CN104147096A - Preparation method for licorice fluid extract - Google Patents

Preparation method for licorice fluid extract Download PDF

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Publication number
CN104147096A
CN104147096A CN201410401548.7A CN201410401548A CN104147096A CN 104147096 A CN104147096 A CN 104147096A CN 201410401548 A CN201410401548 A CN 201410401548A CN 104147096 A CN104147096 A CN 104147096A
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China
Prior art keywords
concentration
filtrate
ethanol
time
radix glycyrrhizae
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Pending
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CN201410401548.7A
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Chinese (zh)
Inventor
汪海博
李亚林
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BAOJI JINSEN PHARMACEUTICAL Co Ltd
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BAOJI JINSEN PHARMACEUTICAL Co Ltd
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Priority to CN201410401548.7A priority Critical patent/CN104147096A/en
Publication of CN104147096A publication Critical patent/CN104147096A/en
Pending legal-status Critical Current

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Abstract

The invention provides a preparation method for licorice fluid extract. The method comprises the following steps: material dissolving; dissolving with alcohol; press filtration; squeezing; concentration; blending; and filling and sealing. Compared with a traditional ternary alcohol precipitation process, the preparation method for the licorice fluid extract provided by the invention has the following advantages: a production cycle is shortened to 6 d from original 12 d, production cost is greatly reduced, and the disadvantages of decrease and instability of a pH value in the traditional process are overcome through repeated adjusting of the pH value.

