CN106349240A - Technique for extracting fibrauretine by using mixed solvent - Google Patents
Technique for extracting fibrauretine by using mixed solvent Download PDFInfo
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- CN106349240A CN106349240A CN201610729907.0A CN201610729907A CN106349240A CN 106349240 A CN106349240 A CN 106349240A CN 201610729907 A CN201610729907 A CN 201610729907A CN 106349240 A CN106349240 A CN 106349240A
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- mixed solvent
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- fibrauretin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D455/00—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
- C07D455/03—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing quinolizine ring systems directly condensed with at least one six-membered carbocyclic ring, e.g. protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
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Abstract
The invention discloses a technique for extracting fibrauretine by using a mixed solvent. The technique aims to enhance the fibrauretine extraction rate, shorten the extraction time and enhance the production efficiency; and the filtrate can be easily filtered, thereby reducing the number of times of cleaning the filter screen by the workers, lowering the labor intensity, reducing the acid water consumption, and also reducing the sodium chloride consumption and sewage treatment quantity. The technical scheme is as follows: extracting herba fibraureae recisae powder by using a mixed solvent, merging the filtrates, cooling, and filtering to remove insoluble impurities; concentrating and filtering the filtrate; regulating the filtrate to an alkaline state, standing to precipitate insoluble substances, filtering, adding sodium chloride into the filtrate to perform salting-out, and filtering to obtain a crude product; dissolving the crude product with ethanol by heating, and filtering while the solution is hot to remove insoluble impurities; and after the filtrate becomes cool, slowly adding concentrated hydrochloric acid to precipitate palmatine hydrochloride, filtering, and drying to obtain the product.
Description
Technical field
The invention belongs to technical field of plant extraction is and in particular to a kind of mixed solvent extracts the process of fibrauretin.
Background technology
Fibrauretin (Palmatine) is the pure natural plant medicine that China voluntarily develops, and now has been loaded into Chinese Pharmacopoeia, this
Product have broad-spectrum antibacterial antivirus action, the multiple pharmacological action substantially increasing leukocytes phagocytic antibacterial, good antiinflammatory and increasing
Strong immunity of organisms effect.It is used for gynecological inflammation, bacillary dysentery, enteritis, respiratory tract and urinary tract infection, surgical infection, eye conjunctiva
Scorching.1.Gynecological inflammation urgent chronic pelvic inflammatory disease, acute and chronic adnexitis, cervical erosion, endometritis, mould toxicity vaginitiss, puerperium
Phase infection etc..2. urinary tract infection；3rd, surgical infection, eye conjunctivitis；4th, respiratory tract infection Deng Quan section medication.This product has to funguses
Inhibitory action is especially stronger to Candida albicans, achorion gypseum, Fonsecaea pedrosor effect.
The acquisition of fibrauretin is mainly extracted by menispermaceous plantss Caulis Fibraureae, but the yield with exhaustive exploitation Caulis Fibraureae is also more next
Fewer.The main flow extraction process of existing fibrauretin is sour water cold extraction technique, has extraction ratio low, and time-consuming for operation, and it is difficult to filter, and saltouts
Salt dosage is big, the shortcomings of sewage load is big.
Content of the invention
In order to solve the problems of the prior art, the present invention proposes the process that a kind of mixed solvent extracts fibrauretin,
Improve the extraction ratio of fibrauretin, decrease extraction time, improve production efficiency, filtrate is easily filtered, decrease workman's cleaning
The number of times of filter screen, reduces labor intensity, decreases the consumption of sour water, decreases consumption and the sewage load of sodium chloride.
