CN113527234A - Extraction and separation method of andrographolide - Google Patents

Extraction and separation method of andrographolide Download PDF

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Publication number
CN113527234A
CN113527234A CN202110998511.7A CN202110998511A CN113527234A CN 113527234 A CN113527234 A CN 113527234A CN 202110998511 A CN202110998511 A CN 202110998511A CN 113527234 A CN113527234 A CN 113527234A
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Prior art keywords
andrographolide
adsorbent
andrographis paniculata
andrographis
additive
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CN202110998511.7A
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Chinese (zh)
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黄璐
王志成
方植伟
胡玉
张迎
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Hunan Huakang Biotechnology Co ltd
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Hunan Huakang Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic 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
    • C07D307/56Heterocyclic 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
    • C07D307/60Two oxygen atoms, e.g. succinic anhydride

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides an extraction and separation method of andrographolide, and relates to the technical field of andrographolide extraction. According to the invention, the selected common andrographis herb is smashed to obtain smashed common andrographis herb, then the additive and ethanol are added into the smashed common andrographis herb, and the smashed common andrographis herb is mixed and extracted under the condition of negative pressure, so that a better extraction effect is achieved, then common andrographis herb extract is obtained by filtering, the extract is adsorbed by using an adsorbent, then the filtering is carried out, impurities are further removed, the adsorption is carried out by using a packed column, then the desorption is carried out after the adsorption, so that eluent is obtained, so that most of the impurities are removed, then the vacuum crystallization is carried out, the andrographolide crystal is washed, and then the andrographolide finished product is smashed to form andrographolide, so that the impurities contained in the andrographolide finished product are less, and a better use effect is achieved.

Description

Extraction and separation method of andrographolide
Technical Field
The invention relates to the technical field of andrographolide extraction, and particularly relates to an extraction and separation method of andrographolide.
Background
In the existing andrographolide extraction process, andrographis paniculata is used as a raw material, and andrographis paniculata is crushed, extracted, crystallized and refined to obtain andrographolide, and the existing extraction method is mainly used for extracting through ultrasonic wave assistance, ultrasonic wave microwave assistance and enzymolysis assistance, so that the obtained andrographolide through extraction has more impurities, and a better using effect is difficult to achieve.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for extracting and separating andrographolide.
In order to achieve the purpose, the invention adopts the following technical scheme: an extraction and separation method of andrographolide, wherein the preparation material of andrographolide comprises andrographis paniculata medicinal materials, an adsorbent and an additive, and the components of the materials are as follows: 82-94% of andrographis paniculata medicinal material, 3-12% of adsorbent and 3-6% of additive.
In order to remove impurities, the improvement of the invention is that the adsorbent is one or a mixture of more of acid activated clay, bleaching earth and activated carbon in any proportion.
For better extraction, the invention improves that the additive is one or a mixture of more of sodium dodecyl sulfate, methyl amyl alcohol, polyacrylamide, triethyl hexyl phosphoric acid and fatty acid polyglycol ester in any proportion.
In order to achieve different effects, the invention has the improvement that the components of each material are as follows: 84% of andrographis paniculata medicinal material, 10% of adsorbent and 6% of additive.
In order to achieve different effects, the invention has the improvement that the components of each material are as follows: 88% of andrographis paniculata medicinal material, 7% of adsorbent and 5% of additive.
In order to achieve different effects, the invention has the improvement that the components of each material are as follows: 92% of andrographis paniculata medicinal material, 4% of adsorbent and 4% of additive.
