CN112315992A - Preparation method of high-solubility full-ingredient honeysuckle extract - Google Patents

Preparation method of high-solubility full-ingredient honeysuckle extract Download PDF

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CN112315992A
CN112315992A CN202011296457.3A CN202011296457A CN112315992A CN 112315992 A CN112315992 A CN 112315992A CN 202011296457 A CN202011296457 A CN 202011296457A CN 112315992 A CN112315992 A CN 112315992A
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resin
honeysuckle
embedding
concentration
solution
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胡力飞
徐浪
陈志元
袁咏红
孙代华
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Jingpai Zhengtang Pharmaceutical Co ltd
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Jingpai Zhengtang Pharmaceutical Co ltd
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    • A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
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    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract

The invention discloses a preparation method of a high-solubility full-ingredient honeysuckle extract, which comprises the steps of extracting chlorogenic acid and flavonoid ingredients in honeysuckle by a conventional extraction tank, adsorbing condensate in the extraction process by XDA-8G or LX-3020 resin to recover volatile oil ingredients in the honeysuckle, embedding and backfilling the recovered volatile oil, so that the honeysuckle extract prepared by the method is rich in chlorogenic acid, flavonoid and volatile oil ingredients, and has high water solubility and special and durable fragrance of honeysuckle.

Description

Preparation method of high-solubility full-ingredient honeysuckle extract
Technical Field
The invention relates to the technical field of extraction of medicinal active ingredients, in particular to a preparation method of a high-solubility full-ingredient honeysuckle extract.
Background
Flos Lonicerae (honeyysuckle), also known as Lonicera Japonica and Lonicera Japonica, is the dried bud of plant of Lonicera of Caprifoliaceae. The honeysuckle element attracts much attention due to its wide range of effective chemical components and medicinal value, and is widely used in medical, chemical and pharmacological research. The health-care tea has obvious effects on the aspects of relieving fever, resisting inflammation, resisting bacteria, resisting viruses, resisting oxidation, resisting ultraviolet rays, protecting liver, benefiting gallbladder, enhancing immunity and the like, and simultaneously has certain effects on the aspects of resisting tumors, regulating and controlling blood fat and blood sugar, protecting nerves, treating gynecological diseases and the like due to chemical components and pharmacological action. The honeysuckle flower contains volatile oil, organic acids, flavonoids, iridoids, stigmasterol, phenylalanine, daucosterol, trace elements and other compounds.
At present, researches on extraction and separation of honeysuckle mostly focus on the extraction and separation of chlorogenic acid, and the extraction and separation of volatile oil is also researched. However, when chlorogenic acid or flavonoid ingredients in honeysuckle are extracted and processed, due to the characteristic of low boiling point of the volatile oil, the honeysuckle volatile oil is lost along with the volatilization of the solvent in the concentration and drying processes of the honeysuckle extract, and the prepared extract has no honeysuckle fragrance. The conventional volatile oil extraction device can only extract and enrich volatile oil components, and cannot extract and separate other natural components. And the volatile oil component is fat-soluble component and insoluble in water, thereby limiting the application range.
Disclosure of Invention
The invention aims to provide a preparation method of a high-solubility full-ingredient honeysuckle extract, which has the advantages of simple process, low production cost and easy popularization.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a high-solubility full-ingredient honeysuckle extract comprises the following steps:
(1) extraction: taking the crushed honeysuckle raw material, sieving the honeysuckle raw material by a 30-mesh sieve, adding a solvent with the volume of 8-20 times to extract for three times, extracting for 1-3 hours each time, and combining the extracting solutions.
(2) Disc centrifugation: centrifuging the extractive solution with a disc centrifuge, and collecting centrifugate.
(3) Membrane filtration: and filtering the centrifugate by adopting a ceramic membrane.
(4) Concentration: and (3) carrying out reduced pressure concentration on the filtrate until the solid content is more than 60%, wherein the concentration temperature is 40-75 ℃, and thus obtaining a concentrated solution.