In order to realize object above, the technical solution adopted in the present invention is: comprises the following steps:
1) Caulis Fibraureae powder is adopted mixed solvent to extract 2～5 times, Extracting temperature controls at 30～70 DEG C, cool down after extraction
Filter the insoluble impurity of removal and obtain filtrate, described mixed solvent is organic solvent cxhyozAcid is added to obtain after mixing with pure water；
2), after concentrating filtrate, standing cooled and filtered obtains concentrated solution；
3) alkali tune after filtering concentrated solution, ph value controls 9～10, and standing separates out after it and filters after insoluble matter, to filtrate
Saltout, filter to take much filtrate after saltouing and obtain crude product；
4) by crude product ethanol heating for dissolving, filtered while hot removes insoluble matter impurity, is slowly added to dense after filtrate cooling
Hydrochloric acid, filters after separating out Palmatine Hydro-chloride, takes much filtrate drying to obtain fibrauretin product.
Described step 1) in extract every time the cubical content of mixed solvent be 4～8 times of Caulis Fibraureae powder quality.
Organic solvent c in described mixed solventxhyozVolumetric ratio with pure water is 5:1～7:1, acid in described mixed solvent
Percent by volume be 1～2%.
Described acid is hydrochloric acid, formic acid, acetic acid or ethanedioic acid, the acid that acid is 0.5%～1% using volumetric concentration.
Described organic solvent cxhyozThe span of middle x is: the span of 1～3, y is: the span of 4～8, z
For: 1～2.
Described step 3) in alkali tune when the alkali that uses be sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate.
Described step 3) in filtrate is saltoutd using sodium chloride, in filtrate the mass concentration of sodium chloride be 7%～
10%.
Described step 4) in the cubical content of ethanol be 15～20 times of crude product quality, ethanol adopt volumetric concentration be 80%～
95% ethanol.
Described step 4) with adding activated carbon decolorizing 0.5～2 hour, the quality of activated carbon in ethanol heating for dissolving crude product
It is the 0.2%～1% of crude product quality.
Compared with prior art, Caulis Fibraureae powder is first extracted by the present invention with mixed solvent, and cooled and filtered removes insoluble
Impurity, mixed solvent is organic solvent cxhyozAdd acid to obtain after mixing with pure water, secondly by filtrate thickening filtration, again will
Filtrate alkali tune, standing separates out after it and filters after insoluble matter, and filtrate adds sodium chloride to be saltoutd, and filters to obtain crude product, finally will be thick
Product ethanol heating for dissolving, filtered while hot removes insoluble matter impurity, is slowly added to concentrated hydrochloric acid, separates out hydrochloric acid bar after filtrate cooling
After Martin, filtration drying obtains product.The present invention improves the extraction ratio of fibrauretin, decreases extraction time, improves production effect
Rate, filtrate is easily filtered, and decreases the number of times that workman clears up filter screen, reduces labor intensity, due to decreasing the consumption of sour water,
Just decrease consumption and the sewage load of sodium chloride.
Brief description
Fig. 1 is method of the present invention flow chart.
Specific embodiment
With reference to specific embodiment and Figure of description, the present invention is further explained.
Referring to Fig. 1, the present invention comprises the following steps:
1) Caulis Fibraureae powder is adopted mixed solvent to extract 2～5 times, Extracting temperature controls at 30～70 DEG C, cool down after extraction
Filter the insoluble impurity of removal and obtain filtrate, the cubical content extracting mixed solvent every time is 4～8 times of Caulis Fibraureae powder quality, described
Mixed solvent is organic solvent cxhyozAcid is added to obtain after mixing with pure water, organic solvent c in mixed solventxhyozWith pure water
Volumetric ratio is 5:1～7:1, and in mixed solvent, the percent by volume of acid is 1～2%, and acid is hydrochloric acid, formic acid, acetic acid or ethanedioic acid,
The acid that acid is 0.5%～1% using volumetric concentration, organic solvent cxhyozThe span of middle x is: the span of 1～3, y
For: the span of 4～8, z is: 1～2；
2), after concentrating filtrate, standing cooled and filtered obtains concentrated solution；
3) alkali tune after filtering concentrated solution, ph value controls 9～10, and standing separates out after it and filters after insoluble matter, to filtrate
Saltout, filter to take much filtrate after saltouing and obtain crude product, the alkali using during alkali tune is sodium hydroxide, potassium hydroxide, sodium carbonate or carbon
Sour hydrogen sodium, is saltoutd using sodium chloride to filtrate, and in filtrate, the mass concentration of sodium chloride is 7%～10%；
4) by crude product ethanol heating for dissolving, add activated carbon decolorizing 0.5～2 hour in heating for dissolving crude product, activated carbon
Quality be the 0.2%～1% of crude product quality, filtered while hot remove insoluble matter impurity, after filtrate cooling after be slowly added to dense salt
Acid, filters after separating out Palmatine Hydro-chloride, takes much filtrate drying to obtain fibrauretin product, the cubical content of ethanol is crude product quality
15～20 times, the ethanol that ethanol is 80%～95% using volumetric concentration.
