乙醇水溶液的pH更换为3.5,得38.42g当归六黄汤冻干粉,标记为DM5,干膏率53.81%。当归六黄汤冻干粉DM5中含有黄芩苷17.63mg/g、小檗碱21.01mg/g、黄柏碱1.23mg/g、阿魏酸0.53mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量和阿魏酸含量均有所降低,可能是由于当归提取过程中有效成分无法完全提取出(本领域技术人员均知道,当归中含有阿魏酸)。
对比例6的步骤12)中仅将乙醇水溶液的浓度更换为40wt%,得36.21g当归六黄汤冻干粉,标记为DM6,干膏率50.66%。当归六黄汤冻干粉DM6中含有黄芩苷17.58mg/g、小檗碱20.98mg/g、黄柏碱1.24mg/g、阿魏酸0.62mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.92mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量有所降低,可能是由于生地黄、熟地黄和黄芪提取过程中有效成分无法完全提取出部分有效成分(比如黄芪中含有的黄芪甲苷)。
对比例7的步骤12)中仅将乙醇水溶液的浓度更换为65wt%,得36.43g当归六黄汤冻干粉,标记为DM7,干膏率50.97%。当归六黄汤冻干粉DM7中含有黄芩苷17.61mg/g、小檗碱20.97mg/g、黄柏碱1.23mg/g、阿魏酸0.61mg/g、表小檗碱2.52mg/g、黄连碱3.87mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量有所降低,可能是由于生地黄、熟地黄和黄芪提取过程中有效成分无法完全提取出部分有效成分(比如黄芪中含有的黄芪甲苷)。
对比例8的步骤12)中仅将乙醇水溶液的pH更换为4.0,得36.38g当归六黄汤冻干粉,标记为DM8,干膏率50.90%。当归六黄汤冻干粉DM8中含有黄芩苷17.59mg/g、小檗碱20.94mg/g、黄柏碱1.24mg/g、阿魏酸0.62mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量有所降低,可能是由于生地黄、熟地黄和黄芪提取过程中有效成分无法完全提取出部分有效成分(比如黄芪中含有的黄芪甲苷)。
对比例9的步骤12)中仅将乙醇水溶液的pH更换为6.5,得37.21g当归六黄汤冻干粉,标记为DM9,干膏率52.09%。当归六黄汤冻干粉DM9中含有黄芩苷17.61mg/g、小檗碱20.99mg/g、黄柏碱1.23mg/g、阿魏酸0.61mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.91mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量有所降低,可能是由于生地黄、熟地黄和黄芪提取过程中有效成分无法完全提取出部分有效成分(比如黄芪中含有的黄芪甲苷)。
对比例10的步骤13)中仅将乙酸水溶液更换为水,得38.19g当归六黄汤冻干粉,标记为DM10,干膏率53.49%。当归六黄汤冻干粉DM10中含有黄芩苷15.23mg/g、小檗碱21.01mg/g、黄柏碱1.24mg/g、阿魏酸0.60mg/g、表小檗碱2.52mg/g、黄连碱3.85mg/g、巴马汀2.92mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量和黄芩苷含量均有所降低,可能是由于黄芩提取过程中有效成分无法完全提取出(本领域技术人员均知道,黄芩中含有黄芩苷)。