The extraction and separation method of andrographolide comprises the following steps:
s1: selecting andrographis paniculata medicinal materials with uniform length and complete shape, chopping the selected andrographis paniculata medicinal materials to enable the size of the andrographis paniculata medicinal materials to be 0.5-1cm, then putting the chopped andrographis paniculata medicinal materials into a crusher to be crushed, wherein the crushing speed is 300-;
s2: placing the crushed common andrographis herb obtained in the step S1 and additives into an extraction container, adding 85-95% ethanol to make the ethanol be 14-20 times of the mass of the common andrographis herb, stirring and extracting under the negative pressure environment, wherein the negative pressure is 0.4-0.6 MPa, the stirring rotation speed is 120-180 r/min, the extraction temperature is 52-58 ℃, the extraction time is 3-4 hours, and filtering the extracted mixed solution to obtain common andrographis herb extract;
s3: pouring the andrographis paniculata extract obtained in the step S2 and an adsorbent into a reaction tank, adjusting the temperature to 54-64 ℃, mixing and removing impurities, stirring at the rotating speed of 80-120 revolutions per minute for 90-120 minutes, and filtering the mixture to obtain an impurity-removed extract;
s4: performing column exchange adsorption impurity removal on the impurity-removed extracting solution obtained in the step S3, wherein the column filling material is macroporous adsorption resin or silica gel, so as to obtain an adsorption column;
s5: washing the adsorption column obtained in S4 with pure water to clear the effluent, and eluting the adsorption column with 2-3 times of 55-65% alcoholic solution to obtain andrographolide eluate;
s6: heating and concentrating the andrographolide eluent obtained in the step S5 under a vacuum condition to 40-50% of the initial volume of the eluent, wherein the vacuum degree is 0.04-0.06MPa, and the temperature is 40-50 ℃ so as to obtain a concentrated solution, and then standing the concentrated solution, and carrying out natural cooling crystallization on the concentrated solution so as to obtain andrographolide crystals;
s7: washing the andrographolide crystals obtained in S6 with pure water, drying after washing, and pulverizing to obtain andrographolide.
In order to achieve better stripping effect, the improvement of the invention is that the alcoholic solution in the step S5 is a mixture of ethanol and methanol in any proportion.
Compared with the prior art, the invention has the advantages and positive effects that,
according to the method, the selected common andrographis herbs are crushed to obtain crushed common andrographis herbs, additives and ethanol are added into the crushed common andrographis herbs, the crushed common andrographis herbs are mixed and extracted under the condition of negative pressure, a good extraction effect is achieved, then common andrographis herb extracting solution is obtained through filtering, the extracting solution is subjected to adsorption treatment through an adsorbent, then impurities are further removed through filtering, the impurities are adsorbed through a packed column, after adsorption, elution is carried out, an eluent is obtained, most of the impurities are removed, then vacuum crystallization is carried out, andrographolide crystals are washed, and then the andrographolide crystals are crushed to form finished andrographolide products, so that the impurities contained in the finished andrographolide products are few, and the good using effect is achieved.
Drawings
FIG. 1 is a flow chart of the extraction and separation method of andrographolide provided by the present invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be further described with reference to the accompanying drawings and examples. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and thus the present invention is not limited to the specific embodiments of the present disclosure.
Referring to fig. 1, the present invention provides a method for extracting and separating andrographolide, wherein the andrographolide preparation material is composed of andrographis paniculata, an adsorbent and an additive, and the components of each material are as follows: 82-94% of andrographis paniculata medicinal material, 3-12% of adsorbent and 3-6% of additive.
The adsorbent is one or a mixture of more of acid activated clay, bleaching earth and activated carbon in any proportion.
The additive is one or a mixture of more of sodium dodecyl sulfate, methyl amyl alcohol, polyacrylamide, triethyl hexyl phosphoric acid and fatty acid polyglycol ester in any proportion.
Example one
The components of each material are as follows: 84% of andrographis paniculata medicinal material, 10% of adsorbent and 6% of additive.