Caulis Fibraureae powder is extracted according to 4 to 8 times of consumptions by the inventive method first with mixed solvent, extracts 2 to 5 times, carries
Take temperature control at 30 to 70 DEG C, merging filtrate cooled and filtered removes insoluble impurity, mixed solvent adopts cxhyozWith water with 7:
The ratio of 1 to 5:1 adds, after being mixed, the acid that concentration is 0.5% to 1%, in sour hydrochloric acid, formic acid, acetic acid and ethanedioic acid
A kind of；Secondly, after filtrate being concentrated, stand cooled and filtered；Alkali tune after filtering concentrated solution again, the alkali using during alkali tune is
One of sodium hydroxide, potassium hydroxide, sodium carbonate and sodium bicarbonate, ph value controls between 9 to 10, and standing treats that it separates out not
Filter after molten thing, filtrate adds 7% to 10% sodium chloride to be saltoutd, and filters to obtain crude product after 24 hours；Finally crude product is used
The ethanol heating for dissolving of the 80% to 95% of 15 to 20 times amount, the activated carbon decolorizing of addition 0.2% to 1% 0.5 to 2 hours, take advantage of
Heat filtering removes insoluble matter impurity, is slowly added to concentrated hydrochloric acid, after separating out Palmatine Hydro-chloride, filtration drying obtains after filtrate cooling
Product.
Present invention uses after mixed solvent extracts, the discharge capacity of waste water is reduced to the 1/8 of original sour water cold extraction technique,
The usage amount of sodium chloride is also reduced to 1/8, and sour water usage amount is reduced to 1/8, and present one order of classes or grades at school of workman produces a collection of fibrauretin,
Extraction time reduces 12 hours, and filter screen clearing times reduce 3 times, substantially reduce labor time and intensity.The present invention and tradition
Sour water cold extraction carries out Experimental Comparison and is as follows:
Find out, sour water cold extraction crude yield is high from above yield nuclear test result, but refined rear finished product is few, main cause
Be sour water cold extraction technique after saltouing during filtration under diminished pressure due to filtration difficulty so that filtrate is drained near filter paper and is separated out chlorine
Change sodium although crude yield is high, but have a lot of impurity, such as sodium chloride.Sour water cold extraction technique after using filter press technique
It is low that crude yield carries yield than present invention mixed solvent.
After original sour water cold extraction technique changes to alcohol extraction process, the production cycle went out a collection of the present invention from original every two days
Goods, one and half go out parcel till now, output increased to original 1.2 to 1.3 times, improve 25% to the utilization ratio of drug of Caulis Fibraureae
To 35%, save and dropped production cost.
Embodiment one:
The present invention comprises the following steps:
1) Caulis Fibraureae powder 200g is adopted mixed solvent to extract 3 times, Extracting temperature controls at 50 DEG C, cold filtration after extraction
Remove insoluble impurity and obtain filtrate, the cubical content of each mixed solvent is 6 times (1200ml) of Caulis Fibraureae powder quality, described mixing
Solvent is organic solvent cxhyozAcid is added to obtain after mixing with pure water, in mixed solvent, organic solvent and the volumetric ratio of pure water are
5:1, in mixed solvent, the percent by volume of acid is 1%；
2), after concentrating filtrate, standing cooled and filtered obtains concentrated solution, and the volume of concentrate is about 450ml；
3) alkali tune after concentrated solution being filtered, ph value controls 9, and standing separates out after it and filters after insoluble matter, and filtrate is saltoutd,
Add 40g sodium chloride in filtrate, saltout 24 hours, filter to take much filtrate after saltouing and obtain crude product 4.8g, use during alkali tune
Alkali is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate；
4) by crude product ethanol heating for dissolving, add activated carbon decolorizing 0.5～2 hour in heating for dissolving crude product, activated carbon
Quality be 0.1g, filtered while hot removes insoluble matter impurity, is slowly added to concentrated hydrochloric acid 3ml, separates out hydrochloric acid bar after filtrate cooling
Filter after Martin, take much filtrate drying to obtain fibrauretin product 2.6g, the cubical content 50ml of ethanol, ethanol adopts volumetric concentration
Ethanol for 80%.
