CN107151259B - The method that solid residue after a kind of pair of citrus pectin extraction is comprehensively utilized - Google Patents
The method that solid residue after a kind of pair of citrus pectin extraction is comprehensively utilized Download PDFInfo
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Abstract
The method that solid residue after extracting the invention discloses a kind of pair of citrus pectin is comprehensively utilized, comprising the following steps: (1) aurantiamarin crude, the purification of (2) aurantiamarin, the acquisition of (3) tangeritin extract, the acquisition of (4) citrus feed addictive and (5) alkalinity extracting solution acquisition.The present invention has the characteristics that simple process, mild condition, environmental-friendly and easy to industrialized production, realizes the complete utilization that citrus pectin extracts solid residue, increases the remarkable in economical benefits of orange peel deep processing, belong to environmentally protective production technology.
Description
Technical field
The invention belongs to field of deep processing of farm products, are related to the solid residue after a kind of pair of citrus pectin is extracted and integrate
The method utilized.
Background technique
China is the world's largest citrus fruit producing country, and total output is up to 36,000,000 tons.Orange peel is citrus fruit
The Main By product of processing, the pectin content in orange peel are much higher than other fruit peels up to 20~30%.It is mentioned from orange peel
Pectin is taken to realize industrialized production in China, but the citrus peel residue after pectin extraction still accounts for the 70~80% of material quality,
China is not high to this fraction solids residue utilization rate, is largely landfilled.With the aggravation of product competition and mentioning for environmental consciousness
Height, pectin production enterprise are badly in need of reducing production cost and environmental protection treatment pressure.It is worth noting that, containing comparable in orange peel
Flavone compound (aurantiamarin, narirutin, naringin etc.) and a large amount of dietary fiber are (cellulose, hemicellulose, oligomeric
Sugar etc.) and crude protein, various vitamins, microelement etc. (iron, manganese, zinc, copper, selenium), there is certain medical value and battalion
Effect is supported, therefore the product obtained after deep processing can be used for medicine, health food and feedstuff industry.
That announces at present carries out the patent of comprehensive extraction and application it has been reported that such as patent to the orange peel for extracting pectin
201410195428.6 disclose the method for a kind of combined extracting aurantiamarin and pectin from orange peel, and this method is first to citrus
Skin carries out that alkali carries acid is heavy to obtain aurantiamarin therein, then extracts the pectin in residue again, and since pectin extraction is rear, extraction is deposited
In mass transfer barrier, it is lower (< 3%) to lead to the recovery rate of aurantiamarin, and is easy to add impurities in aurantiamarin crude product, because
This also needs to be dissolved with alkaline ethanol solution in purification, and carries out the heavy aurantiamarin that just can get high-purity of quadratic acid, furthermore should
Patent does not carry out comprehensive utilization to the residue after extraction.Patent 201610339258.3 discloses one kind and discloses a kind of utilization
The method that citrus peel classification obtains pectin, orange peel fiber and orange peel fermented beverage, this method are returned while extracting pectin
Orange peel fiber has been received, but the higher flavone compound of added value in orange peel has not been extracted.
It can be seen that developing the method that the solid residue after a kind of pair of citrus pectin is extracted is comprehensively utilized, can not only show
The problem of writing the economic benefit for improving orange peel deep processing, and advantageously accounting for the sector wasting of resources and a large amount of discharge waste residues,
It has important practical significance.
