CN109180618A - A kind of decoloration process of andrographolide - Google Patents
A kind of decoloration process of andrographolide Download PDFInfo
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- CN109180618A CN109180618A CN201810886916.XA CN201810886916A CN109180618A CN 109180618 A CN109180618 A CN 109180618A CN 201810886916 A CN201810886916 A CN 201810886916A CN 109180618 A CN109180618 A CN 109180618A
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- CN
- China
- Prior art keywords
- leaching liquor
- extractor
- coarse powder
- constant temperature
- andrographolide
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- 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
Abstract
The invention discloses a kind of decoloration process of andrographolide, comprising the following steps: and it takes the leaf of Herba Andrographitis by its naturally dry, is ground into the coarse powder that partial size is less than 20mm, it is spare；By Herba Andrographitis coarse powder alcohol steep, leaching liquor is filtered to obtain；2~3% (W/V) active carbons are added in leaching liquor, are heated to 65~75 DEG C, stirring and leaching liquid carries out adsorption bleaching, and the adsorption bleaching time 20-40min is filtered to remove active carbon after absorption.The clarity for the leaching liquor that the present invention is prepared is good, and front and back content loss of decolourizing is small, while active carbon additional amount is few in decolorization, and preparation cost is low.
Description
Technical field
The invention belongs to pharmaceutical technology field, the decoloration process of specifically a kind of andrographolide.
Background technique
The patent of invention of Patent No. ZL201410076514.5 discloses a kind of extraction process of andrographolide, system
Can decolourize to extracted obtained Herba Andrographitis leaching liquor during standby, but its decolourize to Herba Andrographitis leaching liquor after punching
The loss of lotus lactone content is larger, while active carbon additional amount is more in decolorization, and andrographolide is as a kind of maturation
Drug, it is general using producing in enormous quantities, result in andrographolide preparation cost to increase in this way.
Summary of the invention
To solve the above-mentioned problems in the prior art, the present invention provides a kind of decoloration process of andrographolide.
The clarity for the leaching liquor that the decoloration process of the andrographolide is prepared is good, and front and back Determination of Andrographolide loss of decolourizing
It is small, while active carbon additional amount is few in decolorization, preparation cost is low.
The technical solution adopted by the present invention is that:
A kind of decoloration process of andrographolide, comprising the following steps:
S1, crushing: taking the leaf of Herba Andrographitis by its naturally dry, be ground into the coarse powder that partial size is less than 20mm, spare；
S2, extraction: by gained Herba Andrographitis coarse powder alcohol steep in step S1, leaching liquor is filtered to obtain；
S3, decoloration: being added 2%~3% (W/V) active carbon for gained leaching liquor in step S2, be heated to 65 DEG C~75 DEG C,
Stirring and leaching liquid carries out adsorption bleaching, and the adsorption bleaching time 20min-40min is filtered to remove active carbon after absorption.
Preferably, leaching liquor heating temperature is 70 DEG C -75 DEG C in the step 3, the adsorption bleaching time 30min-
40min。
Preferably, active carbon additional amount is 2% (W/V) after leaching liquor mixes in the S3, leaching liquor is heated to 75
DEG C carry out adsorption bleaching 40mim.
Preferably, decoloration includes following sub-step in the step S2:
S21, gained Herba Andrographitis coarse powder in step S1 is divided into equiponderant n (n is positive integer) part, slowly put into respectively
1 carries out extracting at constant temperature into n extractor, and the extracting at constant temperature includes following sub-step:
S22, primary extraction: 1 primary extraction stoste is added into n extractor, and 40 DEG C of constant temperature impregnate 6h, filter once
Leaching liquor；It is 60% ethyl alcohol that stoste is once extracted in No. 1 pot for solvent extraction, and additional amount is 3 times of coarse powder weight in extractor；
S23, secondary extraction: 1 secondary extraction stoste is added into n extractor, and 40 DEG C of constant temperature impregnate 2h, filter secondary
Leaching liquor, primary extraction stoste of the secondary leaching liquor of gained as next extractor；Secondary extraction stoste in No. 1 extractor
For 60% ethyl alcohol, additional amount is 2 times of coarse powder weight in extractor；
S24, extract three times: 1 60% ethyl alcohol that weight is 2 times of coarse powder weight, 40 DEG C of constant temperature leachings are added into n extractor
2h is steeped, filters to obtain leaching liquor three times, gained secondary extraction stoste of the leaching liquor as next extractor three times；
S25, it is distilled to recover ethyl alcohol: 1 filter residue into n extractor is distilled, until concentration of alcohol is 40%.
Beneficial effects of the present invention are as follows:
30% or more the usage amount that active carbon is reduced in andrographolide decoloration process of the invention, before but obtaining decoloration
Heart lotus lactone content loses lower leaching liquor afterwards, not only increases the utilization rate of creat lactone, while reducing and being produced into
This.
Specific embodiment
The embodiment of the present invention is described in detail below.