Embodiment two:
The present invention comprises the following steps:
1) Caulis Fibraureae powder 200g is adopted mixed solvent to extract 4 times, Extracting temperature controls at 60 DEG C, cold filtration after extraction
Remove insoluble impurity and obtain filtrate, the cubical content extracting mixed solvent every time is 5 times (1000ml) of Caulis Fibraureae powder quality, described
Mixed solvent is organic solvent cxhyozAcid is added to obtain after mixing with pure water, the volume of organic solvent and pure water in mixed solvent
For 5:1, in mixed solvent, the percent by volume of acid is 1.6% to ratio；
2), after concentrating filtrate, standing cooled and filtered obtains concentrated solution (500ml)；
3) alkali tune after concentrated solution being filtered, ph value controls 9, and standing separates out after it and filters after insoluble matter, and filtrate is saltoutd,
Use salt 50g when saltouing, saltout 36 hours, filter to take much filtrate after saltouing and obtain crude product 5g, the alkali using during alkali tune is hydroxide
Sodium, potassium hydroxide, sodium carbonate or sodium bicarbonate, are saltoutd using sodium chloride to filtrate；
4) by crude product ethanol heating for dissolving, add activated carbon decolorizing 0.5～2 hour in heating for dissolving crude product, activated carbon
Quality be 0.15g, filtered while hot removes insoluble matter impurity, is slowly added to concentrated hydrochloric acid 3ml, separates out hydrochloric acid bar after filtrate cooling
Filter after Martin, take much filtrate drying to obtain fibrauretin product 3g, the cubical content of ethanol is 80ml, and ethanol adopts volumetric concentration
Ethanol for 90%.
Embodiment three:
The present invention comprises the following steps:
1) Caulis Fibraureae powder 200g is adopted mixed solvent to extract 5 times, Extracting temperature controls at 70 DEG C, cold filtration after extraction
Remove insoluble impurity and obtain filtrate, the cubical content extracting mixed solvent every time is 6 times (1200ml) of Caulis Fibraureae powder quality, described
Mixed solvent is organic solvent cxhyozAcid is added to obtain after mixing with pure water, the volume of organic solvent and pure water in mixed solvent
For 6:1, in mixed solvent, the percent by volume of acid is 1.5% to ratio；
2), after concentrating filtrate, standing cooled and filtered obtains concentrated solution 600ml；
3) alkali tune after filtering concentrated solution, ph value controls 10, and standing separates out after it and filters after insoluble matter, to filtrate salt
Analysis, salt dosage of saltouing is 55g, saltouts 48 hours, filters to take much filtrate and obtain crude product 4.8g after saltouing, the alkali using during alkali tune is
Sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate；
4) by crude product ethanol heating for dissolving, add activated carbon decolorizing 0.5～2 hour in heating for dissolving crude product, activated carbon
Quality be 0.2g, filtered while hot removes insoluble matter impurity, is slowly added to concentrated hydrochloric acid 3ml, separates out hydrochloric acid bar after filtrate cooling
Filter after Martin, take much filtrate drying to obtain fibrauretin product 2.8g, the cubical content 6.5ml of ethanol, ethanol adopts volume dense
Spend the ethanol for 85%.