The extraction and separation method of andrographolide comprises the following steps:
s1: selecting andrographis paniculata medicinal materials with uniform length and complete shape, chopping the selected andrographis paniculata medicinal materials to enable the size of the andrographis paniculata medicinal materials to be 0.5-1cm, then putting the chopped andrographis paniculata medicinal materials into a crusher to be crushed, wherein the crushing speed is 300 revolutions per minute, and the crushing time is 30 minutes, so that crushed andrographis paniculata is obtained;
s2: placing the crushed common andrographis herb obtained in the step S1 and additives into an extraction container, adding 85% ethanol to make the ethanol be 16 times of the mass of the common andrographis herb, stirring and extracting under a negative pressure environment, wherein the negative pressure is 0.4 MPa, the stirring speed is 120 revolutions per minute, the extraction temperature is 54 ℃, the extraction time is 4 hours, and then filtering the extracted mixed solution to obtain common andrographis herb extracting solution;
s3: pouring the andrographis paniculata extract obtained in the step S2 together with an adsorbent into a reaction tank, adjusting the temperature to 56 ℃, mixing and removing impurities, stirring at the rotating speed of 100 revolutions per minute for 120 minutes, and filtering the mixture to obtain an impurity-removed extract;
s4: performing column exchange adsorption impurity removal on the impurity-removed extracting solution obtained in the step S3, wherein the column filling material is macroporous adsorption resin or silica gel, so as to obtain an adsorption column;
s5: washing the adsorption column obtained in S4 with pure water to clear the effluent, and eluting the adsorption column with alcohol solution with concentration of 58% 3 times of the volume of the adsorption column to obtain andrographolide eluent;
s6: heating and concentrating the andrographolide eluent obtained in the step S5 under a vacuum condition to 50% of the initial volume of the eluent, wherein the vacuum degree is 0.06MPa, and the temperature is 44 ℃, so as to obtain a concentrated solution, standing the concentrated solution, and carrying out natural cooling crystallization on the concentrated solution, so as to obtain andrographolide crystals;
s7: washing the andrographolide crystals obtained in S6 with pure water, drying after washing, and pulverizing to obtain andrographolide.
The alcohol solution in step S5 is a mixture of ethanol and methanol in any ratio.
Example two
The components of each material are as follows: 88% of andrographis paniculata medicinal material, 7% of adsorbent and 5% of additive.
The extraction and separation method of andrographolide comprises the following steps:
s1: selecting andrographis paniculata medicinal materials with uniform length and complete shape, chopping the selected andrographis paniculata medicinal materials to enable the size of the andrographis paniculata medicinal materials to be 0.5-1cm, then putting the chopped andrographis paniculata medicinal materials into a crusher to be crushed, wherein the crushing speed is 360 revolutions per minute, and the crushing time is 26 minutes, so that crushed andrographis paniculata is obtained;
s2: placing the crushed common andrographis herb obtained in the step S1 and additives into an extraction container, adding 90% ethanol to make the ethanol 17 times of the mass of the common andrographis herb, stirring and extracting under a negative pressure environment, wherein the negative pressure is 0.5 MPa, the stirring speed is 160 revolutions per minute, the extraction temperature is 56 ℃, the extraction time is 4 hours, and filtering the extracted mixed solution to obtain common andrographis herb extracting solution;
s3: pouring the andrographis paniculata extract obtained in the step S2 and an adsorbent into a reaction tank, adjusting the temperature to 60 ℃, mixing and removing impurities, stirring at the rotation speed of 120 revolutions per minute for 120 minutes, and filtering the mixture to obtain an impurity-removed extract;
s4: performing column exchange adsorption impurity removal on the impurity-removed extracting solution obtained in the step S3, wherein the column filling material is macroporous adsorption resin or silica gel, so as to obtain an adsorption column;
s5: washing the adsorption column obtained in S4 with pure water to clear the effluent, and eluting the adsorption column with 3 times of 62% alcohol solution to obtain andrographolide eluate;
s6: heating and concentrating the andrographolide eluent obtained in the step S5 under a vacuum condition to 48% of the initial volume of the eluent, wherein the vacuum degree is 0.05MPa, and the temperature is 48 ℃, so as to obtain a concentrated solution, standing the concentrated solution, and carrying out natural cooling crystallization on the concentrated solution, so as to obtain andrographolide crystals;
s7: washing the andrographolide crystals obtained in S6 with pure water, drying after washing, and pulverizing to obtain andrographolide.