A kind of embodiment 1: decoloration process of andrographolide, comprising the following steps:
S1. it crushes: taking the leaf of Herba Andrographitis by its naturally dry, be ground into the coarse powder that partial size is less than 20mm, it is spare；
S2. it extracts: gained Herba Andrographitis coarse powder in step S1 is divided into equiponderant n (n is positive integer) part, it is slow respectively
Investment 1 carries out extracting at constant temperature into n extractor, carries out extracting at constant temperature using following endless form；
No. 1 extractor:
S21. primary extraction: being added 60% ethyl alcohol, and additional amount is 3 times of coarse powder weight in extractor, and 40 DEG C of constant temperature impregnate
6h filters to obtain a leaching liquor；
S22. two extractions: being added 60% ethyl alcohol, and additional amount is 2 times of coarse powder weight in extractor, and 40 DEG C of constant temperature impregnate
2h filters to obtain secondary leaching liquor；
S23. it extracts three times: 60% ethyl alcohol is added, additional amount is 2 times of coarse powder weight in extractor, and 40 DEG C of constant temperature impregnate
2h filters to obtain leaching liquor three times；
No. 2 extractors:
S21. primary extraction: being added the secondary leaching liquor of No. 1 tank, and for primary extraction stoste, 40 DEG C of constant temperature impregnate 6h, filtering
Obtain a leaching liquor；
S22. two extractions: being added the leaching liquor three times of No. 1 tank, is secondary extraction stoste, and 40 DEG C of constant temperature impregnate 2h, filtering
Obtain secondary leaching liquor；
S23. it extracts three times: 60% ethyl alcohol is added, additional amount is 2 times of coarse powder weight in extractor, and 40 DEG C of constant temperature impregnate
2h filters to obtain leaching liquor three times；
No. 3 extractors:
S21. primary extraction: being added the secondary leaching liquor of No. 2 tanks, and for primary extraction stoste, 40 DEG C of constant temperature impregnate 2h, filtering
Obtain a leaching liquor；
S22. two extractions: being added the leaching liquor three times of No. 2 tanks, is secondary extraction stoste, and 40 DEG C of constant temperature impregnate 2h, filtering
Obtain secondary leaching liquor；
S23. it extracts three times: 60% ethyl alcohol is added, additional amount is 2 times of coarse powder weight in extractor, and 40 DEG C of constant temperature impregnate
2h filters to obtain leaching liquor three times；
And so on be recycled to n extractor；
N extractor:
S21. primary extraction: being added the secondary leaching liquor of n-1 tank, and for primary extraction stoste, 40 DEG C of constant temperature impregnate 2h, mistake
Filter to obtain a leaching liquor；
S22. two extractions: being added the leaching liquor three times of n-1 tank, is secondary extraction stoste, and 40 DEG C of constant temperature impregnate 2h, mistake
Filter to obtain secondary leaching liquor；
S23. it extracts three times: 60% ethyl alcohol is added, additional amount is 2 times of coarse powder weight in extractor, and 40 DEG C of constant temperature impregnate
2h filters to obtain leaching liquor three times；
It is distilled to recover ethyl alcohol: 1 filter residue into n extractor is distilled, until concentration of alcohol is 40%；
S3. decolourize: a leaching liquor of collection 1 to n extractor is added 2% (W/V) active carbon, is heated to after mixing
65 DEG C, stirring and leaching liquid carries out adsorption bleaching, and the adsorption bleaching time 20min is filtered to remove active carbon after absorption.
The leaching liquor after decolourizing in embodiment 1 is observed, clarity is as shown in table 1；Measure leaching liquor decoloration in embodiment 1
The loss of front and back Determination of Andrographolide, measurement result are as shown in table 1.
S4. it is concentrated: the leaching liquor after decoloration is subjected to vacuum-concentrcted, being concentrated into relative density is 1.02g/cm3, is obtained
Andrographolide concentrate；Wherein, the vacuum-concentrcted temperature is 40 DEG C, vacuum degree is -0.05Mpa；
S5. crystallization: by andrographolide concentrate, crystallization 8h, filtering, obtained solid are that andrographolide is thick at 2 DEG C
Product.
The content of giving money as a gift of crude product in embodiment 1 is measured, test result is as shown in table 1.
Decoloration process parameter in embodiment 2-9, comparative example 1 is as shown in table 1, remaining preparation process is with embodiment 1, respectively
The content of giving money as a gift of leaching liquor, crude product after decolourizing in embodiment 2-9 and comparative example 1 is tested, test result such as 1 institute of table
Show.
Table 1
It can be seen from Table 1 that embodiment 1-9 is compared with comparative example 1, the Determination of Andrographolide before and after guaranteeing decoloration
It loses in approximate situation, reduces production cost.The effect of especially embodiment 3 is best, and embodiment 3 is compared to existing skill
There is better clarity, crude product to give money as a gift content in the case where reducing 30%-50% active carbon additional amount, and have for art
There is lower Determination of Andrographolide to lose, preparation cost significantly reduces；Embodiment 4 is taken second place, and embodiment 4 is compared to existing skill
Art there is better clarity, crude product to give money as a gift content in the case where reducing 16%-37% active carbon additional amount, system
Standby cost is lower.