(5) Resin adsorption: and (3) refluxing the condensate in the extraction process in the step (1) to an extraction tank body, and enriching and recovering aroma components in the condensate through adsorption resin, wherein the resin flow rate is required to be 1-2 BV/h.
(6) And (3) elution: and (3) eluting the resin by using 95% or absolute ethyl alcohol to obtain an ethanol eluent rich in volatile oil, wherein the elution flow rate is 1-4 BV/h.
(7) Embedding: embedding the volatile oil by adopting hydroxypropyl beta cyclodextrin to obtain an embedding solution.
(8) Backfilling of flavor components: and (4) adding the embedding solution into the concentrated solution obtained in the step (4) and uniformly mixing.
(9) And (3) drying: and drying the mixed feed liquid by adopting vacuum drying equipment.
Preferably, a mixed solvent of water and ethanol is adopted in the step (1), wherein the concentration of the ethanol is 0-50%.
Preferably, in the step (3), the ceramic membrane has a membrane pore size of 0.02 μm to 1.4. mu.m.
Preferably, the resin in step (5) is an XDA-8G or LX-3020 resin.
Preferably, the resin is eluted with 3 column volumes of ethanol in step (6).
Preferably, the specific embedding step in step (7) is: taking a hydroxypropyl beta cyclodextrin water solution with half volume of the eluent, slowly adding ethanol eluent, carrying out ultrasonic treatment for 20-40 min, filtering by adopting a filter with the pore diameter of 0.45-5 mu m, adding Arabic gum with the volume of 1-3% of the solution, dissolving, and then carrying out ultrasonic treatment for 5-10 min again.
Preferably, the concentration of the hydroxypropyl beta cyclodextrin aqueous solution in the step (7) is 1 to 5 wt%.
Preferably, the temperature in step (9) is controlled to below 70 ℃.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the product has aromatic flavor: the honeysuckle extract prepared by the invention has the unique fragrance of honeysuckle by fragrance recovery and backfilling into the extract, and the fragrance is strong and durable by embedding the honeysuckle volatile oil through an embedding technology.
Secondly, the dissolubility is good: essential oils are fat-soluble components, insoluble in water. However, the honeysuckle volatile oil is embedded by adopting the water-soluble auxiliary material, so that the honeysuckle extract has very good water solubility, and can form a more stable dissolving system after being dissolved by adding the Arabic gum, thereby being more suitable for the application of products in foods and cosmetics.
Thirdly, the solvent selection interval is wide: the method is suitable for extracting water and low alcohol, can effectively avoid the defect that high-concentration alcohol influences the aroma resin enrichment of the condensate, and can better extract other functional components in the honeysuckle while keeping the volatile oil component.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to the process of fig. 1, a method for preparing a high-solubility full-ingredient honeysuckle extract comprises the following steps:
(1) extraction: taking 10Kg of crushed honeysuckle raw material, sieving with a 30-mesh sieve, adding purified water with 20 times of volume for extraction for three times, 3 hours each time, and combining the extracting solutions, wherein the extraction temperature is 95 ℃.
(2) Disc centrifugation: centrifuging the extractive solution with a disc centrifuge, and collecting centrifugate.
(3) Membrane filtration: the centrifugate is filtered by a ceramic membrane, and the aperture of the membrane is 1.4 mu m.
(4) Concentration: and (3) carrying out reduced pressure concentration on the filtrate until the solid content is 61.3%, wherein the concentration temperature is required to be 40-75 ℃.
(5) Resin adsorption: and (2) enriching and recovering the aroma components in the condensate in the extraction process of the step (1) through XDA-8G resin in the process of refluxing the condensate to the extraction tank body, wherein the resin flow rate is required to be 1 BV/h.
(6) And (3) elution: eluting the resin by 95% (3 times of column volume) to obtain ethanol eluent rich in volatile oil at an elution flow rate of 1 BV/h.
(7) Embedding: embedding volatile oil with hydroxypropyl beta cyclodextrin, collecting hydroxypropyl beta cyclodextrin water solution (concentration 1%) of half volume of eluate, slowly adding ethanol eluate, ultrasonically treating for 20min, filtering with 0.45 μm pore diameter titanium rod filter, adding acacia gum 3% of eluate volume, dissolving, and ultrasonically treating for 5 min.
(8) Backfilling of flavor components: and (4) adding the embedding solution into the concentrated solution obtained in the step (4) and uniformly mixing.