Claims (9)
1. a kind of mixed solvent extracts the process of fibrauretin it is characterised in that comprising the following steps:
1) Caulis Fibraureae powder is adopted mixed solvent to extract 2～5 times, Extracting temperature controls at 30～70 DEG C, cold filtration after extraction
Remove insoluble impurity and obtain filtrate, described mixed solvent is organic solvent cxhyozAcid is added to obtain after mixing with pure water；
2), after concentrating filtrate, standing cooled and filtered obtains concentrated solution；
3) alkali tune after concentrated solution being filtered, ph value controls 9～10, and standing separates out after it and filters after insoluble matter, and filtrate is saltoutd,
Filter to take much filtrate after saltouing and obtain crude product；
4) by crude product ethanol heating for dissolving, filtered while hot removes insoluble matter impurity, is slowly added to concentrated hydrochloric acid after filtrate cooling,
Filter after separating out Palmatine Hydro-chloride, take much filtrate drying to obtain fibrauretin product.
2. a kind of mixed solvent according to claim 1 extracts the process of fibrauretin it is characterised in that described step
1) cubical content extracting mixed solvent in every time is 4～8 times of Caulis Fibraureae powder quality.
3. a kind of mixed solvent according to claim 2 extracts the process of fibrauretin it is characterised in that described mixing
Organic solvent c in solventxhyozBe 5:1～7:1 with the volumetric ratio of pure water, in described mixed solvent the percent by volume of acid be 1～
2%.
4. a kind of mixed solvent according to claim 3 extracts the process of fibrauretin it is characterised in that described acid is
Hydrochloric acid, formic acid, acetic acid or ethanedioic acid, the acid that acid is 0.5%～1% using volumetric concentration.
5. a kind of mixed solvent according to claim 4 extracts the process of fibrauretin it is characterised in that described organic
Solvent cxhyozThe span of middle x is: the span of 1～3, y is: the span of 4～8, z is: 1～2.
6. a kind of mixed solvent according to claim 1 extracts the process of fibrauretin it is characterised in that described step
3) alkali using during alkali tune in is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate.
7. a kind of mixed solvent according to claim 1 extracts the process of fibrauretin it is characterised in that described step
3) in, filtrate is saltoutd using sodium chloride, in filtrate, the mass concentration of sodium chloride is 7%～10%.
8. a kind of mixed solvent according to claim 1 extracts the process of fibrauretin it is characterised in that described step
4) in, the cubical content of ethanol is 15～20 times of crude product quality, the ethanol that ethanol is 80%～95% using volumetric concentration.
9. a kind of mixed solvent according to claim 1 extracts the process of fibrauretin it is characterised in that described step
4) with adding activated carbon decolorizing 0.5～2 hour in ethanol heating for dissolving crude product, the quality of activated carbon is crude product quality
0.2%～1%.
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| CN201610729907.0A CN106349240A (en) | 2016-08-25 | 2016-08-25 | Technique for extracting fibrauretine by using mixed solvent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058575A (en) * | 2006-04-21 | 2007-10-24 | 杭州豪迈医药科技有限公司 | Method of extracting and refining palmatin hydrochloride and application thereof |
| CN101619062A (en) * | 2009-07-02 | 2010-01-06 | 华宝食用香精香料（上海）有限公司 | Natural fibrauretine crystal and macroporous adsorbent resin preparation method thereof |
| CN104873503A (en) * | 2015-05-19 | 2015-09-02 | 何忠梅 | Preparation method of palmatine and composition thereof and novel medical application |
-
2016
- 2016-08-25 CN CN201610729907.0A patent/CN106349240A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058575A (en) * | 2006-04-21 | 2007-10-24 | 杭州豪迈医药科技有限公司 | Method of extracting and refining palmatin hydrochloride and application thereof |
| CN101619062A (en) * | 2009-07-02 | 2010-01-06 | 华宝食用香精香料（上海）有限公司 | Natural fibrauretine crystal and macroporous adsorbent resin preparation method thereof |
| CN104873503A (en) * | 2015-05-19 | 2015-09-02 | 何忠梅 | Preparation method of palmatine and composition thereof and novel medical application |
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