Summary of the invention
Solid residue after extracting technical problem to be solved by the invention is to provide a kind of pair of citrus pectin integrates
The method utilized.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
The method that solid residue after a kind of pair of citrus pectin extraction is comprehensively utilized, comprising the following steps:
(1) aurantiamarin is crude: the raw material residue after extraction citrus pectin being washed with water to pH >=6, alkalinity is then added
Aqueous solution extracts residue, obtains alkaline extracting solution and slightly mentions residue；Ultrafiltration removal of impurities is carried out to the alkaline extracting solution, it will
Obtained ultrafiltration permeate concentration, obtains evaporation water and concentrate for the concentrate acid precipitation and the precipitating is washed with water
To water colorless out, aurantiamarin crude product is obtained；
(2) aurantiamarin refines: after aurantiamarin crude product obtained in step (1) is extracted with hot ethanol, filter while hot, will
To extracting solution crystallisation by cooling after filter, by obtained crystal by vacuum drying obtain aurantiamarin finished product；Ethyl alcohol in mother liquor
It is distilled to recover, obtains medicinal extract；
(3) acquisition of tangeritin extract: residue obtained in step (1) is washed with water to pH≤8, ethyl alcohol is added
Aqueous solution heating and refluxing extraction, is filtered while hot, and filtrate ultra-filtration and separation obtains solid residue and ultrafiltration permeate, by the ultrafiltration
After ethanol distillation recycling in permeate, remaining slurry is evaporated under reduced pressure, residue is obtained, by the residue and
Medicinal extract obtained in step (2) is dried in vacuo after merging, or is dried in vacuo respectively, and tangeritin extract is obtained；
(4) acquisition of citrus feed addictive: the solid residue obtained in step (3) is washed with water to no ethyl alcohol and is remained
Dry afterwards, crushing, obtains citrus feed addictive；
(5) acquisition of alkaline extracting solution: alkalinity of the evaporation water in preparation steps (1) obtained in step (1) is mentioned
Take liquid.
In step (1), the water content for extracting the raw material residue after citrus pectin is 75~85%, having a size of 3~
10mm；The alkaline aqueous solution is sodium hydrate aqueous solution.
In step (1), the mass volume ratio of the solid-liquid of the extraction is 1:2~1:5g/mL, and pH is 11.5~12.5, temperature
Degree is 20~30 DEG C, and mixing speed is 30~60rpm, is filtered after extracting 40~90 minutes, collects filtrate and filter residue, filter residue is with phase
Extracted again with technique, total extraction time is 2~3 times, merge all filtrates respectively and all filter residues obtain alkaline extracting solution and
Slightly mention residue.
The ultrafiltration retaining molecular weight that ultrafiltration described in step (1) uses is 3000~8000 dalton, the ultrafiltration
The condition of the concentration of permeate are as follows: vacuum degree is 1~3Kpa, and thickening temperature is 60~65 DEG C, and it is original to be concentrated into ultrafiltration permeate
The 1/5~1/10 of volume.
In step (1), the condition of the acid precipitation are as follows: with sulfuric acid or aqueous hydrochloric acid solution by concentrate be adjusted to pH 3~
4.5,6~12h is kept at 4~10 DEG C, is precipitated after filtering.
In step (2), method that the aurantiamarin crude product is extracted with hot ethanol are as follows: by aurantiamarin crude product according to 1:10~1:
The solid-liquid mass volume ratio of 20g/mL is mixed with ethyl alcohol, is heated to reflux 60~100 minutes at 65~75 DEG C, is collected filtrate respectively
With undissolved solid, undissolved solid is extracted again with same process, total extraction time is 2~3 times, and merging filtrate obtains
To extracting solution；The crystallisation by cooling condition are as follows: the extracting solution is cooled to 4~10 DEG C, forms white crystal, growing the grain 6~
12h。
In step (3), the condition that ethanol water heating and refluxing extraction is added are as follows: use the second of 70~95%v/v
Alcohol solution, solid-liquid mass volume ratio are 1:2~1:5g/mL, are heated to reflux at 60~80 DEG C 60~100 minutes；It is described super
Filter separation is carried out using the ceramic membrane that molecular cut off is 5~150,000 dalton, it is preferred that ultrafiltrate temperature is 40 DEG C.
In step (2) and (3), the condition of ethanol distillation recycling is 77~79 DEG C of vapo(u)rizing temperature.