(9) And (3) drying: and drying the mixed feed liquid by adopting vacuum drying equipment, and controlling the temperature at 70 ℃ to obtain 1.26Kg of honeysuckle extract. The content of total flavone is detected to be 30.4 percent, the content of chlorogenic acid is detected to be 13.2 percent, and the solubility is detected to be 30g/100g water. The prepared honeysuckle extract can be quickly dissolved in purified water, and is clear and transparent after being dissolved, and the fragrance is lasting and strong.
Example 2
A preparation method of a high-solubility full-ingredient honeysuckle extract comprises the following steps:
(1) extraction: taking 10Kg of crushed honeysuckle raw material, sieving with a 30-mesh sieve, adding 15 times of 30% ethanol, heating, refluxing and extracting for three times, 2 hours each time, and combining the extracting solutions.
(2) Disc centrifugation: centrifuging the extractive solution with a disc centrifuge, and collecting centrifugate.
(3) Membrane filtration: the centrifugate is filtered by ceramic membrane with pore diameter of 0.05 μm.
(4) Concentration: and (3) carrying out reduced pressure concentration on the filtrate until the solid content is 68.5%, wherein the concentration temperature is required to be 40-75 ℃.
(5) Resin adsorption: and (3) enriching and recovering the aroma components in the condensate in the extraction process of the step (1) through XDA-8G resin in the process of refluxing the condensate to the extraction tank body, wherein the resin flow rate is required to be 1.5 BV/h.
(6) And (3) elution: eluting the resin with 95% ethanol (3 times of column volume) to obtain ethanol eluate rich in volatile oil at an elution flow rate of 2.5 BV/h.
(7) Embedding: embedding volatile oil with hydroxypropyl beta cyclodextrin, collecting hydroxypropyl beta cyclodextrin water solution (concentration 3%) of half volume of eluate, slowly adding ethanol eluate, ultrasonically treating for 30min, filtering with 1 μm titanium rod filter, adding acacia gum 2% of eluate volume, dissolving, and ultrasonically treating for 7.5 min.
(8) Backfilling of flavor components: and (4) adding the embedding solution into the concentrated solution obtained in the step (4) and uniformly mixing.
(9) And (3) drying: and drying the mixed feed liquid by adopting vacuum drying equipment, and controlling the temperature at 60 ℃ to obtain 1.19Kg of honeysuckle extract. The content of total flavone is 35.3%, the content of chlorogenic acid is 12.5%, and the solubility is 25g/100g water. The prepared honeysuckle extract can be quickly dissolved in purified water, and is clear and transparent after being dissolved, and the fragrance is lasting and strong.
Example 3
A preparation method of a high-solubility full-ingredient honeysuckle extract comprises the following steps:
(1) extraction: taking 10Kg of crushed honeysuckle raw material, sieving with a 30-mesh sieve, adding 8 times of 50% ethanol, heating, refluxing and extracting for three times, 1-3 hours each time, and combining the extracting solutions.
(2) Disc centrifugation: centrifuging the extractive solution with a disc centrifuge, and collecting centrifugate.
(3) Membrane filtration: the centrifugate is filtered by a ceramic membrane, and the aperture of the membrane is 0.02.
(4) Concentration: and (3) carrying out reduced pressure concentration on the filtrate until the solid content is more than 70.3%, wherein the concentration temperature is required to be 40-75 ℃.
(5) Resin adsorption: and (2) enriching and recovering the aroma components in the condensate in the extraction process of the step (1) through LX-3020 resin in the process of refluxing the condensate to the extraction tank body, wherein the resin flow rate is required to be 2 BV/h.
(6) And (3) elution: and (3) eluting the resin by absolute ethyl alcohol (3 times of the volume of the column) to obtain an ethanol eluent rich in volatile oil, wherein the elution flow rate is 4 BV/h.
(7) Embedding: embedding volatile oil with hydroxypropyl beta cyclodextrin, collecting hydroxypropyl beta cyclodextrin water solution (concentration 5%) of half volume of eluate, slowly adding ethanol eluate, performing ultrasonic treatment for 40min, filtering with 5 μm titanium rod filter, adding acacia gum of 1% volume of eluate, dissolving, and performing ultrasonic treatment for 10 min.
(8) Backfilling of flavor components: and (4) adding the embedding solution into the concentrated solution obtained in the step (4) and uniformly mixing.
(9) And (3) drying: drying the mixed feed liquid by using vacuum drying equipment at the temperature of below 50 ℃ to obtain 1.23Kg of honeysuckle extract. The content of total flavone is detected to be 37.2 percent, the content of chlorogenic acid is detected to be 12.7 percent, and the solubility is detected to be 20g/100g water. The prepared honeysuckle extract can be quickly dissolved in purified water, and is clear and transparent after being dissolved, and the fragrance is lasting and strong.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (8)