EXAMPLE III
The components of each material are as follows: 92% of andrographis paniculata medicinal material, 4% of adsorbent and 4% of additive.
The extraction and separation method of andrographolide comprises the following steps:
s1: selecting andrographis paniculata medicinal materials with uniform length and complete shape, chopping the selected andrographis paniculata medicinal materials to enable the size of the andrographis paniculata medicinal materials to be 0.5-1cm, then putting the chopped andrographis paniculata medicinal materials into a crusher to be crushed, wherein the crushing speed is 420 revolutions per minute, and the crushing time is 24 minutes, so that crushed andrographis paniculata is obtained;
s2: placing the crushed common andrographis herb obtained in the step S1 and additives into an extraction container, adding 95% ethanol to make the ethanol be 18 times of the mass of the common andrographis herb, stirring and extracting under a negative pressure environment, wherein the negative pressure is 0.6 MPa, the stirring speed is 180 revolutions per minute, the extraction temperature is 56 ℃, the extraction time is 3.5 hours, and then filtering the extracted mixed solution to obtain common andrographis herb extracting solution;
s3: pouring the andrographis paniculata extract obtained in the step S2 and an adsorbent into a reaction tank, adjusting the temperature to 62 ℃, mixing and removing impurities, stirring at the rotation speed of 120 revolutions per minute for 120 minutes, and filtering the mixture to obtain an impurity-removed extract;
s4: performing column exchange adsorption impurity removal on the impurity-removed extracting solution obtained in the step S3, wherein the column filling material is macroporous adsorption resin or silica gel, so as to obtain an adsorption column;
s5: washing the adsorption column obtained in S4 with pure water to clear the effluent, and eluting the adsorption column with 3 times of 64% alcohol solution to obtain andrographolide eluate;
s6: heating and concentrating the andrographolide eluent obtained in the step S5 under a vacuum condition until the volume of the eluent is 50% of the initial volume, the vacuum degree is 0.04MPa, and the temperature is 48 ℃, so as to obtain a concentrated solution, standing the concentrated solution, and carrying out natural cooling crystallization on the concentrated solution, so as to obtain andrographolide crystals;
s7: washing the andrographolide crystals obtained in S6 with pure water, drying after washing, and pulverizing to obtain andrographolide.
The method comprises the steps of crushing selected common andrographis herbs to obtain crushed common andrographis herbs, adding an additive and ethanol into the crushed common andrographis herbs, mixing and extracting under the condition of negative pressure to achieve a good extraction effect, filtering to obtain common andrographis herb extracting solution, adsorbing the extracting solution by using an adsorbent, filtering, further removing impurities, adsorbing by using a filling column, eluting after adsorption to obtain eluent to remove most of impurities, carrying out vacuum crystallization, washing andrographolide crystals, crushing to form finished andrographolide products, and enabling the impurities contained in the finished andrographolide products to be less so as to achieve a good using effect.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes by using the technical contents disclosed in the above description to other fields, but any simple modification, equivalent change and change made to the above embodiments according to the technical essence of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims (8)

1. An andrographolide, comprising: the preparation material of the andrographolide is composed of andrographis paniculata medicinal materials, an adsorbent and an additive, and the components of each material are as follows: 82-94% of andrographis paniculata medicinal material, 3-12% of adsorbent and 3-6% of additive.
2. The andrographolide of claim 1, wherein: the adsorbent is one or a mixture of more than one of acid activated clay, bleaching earth and activated carbon in any proportion.
3. The andrographolide of claim 1, wherein: the additive is one or a mixture of more of sodium dodecyl sulfate, methyl amyl alcohol, polyacrylamide, triethyl hexyl phosphoric acid and fatty acid polyglycol ester in any proportion.