In step (3), the vacuum degree of the vacuum distillation is 1~3Kpa, and the temperature of vacuum distillation is 55~60 DEG C；It is described
Vacuum drying vacuum degree is 1~3Kpa, and 55~60 DEG C, the vacuum drying time is 4~6h.
In step (4), the drying are as follows: flowed with after the moisture in screw extrusion dewaterer removing solid residue with belt
Dryer is dehydrated, it is preferred that drying temperature is 80 DEG C, and the water content of residue is down to 10wt% or less；After drying
Residue be pulverized into powder.
The utility model has the advantages that compared with prior art, present invention process is simple, mild condition is raw citrus pectin is greatly decreased
While producing the waste residue of discharge, can producing high pure hesperidin, (up to 5% or more, the recovery rate after purification reaches coarse extraction rate
3.5% or more, content of hesperidin in finished product is up to 95% or more), (up to 4% or more, general flavone content reaches recovery rate tangeritin
60% or more), the products such as citrus feed addictive (recovery rate up to 75% or more) are avoiding the loss of orange peel functional component
Meanwhile eliminating the discharge of solid residue.On the other hand, the water that steams formed in aurantiamarin concentration process is back to extract,
Avoid a large amount of discharges of waste water.As it can be seen that the present invention improves the utilization rate of orange peel raw material, increasing the same of economic benefit
When, it is thus also avoided that extract pollution of the waste residue to environment.
Detailed description of the invention
Fig. 1 is the flow chart that the solid residue after extracting to citrus pectin is comprehensively utilized.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
The recovery rate of product refers to target product obtained in 100g over dry citrus peel raw material in embodiment.
Pectin extraction residue according to the present invention be using document (research of orange peel pectous extracting method, grain with
Food industry, 2012,19 (5)) provided by obtain after acidity extraction pectin, the concrete technology condition of use are as follows: with hydrochloric acid
As acid is extracted, 85 DEG C of extraction temperature, solid-to-liquid ratio (in terms of dry weight, mass volume ratio g:mL) 1:20, hydrolysis pH is 2.0, extraction
Time 90min.The fresh citrus peel of 100g (water content 75~80%) can get the wet pericarp of 90~220g by above method
(water content 75%~90%), these residues are used in following embodiment.
Embodiment 1
It is the extraction that raw material carries out aurantiamarin to extract the orange peel after pectin (water content 83%), solid-to-liquid ratio 1:2 is adjusted
To pH=12.5, extraction time is 90 minutes, and Extracting temperature is 30 DEG C, and mixing speed 60rpm obtains filtrate after filtering, presses
This condition is extracted 2 times, is merged all filtrates and is obtained alkaline extracting solution.Alkaline extracting solution uses molecular cut off for 3000 dalton
Ultrafiltration membrane ultrafiltration, collect ultrafiltration permeate.
The vacuum distillation of ultrafiltration permeate is concentrated into the 1/10 of original volume, condition is concentrated are as follows: vacuum degree 1Kpa, temperature are
65℃.Concentrate is adjusted to pH 3 with sulfuric acid, and keeps 6h at 4 DEG C, is precipitated after filtering, and with 4 DEG C of deionized waters
Washing is precipitated to out water colorless, as aurantiamarin crude product, and wherein the content of aurantiamarin is 83.6%, and the recovery rate of aurantiamarin is
5.2%.
Aurantiamarin crude product is refined, aurantiamarin crude product is mixed according to the solid-to-liquid ratio of 1:20 with 95% ethanol water,
Heating and refluxing extraction 60 minutes, are filtered while hot at 65 DEG C, collect filtrate and undissolved solid respectively, to undissolved solid press with
Upper condition heating and refluxing extraction 2 times simultaneously filters.Merge the above filtrate and obtain extracting solution, extracting solution is cooled to 4 DEG C, growing the grain 6h,
Form crystal, the crystal being collected by filtration is dried in vacuo, and vacuum degree is 1~3Kpa, 55 DEG C, dry 4h, obtain aurantiamarin at
Product.Ethanol distillation recycling is carried out to crystalline mother solution, 78 DEG C of vapo(u)rizing temperature, the solid of precipitation is as medicinal extract.In aurantiamarin finished product
Content of hesperidin is 95.3%, and aurantiamarin recovery rate is 3.9%.
