CN110437187A - A kind of purification process of potassium dehydroandrographolide succinate - Google Patents
A kind of purification process of potassium dehydroandrographolide succinate Download PDFInfo
- Publication number
- CN110437187A CN110437187A CN201910798271.9A CN201910798271A CN110437187A CN 110437187 A CN110437187 A CN 110437187A CN 201910798271 A CN201910798271 A CN 201910798271A CN 110437187 A CN110437187 A CN 110437187A
- Authority
- CN
- China
- Prior art keywords
- purification process
- process according
- dehydroandrographolide succinate
- potassium dehydroandrographolide
- concentration
- 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.)
- Pending
Links
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 27
- 239000011591 potassium Substances 0.000 title claims abstract description 27
- YTHKMAIVPFVDNU-GPTWTFMPSA-N 4-[[(1r,2r,4ar,5r,8as)-2-(3-carboxypropanoyloxy)-1,4a-dimethyl-6-methylidene-5-[(e)-2-(5-oxo-2h-furan-4-yl)ethenyl]-3,4,5,7,8,8a-hexahydro-2h-naphthalen-1-yl]methoxy]-4-oxobutanoic acid Chemical compound C(/[C@@H]1C(=C)CC[C@H]2[C@@]1(C)CC[C@H]([C@]2(COC(=O)CCC(O)=O)C)OC(=O)CCC(O)=O)=C\C1=CCOC1=O YTHKMAIVPFVDNU-GPTWTFMPSA-N 0.000 title claims abstract description 26
- 238000000746 purification Methods 0.000 title claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 235000019441 ethanol Nutrition 0.000 claims abstract description 19
- 239000012043 crude product Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000011109 contamination Methods 0.000 abstract description 3
- 230000000813 microbial effect Effects 0.000 abstract description 3
- 230000003321 amplification Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 6
- 239000003814 drug Substances 0.000 description 4
- 238000000108 ultra-filtration Methods 0.000 description 4
- 239000012467 final product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 241000746375 Andrographis Species 0.000 description 1
- BOJKULTULYSRAS-OTESTREVSA-N Andrographolide Chemical compound C([C@H]1[C@]2(C)CC[C@@H](O)[C@]([C@H]2CCC1=C)(CO)C)\C=C1/[C@H](O)COC1=O BOJKULTULYSRAS-OTESTREVSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- ASLUCFFROXVMFL-UHFFFAOYSA-N andrographolide Natural products CC1(CO)C(O)CCC2(C)C(CC=C3/C(O)OCC3=O)C(=C)CCC12 ASLUCFFROXVMFL-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000001754 anti-pyretic effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000002221 antipyretic Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/60—Two oxygen atoms, e.g. succinic anhydride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of purification process of potassium dehydroandrographolide succinate, by the concentration and additional amount that accurately control ethyl alcohol, reduce impurity generation, and this method is more conducive to industrialization amplification compared with the existing technology, it is lower to equipment requirement, it can be achieved that the closed production of overall process, reduces microbial contamination risk, the quality for guaranteeing product, has practical extending application value.
Description
Technical field
The present invention relates to a kind of purification process of potassium dehydroandrographolide succinate.
Background technique
Potassium dehydroandrographolide succinate is the andrographolide and the resulting Herba Andrographitis of Potassium Suceinate anhydride reactant extracted from Chinese medicine Folium Andrographis
Lactone disuccinic acid half ester sylvite, for white to faint yellow solid.With antiviral, antipyretic, antiinflammation.Potassium dehydroandrographolide succinate is because having
The features such as significant in efficacy low with toxicity, has been cited as one of first batch of institute of traditional Chinese medicine's first aid indispensability Chinese patent drug in China.As the medicine is facing
Bed is widely used, and Reporting of harms increases year by year, main reason is that purity is not high enough.