4. The andrographolide of claim 1, wherein: the components of each material are as follows: 84% of andrographis paniculata medicinal material, 10% of adsorbent and 6% of additive.
5. The andrographolide of claim 1, wherein: the components of each material are as follows: 88% of andrographis paniculata medicinal material, 7% of adsorbent and 5% of additive.
6. The andrographolide of claim 1, wherein: the components of each material are as follows: 92% of andrographis paniculata medicinal material, 4% of adsorbent and 4% of additive.
7. The method for extracting and separating andrographolide according to claim 1, wherein the steps of: the method comprises the following steps:
s1: selecting andrographis paniculata medicinal materials with uniform length and complete shape, chopping the selected andrographis paniculata medicinal materials to enable the size of the andrographis paniculata medicinal materials to be 0.5-1cm, then putting the chopped andrographis paniculata medicinal materials into a crusher to be crushed, wherein the crushing speed is 300-;
s2: placing the crushed common andrographis herb obtained in the step S1 and additives into an extraction container, adding 85-95% ethanol to make the ethanol be 14-20 times of the mass of the common andrographis herb, stirring and extracting under the negative pressure environment, wherein the negative pressure is 0.4-0.6 MPa, the stirring rotation speed is 120-180 r/min, the extraction temperature is 52-58 ℃, the extraction time is 3-4 hours, and filtering the extracted mixed solution to obtain common andrographis herb extract;
s3: pouring the andrographis paniculata extract obtained in the step S2 and an adsorbent into a reaction tank, adjusting the temperature to 54-64 ℃, mixing and removing impurities, stirring at the rotating speed of 80-120 revolutions per minute for 90-120 minutes, and filtering the mixture to obtain an impurity-removed extract;
s4: performing column exchange adsorption impurity removal on the impurity-removed extracting solution obtained in the step S3, wherein the column filling material is macroporous adsorption resin or silica gel, so as to obtain an adsorption column;
s5: washing the adsorption column obtained in S4 with pure water to clear the effluent, and eluting the adsorption column with 2-3 times of 55-65% alcoholic solution to obtain andrographolide eluate;
s6: heating and concentrating the andrographolide eluent obtained in the step S5 under a vacuum condition to 40-50% of the initial volume of the eluent, wherein the vacuum degree is 0.04-0.06MPa, and the temperature is 40-50 ℃ so as to obtain a concentrated solution, and then standing the concentrated solution, and carrying out natural cooling crystallization on the concentrated solution so as to obtain andrographolide crystals;
s7: washing the andrographolide crystals obtained in S6 with pure water, drying after washing, and pulverizing to obtain andrographolide.
8. The method for extracting and separating andrographolide according to claim 7, wherein the steps of: the alcohol solution in the step S5 is a mixture of ethanol and methanol in any proportion.
CN202110998511.7A 2021-08-27 2021-08-27 Extraction and separation method of andrographolide Pending CN113527234A (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
CN103145660A (en) * 2013-03-25 2013-06-12 成都天台山制药有限公司 Andrographolide and preparation method thereof
CN104140403A (en) * 2014-07-02 2014-11-12 成都通德药业有限公司 Andrographolide separation and purification process
CN105777676A (en) * 2014-12-23 2016-07-20 河南智晶生物科技股份有限公司 Extraction method of andrographolide
CN113045520A (en) * 2021-03-25 2021-06-29 江西新世纪民星动物保健品有限公司 Extraction process of andrographolide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103145660A (en) * 2013-03-25 2013-06-12 成都天台山制药有限公司 Andrographolide and preparation method thereof
CN104140403A (en) * 2014-07-02 2014-11-12 成都通德药业有限公司 Andrographolide separation and purification process
CN105777676A (en) * 2014-12-23 2016-07-20 河南智晶生物科技股份有限公司 Extraction method of andrographolide
CN113045520A (en) * 2021-03-25 2021-06-29 江西新世纪民星动物保健品有限公司 Extraction process of andrographolide

Non-Patent Citations (2)

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Title
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