1. A preparation method of a high-solubility full-ingredient honeysuckle extract is characterized by comprising the following steps: the method comprises the following steps:
(1) extraction: taking the crushed honeysuckle raw material, sieving the honeysuckle raw material by a 30-mesh sieve, adding a solvent with the volume of 8-20 times to extract for three times, extracting for 1-3 hours each time, and combining the extracting solutions.
(2) Disc centrifugation: centrifuging the extractive solution with a disc centrifuge, and collecting centrifugate.
(3) Membrane filtration: and filtering the centrifugate by adopting a ceramic membrane.
(4) Concentration: and (3) carrying out reduced pressure concentration on the filtrate until the solid content is more than 60%, wherein the concentration temperature is 40-75 ℃, and thus obtaining a concentrated solution.
(5) Resin adsorption: and (3) refluxing the condensate in the extraction process in the step (1) to an extraction tank body, and enriching and recovering aroma components in the condensate through adsorption resin, wherein the resin flow rate is required to be 1-2 BV/h.
(6) And (3) elution: and (3) eluting the resin by using 95% or absolute ethyl alcohol to obtain an ethanol eluent rich in volatile oil, wherein the elution flow rate is 1-4 BV/h.
(7) Embedding: embedding the volatile oil by adopting hydroxypropyl beta cyclodextrin to obtain an embedding solution.
(8) Backfilling of flavor components: and (4) adding the embedding solution into the concentrated solution obtained in the step (4) and uniformly mixing.
(9) And (3) drying: and drying the mixed feed liquid by adopting vacuum drying equipment.
2. The method of claim 1, wherein: in the step (1), a mixed solvent of water and ethanol is adopted, wherein the concentration of the ethanol is 0-50%.
3. The method of claim 1, wherein: in the step (3), the membrane aperture of the ceramic membrane is 0.02-1.4 μm.
4. The method of claim 1, wherein: the resin in the step (5) is XDA-8G or LX-3020 resin.
5. The method of claim 1, wherein: and (6) eluting the resin by using ethanol with 3 times of column volume.
6. The method of claim 1, wherein: the specific embedding step in the step (7) is as follows: taking a hydroxypropyl beta cyclodextrin water solution with half volume of the eluent, slowly adding ethanol eluent, carrying out ultrasonic treatment for 20-40 min, filtering by adopting a filter with the pore diameter of 0.45-5 mu m, adding Arabic gum with the volume of 1-3% of the solution, dissolving, and then carrying out ultrasonic treatment for 5-10 min again.
7. The method of claim 6, wherein: the concentration of the hydroxypropyl beta cyclodextrin water solution in the step (7) is 1 to 5 weight percent.
8. The method of claim 1, wherein: the temperature in the step (9) is controlled below 70 ℃.
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113337341A (en) * 2021-06-07 2021-09-03 劲牌持正堂药业有限公司 Method for comprehensively utilizing effective components and aroma of sweet osmanthus

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Application publication date: 20210205