对比例11的步骤13)中仅将乙酸水溶液的pH更换为2.38,得38.47g当归六黄汤冻干粉,标记为DM11,干膏率53.89%。当归六黄汤冻干粉DM11中含有黄芩苷16.32mg/g、小檗碱21.01mg/g、黄柏碱1.24mg/g、阿魏酸0.61mg/g、表小檗碱2.52mg/g、黄连碱3.86mg/g、巴马汀2.92mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量和黄芩苷含量均有所降低,可能是由于黄芩提取过程中有效成分无法完全提取出(本领域技术人员均知道,黄芩中含有黄芩苷)。
对比例12的步骤14)中仅将磷酸盐缓冲液更换为水,得37.87g当归六黄汤冻干粉,标记为DM12,干膏率53.03%。当归六黄汤冻干粉DM12中含有黄芩苷17.63mg/g、小檗碱19.25mg/g、黄柏碱0.87mg/g、阿魏酸0.61mg/g、表小檗碱1.88mg/g、黄连碱3.02mg/g、巴马汀2.21mg/g。可以看到,与实施例1相比,当归六黄汤冻干粉总量、小檗碱、黄柏碱、表小檗碱、黄连碱、巴马汀含量均有所降低,可能是由于黄柏和黄连提取过程中有效成分无法完全提取出(本领域技术人员均知道,黄柏中含有小檗碱和黄柏碱,黄连中含有小檗碱、表小檗碱、黄连碱和巴马汀)。
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 (5)
1.一种当归六黄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:
1)取当归采用乙醇水溶液浸渍后,超声提取,得当归提取液;
在所述当归提取液提取过程中,所用乙醇水溶液的浓度为90~92wt%、pH为4.5~5.5,所用乙醇水溶液中含有HCl;超声提取的温度为40~45℃、频率为30~35Hz、时间为25~35min;
取生地黄、熟地黄和黄芪,采用乙醇水溶液浸渍后,渗漉提取,得生地黄、熟地黄和黄芪提取液;
在所述生地黄、熟地黄和黄芪提取液提取过程中,所用乙醇水溶液的浓度为50~55wt%、pH为5.0~5.5,所用乙醇水溶液中含有HCl;
取黄芩经提取挥发油后,得黄芩挥发油和黄芩药渣;
黄芩药渣经乙酸水溶液浸泡后,煎煮,得黄芩煎煮液;
在所述黄芩煎煮液煎煮过程中,所用的乙酸水溶液的pH为3.30~3.38;
黄柏和黄连经提取挥发油后,得黄柏和黄连挥发油和黄柏和黄连药渣;
黄柏和黄连药渣经磷酸盐缓冲液浸泡后,煎煮,得黄柏和黄连煎煮液;
在所述黄柏和黄连煎煮液煎煮过程中,所用磷酸盐缓冲液的pH为5.8~6.0;
2)取黄柏和黄连煎煮液加入环糊精混匀后,加入黄芩煎煮液和生地黄、熟地黄和黄芪提取液,再加入黄芩挥发油和黄柏和黄连挥发油,最后加入当归提取液,混匀,减压浓缩至无醇味,冻干,即得所述当归六黄汤冻干粉。
2.根据权利要求1所述的当归六黄汤冻干粉的制备方法,其特征在于,在步骤1)所述生地黄、熟地黄和黄芪提取液提取过程中,浸渍的时间为24~28h。
3.根据权利要求1所述的当归六黄汤冻干粉的制备方法,其特征在于,所述当归、生地黄、熟地黄、黄芪、黄芩、黄柏、黄连与环糊精的重量比为1:1:1:1:1:1:1:0.07~0.08。
4.根据权利要求1所述的当归六黄汤冻干粉的制备方法,其特征在于,
在步骤1)所述当归提取液提取过程中,所用乙醇水溶液的用量为当归重量的6~8倍;
所述生地黄、熟地黄和黄芪提取液提取过程中,浸渍所用乙醇水溶液的用量为生地黄、熟地黄和黄芪三味药材总重量的6~8倍;
所述黄芩煎煮液煎煮过程中,所用乙酸水溶液的用量为黄芩重量的5~6倍;
所述黄柏和黄连煎煮液煎煮过程中,所用磷酸盐缓冲液的用量为黄柏和黄连总重量的5~6倍。
5.根据权利要求1所述的当归六黄汤冻干粉的制备方法,其特征在于,
在步骤1)
所述黄芩药渣利用乙酸水溶液浸泡的时间为1~2h,煎煮的时间为1~1.5h;
所述黄柏和黄连药渣利用磷酸水溶液浸泡的时间为1~2h,煎煮的时间为1~1.5h。
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