A specific embodiment of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.
Claims (4)
1. a kind of decoloration process of andrographolide, which comprises the following steps:
S1, crushing: taking the leaf of Herba Andrographitis by its naturally dry, be ground into the coarse powder that partial size is less than 20mm, spare；
S2, extraction: by gained Herba Andrographitis coarse powder alcohol steep in step S1, leaching liquor is filtered to obtain；
S3, decoloration: 2%~3% (W/V) active carbon is added in gained leaching liquor in step S2, is heated to 65 DEG C~75 DEG C, stirring
Leaching liquor carries out adsorption bleaching, and the adsorption bleaching time 20min-40min is filtered to remove active carbon after absorption.
2. a kind of decoloration process of andrographolide according to claim 1, which is characterized in that extracted in the step 3
Liquid heating temperature is 70 DEG C -75 DEG C, the adsorption bleaching time 30min-40min.
3. a kind of decoloration process of andrographolide according to claim 1, which is characterized in that leaching liquor is mixed in the S3
Active carbon additional amount is 2% (W/V) after even, and leaching liquor is heated to 75 DEG C of progress adsorption bleaching 40mim.
4. a kind of decoloration process of andrographolide according to claim 1, which is characterized in that decolourize in the step S2
Including following sub-step:
S21, gained Herba Andrographitis coarse powder in step S1 is divided into equiponderant n (n is positive integer) part, slowly puts into 1 to n respectively
Extracting at constant temperature is carried out in number extractor, the extracting at constant temperature includes following sub-step:
S22, primary extraction: 1 primary extraction stoste is added into n extractor, and 40 DEG C of constant temperature impregnate 6h, filter once to extract
Liquid；It is 60% ethyl alcohol that stoste is once extracted in No. 1 pot for solvent extraction, and additional amount is 3 times of coarse powder weight in extractor；
S23, secondary extraction: 1 secondary extraction stoste is added into n extractor, and 40 DEG C of constant temperature impregnate 2h, filter to obtain secondary extraction
Liquid, primary extraction stoste of the secondary leaching liquor of gained as next extractor；Secondary extraction stoste is in No. 1 extractor
60% ethyl alcohol, additional amount are 2 times of coarse powder weight in extractor；
S24, extract three times: 1 60% ethyl alcohol that weight is 2 times of coarse powder weight is added into n extractor, and 40 DEG C of constant temperature impregnate
2h, filters to obtain leaching liquor three times, gained secondary extraction stoste of the leaching liquor as next extractor three times；
S25, it is distilled to recover ethyl alcohol: 1 filter residue into n extractor is distilled, until concentration of alcohol is 40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810886916.XA CN109180618A (en) | 2018-08-06 | 2018-08-06 | A kind of decoloration process of andrographolide |
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| CN201810886916.XA CN109180618A (en) | 2018-08-06 | 2018-08-06 | A kind of decoloration process of andrographolide |
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| CN109180618A true CN109180618A (en) | 2019-01-11 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194753A (en) * | 2019-07-15 | 2019-09-03 | 成都通德药业有限公司 | A kind of andrographolide process for refining |
| CN114634470A (en) * | 2022-03-25 | 2022-06-17 | 太极集团四川南充制药有限公司 | Extraction method of dehydroandrographolide and andrographis tablet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896890A (en) * | 2014-03-04 | 2014-07-02 | 成都通德药业有限公司 | Process for extracting andrographolide |
| CN104140403A (en) * | 2014-07-02 | 2014-11-12 | 成都通德药业有限公司 | Andrographolide separation and purification process |
| CN108218812A (en) * | 2016-12-13 | 2018-06-29 | 河南后羿实业集团有限公司 | A kind of method that andrographolide is extracted from Herba Andrographitis |
-
2018
- 2018-08-06 CN CN201810886916.XA patent/CN109180618A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896890A (en) * | 2014-03-04 | 2014-07-02 | 成都通德药业有限公司 | Process for extracting andrographolide |
| CN104140403A (en) * | 2014-07-02 | 2014-11-12 | 成都通德药业有限公司 | Andrographolide separation and purification process |
| CN108218812A (en) * | 2016-12-13 | 2018-06-29 | 河南后羿实业集团有限公司 | A kind of method that andrographolide is extracted from Herba Andrographitis |
Non-Patent Citations (1)
| Title |
|---|
| KILAMBI PUNDARIKAKSHUDU ET AL.: "A Simple and Facile Method for the Isolation of Andrographolide from Andrographis Paniculata Nees", 《AM. J. PHARMTECH RES.》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194753A (en) * | 2019-07-15 | 2019-09-03 | 成都通德药业有限公司 | A kind of andrographolide process for refining |
| CN114634470A (en) * | 2022-03-25 | 2022-06-17 | 太极集团四川南充制药有限公司 | Extraction method of dehydroandrographolide and andrographis tablet |
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