Description

A kind of preparation method of Radix Glycyrrhizae fluidextract
Technical field
The invention belongs to Chinese medicine extraction technical field, be specifically related to a kind of preparation method of Radix Glycyrrhizae fluidextract.
Background technology
Radix Glycyrrhizae fluidextract is the fluid extract that the glycyrrhizic acid in Radix Glycyrrhizae extractum is made through alcohol extraction, is a kind of obtundent, normal and preventing phlegm from forming and stopping coughing medicine compatibility application.Traditional preparation method adopts three alcohol precipitation processes, and the production cycle reaches 12 days, and production cost is high.And the Radix Glycyrrhizae fluidextract that traditional preparation method is produced exists pH value to decline and unsettled drawback.
Summary of the invention
The invention provides a kind of preparation method of Radix Glycyrrhizae fluidextract, compared with traditional three alcohol precipitation processes, the production cycle was shortened to 6 days by original 12 days, significantly reduce production cost low, and by re-adjustments pH value, solve traditional handicraft pH value and declined and unsettled drawback.
Technical solution of the present invention: a kind of preparation method of Radix Glycyrrhizae fluidextract, comprises following processing step: material: extracting liquorice extractum adds appropriate pure water and is heated to micro-boiling, fully dissolves Radix Glycyrrhizae extractum and obtains lysate and filter;
Alcohol is molten: in the lysate after filtration, slowly adding concentration is that 85% ethanol obtains mixed liquor, make ethanol content in feed liquid reach 63-66%, in mixed liquor, add kieselguhr mix homogeneously by the 0.15-0.25 of a Radix Glycyrrhizae extractum consumption times weight ratio again, extract at room temperature 90 ± 10 minutes.
Filter pressing: above-mentioned feed liquid is carried out to filter pressing and obtain filtrate for the first time, and the alcohol flushing twice that is 65% by concentration again to the filter cake forming, after twice flushing liquor filtered, merge and obtain filtrate for the second time;
Squeezing: the filter cake rinsing is squeezed, and pressed liquor is filtered and obtains filtrate for the third time;
Concentrated: for the first time filtrate, for the second time filtrate, filtrate merges post-heating to 80~90 DEG C and concentrates for the third time, makes the proportion of 60 DEG C of concentrated solutions reach 1.15-1.20;
Tune is converted: measure glycyrrhizic acid content and the ethanol content of concentrated solution, add pure water and ethanol, make glycyrrhizic acid content >=1.8g/100ml, ethanol content is between 20.0-25.0%; And then the medicinal ammonia adjusting pH value that interpolation concentration is 25.0-28.0% is between 8.3-8.5, leaves standstill after 36-48 hour, to obtain adjusting and converts liquid; Measure to adjust and convert the pH value of liquid, the medicinal ammonia that again adds concentration and be 25.0-28.0% regulates pH value between 8.2-8.4, gets its supernatant and obtains finished fluid;
Embedding: filling and sealing after finished fluid is filtered.
When converting, adds tune the ethanol that concentration is 70-75%.
The advantage that the present invention has compared with traditional handicraft and effect:
1, the production cycle was shortened to 6 days by original 12 days, significantly reduced production cost low;
2,, by re-adjustments pH value, solved traditional handicraft pH value decline and unsettled
Drawback;
3, realize cyclic production, further reduced production cost, saved resource, reduced discharge, protection of the environment.
4, simple to operate, be suitable for industrialized great production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
The first step: material.Extracting liquorice extractum raw material 550kg adds material pot, adds pure water 550kg by 1:1 weight ratio, be heated to micro-boiling and Radix Glycyrrhizae extractum fully dissolved obtain lysate, and by lysate with adding the molten tank of alcohol after 20 eye mesh screens filtrations.
Second step: alcohol is molten.Add to the molten tank of alcohol the ethanol 4950L that the concentration of 9 times of amounts of Radix Glycyrrhizae extractum consumption is 85%, measure with alcohol meter, make ethanol content in feed liquid reach 65%, add again the kieselguhr 110kg of 0.2 times of weight ratio of Radix Glycyrrhizae extractum consumption, after being uniformly mixed, open circulation valve, make lysate extract at room temperature in the molten tank of alcohol after 90 minutes.
The 3rd step: filter pressing.Above-mentioned feed liquid is sent into diaphragm filter press (500 order filter cloth) filter pressing and obtain filtrate for the first time, and filtrate adds fluid reservoir for the first time.Follow that double to send into respectively concentration to diaphragm filter press (500 order filter cloth) be that the filter cake that 65% ethanol 825L forms filter pressing rinses twice, and twice flushing liquor merged after filter pressing and obtain filtrate for the second time respectively, and filtrate adds fluid reservoir for the second time.When filter pressing, oil cylinder of filter press pressure is 15-20Mpa.
The 4th step: squeezing.Then send into diaphragm filter press (500 order filter cloth) compressed air that pressure is 0.10-0.70Mpa, maintain 120 minutes, the filter cake rinsing is squeezed and obtains filtrate for the third time, and filtrate adds fluid reservoir for the third time.When squeezing, oil cylinder of filter press pressure is 15-20Mpa.
The 5th step: concentrated.Filtrate in fluid reservoir is proceeded to concentration pan, be heated to 80~90 DEG C and concentrate and reclaim ethanol, measure when concentrated solution proportion reaches 1.15-1.20 and concentrated at 60 DEG C.The concentration of alcohol of concentration and recovery is 70-75%.
The 6th step: adjust and convert.Concentrated solution is proceeded to adjust and convert tank, stir 60 minutes mix homogeneously, after the glycyrrhizic acid content of sampling and measuring concentrated solution, the ethanol that the concentration of adding pure water and recovery is 70-75%, the content of glycyrrhizic acid and ethanol is all conformed with the regulations, be glycyrrhizic acid content >=1.8g/100ml, ethanol content (volume ratio) is between 20-25%.And then the medicinal ammonia adjusting pH value that interpolation concentration is 25.0-28.0% is between 8.3-8.5, leaves standstill after 36 hours, to obtain adjusting and converts liquid; Measure to adjust and convert the pH value of liquid, the medicinal ammonia that again adds concentration and be 25-28% regulates pH value between 8.2-8.4, gets its supernatant and obtains finished fluid.
The 7th step: embedding.Filling and sealing after finished fluid is filtered.
After alcohol of the present invention is molten, directly filter pressing, shortened to 6 days by the production cycle by original 12 days, had significantly reduced production cost low.The present invention adopts ethanol that the concentration of recovery is 70-75% to adjust and converts, and has realized cyclic production, has further reduced production cost, has saved resource, reduces discharge, protection of the environment.In addition, due to tune, to convert pot liquid temperature higher, makes medicinal ammonia and glycyrrhizic acid response speed very fast, so after 36 hours, pH value can be reduced between 7.9-8.2, must be by re-adjustments pH value, and could solve the decline of traditional handicraft pH value and unsettled drawback.
It is 40 DEG C that the Radix Glycyrrhizae fluidextract that the Radix Glycyrrhizae fluidextract that the present invention is produced and traditional handicraft are produced is put into temperature simultaneously, and humidity is under 75% environment, to do to accelerate experiment, measures its pH value, and its result is as follows:
Can be found out by above data, the pH value stability of the Radix Glycyrrhizae fluidextract that the present invention produces has increased significantly than traditional handicraft, and other index all meets pharmacopeia regulation.
Above-described embodiment, is preferred embodiment of the present invention, is not used for limiting the scope of the present invention, thus all equivalent variations of being done with content described in the claims in the present invention, within all should being included in the claims in the present invention scope.