To improve potassium dehydroandrographolide succinate purity, potassium dehydroandrographolide succinate adverse reaction is reduced, product quality, patent CN1357546A report warp are improved
It crosses product quality made of the potassium dehydroandrographolide succinate raw material of ultrafiltration to significantly improve, still, this method purification process is complicated for operation, ultra-filtration process
Temperature requirement guarantee that potassium dehydroandrographolide succinate be in solution state, and ultrafiltration temperature control it is more difficult；Secondly, the ultrafiltration membrane mistake of this method
It needs to regenerate after filter, needs to retain substance in a large amount of solvent elution film, just can guarantee that film can reuse, but with using
Number increases, and the retention efficiency decline of film, equipment loss is big, high production cost, and industrialization is difficult.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of purification process of potassium dehydroandrographolide succinate, it includes the following steps:
Potassium dehydroandrographolide succinate crude product is taken, the ethyl alcohol that concentration is 20-60% is added to dissolve, filtering, filtrate adds concentration to be the second of 90-100%
Alcoholic solution mixes, and stands crystallization, and filtering, filter residue is dried under reduced pressure, crush to get.
Further, the potassium dehydroandrographolide succinate crude product adds the ethanol solution that concentration is 40% to dissolve.
Further, the mass volume ratio when crude product adds ethanol solution to dissolve is 1g:4-15ml.
Further, described to be dissolved as dissolving by heating, heating temperature is preferably 60 DEG C to 40-80 DEG C.
Further, the filtrate adds concentration to be 95% ethanol solution.
Further, the volume mass ratio for the ethanol solution and crude product that the concentration is 90-100% is 50-100ml:1g,
It is preferred that 100ml:1g.
Further, the standing crystallization time 10h or more, preferably 10-24h；The temperature for standing crystallization is normal
Temperature.
Further, the drying temperature is 50-70 DEG C, and the time is greater than 6h.
The purification process of potassium dehydroandrographolide succinate of the present invention reduces impurity generation by accurately controlling the concentration and additional amount of ethyl alcohol,
This method simultaneously is more conducive to industrialization amplification compared with the existing technology, while equipment requirement is lower, it can be achieved that the closed life of overall process
It produces, reduces microbial contamination risk, have practical extending application value.
Obviously, above content according to the present invention is not being departed from according to the ordinary technical knowledge and customary means of this field
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The specific embodiment of form by the following examples remakes further specifically above content of the invention
It is bright.But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to example below.It is all to be based on above content of the present invention
The technology realized all belongs to the scope of the present invention.
Specific embodiment
The purification process of the potassium dehydroandrographolide succinate of the present invention of embodiment 1
Potassium dehydroandrographolide succinate crude product 10g is taken, 40% ethanol solution 40ml is added, is gradually heated to 60 DEG C, stirs to being completely dissolved, takes advantage of
95% ethyl alcohol of 1000ml is added in heat filtration, filtrate slowly, and stirring to room temperature stands crystallization 10 hours, filtration, and 50 DEG C of filter residue dry
Dry 6 hours, it is finely ground after to obtain the final product.
The purification process of the potassium dehydroandrographolide succinate of the present invention of embodiment 2
Potassium dehydroandrographolide succinate crude product 10g is taken, 60% ethanol solution 50ml is added, is gradually heated to 60 DEG C, stirs to being completely dissolved, takes advantage of
90% ethyl alcohol of 900ml is added in heat filtration, filtrate slowly, and stirring to room temperature stands 24 hours, filtration, and 60 DEG C of dryings 8 of filter residue are small
When, it is finely ground after to obtain the final product.
The purification process of the potassium dehydroandrographolide succinate of the present invention of embodiment 3
Potassium dehydroandrographolide succinate crude product 10g is taken, 20% ethanol solution 70ml is added, is gradually heated to 80 DEG C, stirs to being completely dissolved, takes advantage of
1000ml100% ethyl alcohol is added in heat filtration, filtrate slowly, and stirring to room temperature stands 10 hours, filtration, 70 DEG C of dryings 10 of filter residue
Hour, it is finely ground after to obtain the final product.
Beneficial effects of the present invention are further illustrated below by way of test example.
The potassium dehydroandrographolide succinate that the purification process of the present invention of test example 1 obtains compares
7 batches of potassium dehydroandrographolide succinate crude products are taken respectively, are purified with 6 batches according to 1 method of embodiment, using 1 batch as reference, the production that will be obtained
Product sampling, detects related substance, related substance data such as the following table 1.
Obtain from table 1: after the method for the present invention refines, amount of impurities and total amount are substantially reduced in fine work, total miscellaneous
It is reduced to by 2.92% 1.0% hereinafter, impurity number is reduced to 6 or so by 14.
To sum up, the purification process of potassium dehydroandrographolide succinate of the present invention reduces impurity by accurately controlling the concentration and additional amount of ethyl alcohol
It generates, while equipment requirement is low, it can be achieved that the closed production of overall process, reduces microbial contamination risk, has practical popularization and answer
With value.
Claims (8)
1. a kind of purification process of potassium dehydroandrographolide succinate, it is characterised in that: it includes the following steps:
Potassium dehydroandrographolide succinate crude product is taken, the ethanol solution that concentration is 20-60% is added to dissolve, filtering, filtrate adds concentration to be the second of 90-100%
Alcoholic solution mixes, and stands crystallization, and filtering, filter residue is dried under reduced pressure, crush to get.
2. purification process according to claim 1, it is characterised in that: the potassium dehydroandrographolide succinate crude product adds concentration to be 40% ethyl alcohol
Solution dissolution.
3. purification process according to claim 1 or 2, it is characterised in that: the matter when crude product adds ethanol solution to dissolve
Amount volume ratio is 1g:4-15ml.
4. purification process according to claim 1, which is characterized in that described to be dissolved as dissolving by heating, heating temperature is extremely
40-80 DEG C, preferably 60 DEG C.
5. purification process according to claim 1, which is characterized in that the filtrate adds concentration to be 95% ethanol solution.
6. purification process according to claim 1, which is characterized in that ethanol solution that the concentration is 90-100% and thick
The volume mass ratio of product is 50-100ml:1g, preferably 100ml:1g.
7. purification process according to claim 1, which is characterized in that the standing crystallization time 10h or more；Preferably
10-24h；The temperature for standing crystallization is room temperature.
8. purification process according to claim 1, which is characterized in that the drying temperature is 50-70 DEG C, and the time is greater than
6h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910798271.9A CN110437187A (en) | 2019-08-27 | 2019-08-27 | A kind of purification process of potassium dehydroandrographolide succinate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910798271.9A CN110437187A (en) | 2019-08-27 | 2019-08-27 | A kind of purification process of potassium dehydroandrographolide succinate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110437187A true CN110437187A (en) | 2019-11-12 |
Family
ID=68438013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910798271.9A Pending CN110437187A (en) | 2019-08-27 | 2019-08-27 | A kind of purification process of potassium dehydroandrographolide succinate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110437187A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617527A (en) * | 2012-03-01 | 2012-08-01 | 湖北荷普药业股份有限公司 | Method for preparing potassium dehydroandrographolide succinate or potassium sodium dehydroandroan drographolide succinate |
| CN103087017A (en) * | 2013-02-28 | 2013-05-08 | 成都倍特药业有限公司 | Refinement method of crude potassium sodium dehydroandroan drographolide succinate product |
| CN103113330A (en) * | 2013-02-28 | 2013-05-22 | 成都倍特药业有限公司 | Andrographolide salifying process |
| CN103159710A (en) * | 2013-04-16 | 2013-06-19 | 成都天台山制药有限公司 | Antiviral decalin derivate |
| CN103159709A (en) * | 2013-04-16 | 2013-06-19 | 成都天台山制药有限公司 | Potassium dehydroandrograpolide succinate crystal and preparation method thereof |
| CN107857747A (en) * | 2017-10-16 | 2018-03-30 | 广州普星药业有限公司 | A kind of preparation method of potassium dehydroandrographolide succinate |
-
2019
- 2019-08-27 CN CN201910798271.9A patent/CN110437187A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617527A (en) * | 2012-03-01 | 2012-08-01 | 湖北荷普药业股份有限公司 | Method for preparing potassium dehydroandrographolide succinate or potassium sodium dehydroandroan drographolide succinate |
| CN103087017A (en) * | 2013-02-28 | 2013-05-08 | 成都倍特药业有限公司 | Refinement method of crude potassium sodium dehydroandroan drographolide succinate product |
| CN103113330A (en) * | 2013-02-28 | 2013-05-22 | 成都倍特药业有限公司 | Andrographolide salifying process |
| CN103159710A (en) * | 2013-04-16 | 2013-06-19 | 成都天台山制药有限公司 | Antiviral decalin derivate |
| CN103159709A (en) * | 2013-04-16 | 2013-06-19 | 成都天台山制药有限公司 | Potassium dehydroandrograpolide succinate crystal and preparation method thereof |
| CN107857747A (en) * | 2017-10-16 | 2018-03-30 | 广州普星药业有限公司 | A kind of preparation method of potassium dehydroandrographolide succinate |
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| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191112 |