Claims (2)

1. a preparation method for Radix Glycyrrhizae fluidextract, is characterized in that comprising following processing step:
Material: extracting liquorice extractum adds appropriate pure water and is heated to micro-boiling, fully dissolves Radix Glycyrrhizae extractum and obtains lysate and filter;
Alcohol is molten: in the lysate after filtration, slowly adding concentration is that 85% ethanol obtains mixed liquor, make ethanol content in feed liquid reach 63-66%, in mixed liquor, add kieselguhr mix homogeneously by the 0.15-0.25 of a Radix Glycyrrhizae extractum consumption times weight ratio again, extract at room temperature 90 ± 10 minutes.
Filter pressing: above-mentioned feed liquid is carried out to filter pressing and obtain filtrate for the first time, and the alcohol flushing twice that is 65% by concentration again to the filter cake forming, after twice flushing liquor filtered, merge and obtain filtrate for the second time;
Squeezing: the filter cake rinsing is squeezed, and pressed liquor is filtered and obtains filtrate for the third time;
Concentrated: for the first time filtrate, for the second time filtrate, filtrate merges post-heating to 80~90 DEG C and concentrates for the third time, makes the proportion of 60 DEG C of concentrated solutions reach 1.15-1.20;
Tune is converted: measure glycyrrhizic acid content and the ethanol content of concentrated solution, add pure water and ethanol, make glycyrrhizic acid content >=1.8g/100ml, ethanol content is between 20.0-25.0%; And then the medicinal ammonia adjusting pH value that interpolation concentration is 25.0-28.0% is between 8.3-8.5, leaves standstill after 36-48 hour, to obtain adjusting and converts liquid; Measure to adjust and convert the pH value of liquid, the medicinal ammonia that again adds concentration and be 25.0-28.0% regulates pH value between 8.2-8.4, gets its supernatant and obtains finished fluid;
Embedding: filling and sealing after finished fluid is filtered.
2. the preparation method of a kind of Radix Glycyrrhizae fluidextract as claimed in claim 1, is characterized in that: tune adds the ethanol that concentration is 70-75% while converting.
CN201410401548.7A 2014-08-15 2014-08-15 Preparation method for licorice fluid extract Pending CN104147096A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107412318A (en) * 2017-06-02 2017-12-01 新疆全泰兴药业科技有限公司 A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2155061C1 (en) * 1999-08-09 2000-08-27 Открытое Акционерное Общество "Фармацевтическая Фабрика Санкт-Петербурга" Preparation, radioprotective, general tonic and antiinflammatory drugs and method of their preparing
CN102166252A (en) * 2010-02-26 2011-08-31 太极集团重庆涪陵制药厂有限公司 Method of extracting dilute alcohol soluble substance from liquorice dry extract

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2155061C1 (en) * 1999-08-09 2000-08-27 Открытое Акционерное Общество "Фармацевтическая Фабрика Санкт-Петербурга" Preparation, radioprotective, general tonic and antiinflammatory drugs and method of their preparing
CN102166252A (en) * 2010-02-26 2011-08-31 太极集团重庆涪陵制药厂有限公司 Method of extracting dilute alcohol soluble substance from liquorice dry extract

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
济南部队后勤部卫生部: "《药局技术操作手册》", 31 March 1982, 山东科学技术出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107412318A (en) * 2017-06-02 2017-12-01 新疆全泰兴药业科技有限公司 A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound

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