Using 70% ethanol water from aurantiamarin extraction after residue in heating and refluxing extraction citrus general flavone, solid-to-liquid ratio
For 1:3, heating and refluxing extraction 60 minutes, are filtered while hot at 80 DEG C, and the filtrate of collection is 50,000 dalton using molecular cut off
Ceramic membrane carry out ultra-filtration and separation, collect ultrafiltration permeate.The ethyl alcohol being distilled to recover in ultrafiltration permeate, 78 DEG C of vapo(u)rizing temperature,
After recycling ethyl alcohol, remaining slurry is evaporated under reduced pressure, vacuum degree 1Kpa, vapo(u)rizing temperature is 55 DEG C, and residue is leaching
Cream.It is merged with the medicinal extract obtained before and is dried in vacuo, vacuum degree 1Kpa, 55 DEG C, dry 4h, i.e. acquisition citrus is yellow
Ketone extract.The recovery rate of tangeritin extract is 4.8%, and wherein general flavone content is 65.6%.
The solid residue obtained after extraction tangeritin, which is cleaned with tap water to no ethyl alcohol, to be remained, powder after being dehydrated, being dried
It is broken to become citrus feed addictive, recovery rate 77.3%.
Embodiment 2
It is the extraction that raw material carries out aurantiamarin to extract the orange peel after pectin (water content 81%), solid-to-liquid ratio 1:3 is adjusted
To pH=12.0, extraction time is 40 minutes, and Extracting temperature is 25 DEG C, and mixing speed 30rpm obtains filtrate after filtering, presses
This condition is extracted 2 times, is merged all filtrates and is obtained alkaline extracting solution.Alkaline extracting solution uses molecular cut off for 5000 dalton
Ultrafiltration membrane ultrafiltration, collect ultrafiltration permeate.
The vacuum distillation of ultrafiltration permeate is concentrated into the 1/5 of original volume, condition is concentrated are as follows: vacuum degree 2Kpa, temperature are
60℃.Concentrate is adjusted to pH 3.5 with sulfuric acid, and keeps 8h at 8 DEG C, is precipitated after filtering, and with 4 DEG C of deionizations
Water washing is precipitated to out water colorless, as aurantiamarin crude product, and wherein the content of aurantiamarin is 81.2%, and the recovery rate of aurantiamarin is
5.1%.
Aurantiamarin crude product is refined, aurantiamarin crude product is mixed according to the solid-to-liquid ratio of 1:10 with 95% ethanol solution, and 70
Heating and refluxing extraction 80 minutes, are filtered while hot at DEG C, collect filtrate and undissolved solid respectively, undissolved solid is pressed more than
Condition heating and refluxing extraction 3 times simultaneously filters.Merge the above filtrate and obtain extracting solution, extracting solution is cooled to 8 DEG C, growing the grain 8h, shape
At crystal, the crystal being collected by filtration is dried in vacuo, and vacuum degree 2Kpa, 60 DEG C, dry 6h obtains aurantiamarin finished product.It is right
Crystalline mother solution carries out ethanol distillation recycling, and 77 DEG C of vapo(u)rizing temperature, the solid of precipitation is as medicinal extract.Aurantiamarin in aurantiamarin finished product
Content is 95.6%, and the aurantiamarin recovery rate after refinement treatment is 3.6%.
Using 80% ethanol solution, heating and refluxing extraction citrus general flavone, solid-to-liquid ratio are from the residue after aurantiamarin extraction
1:5, heating and refluxing extraction 80 minutes, are filtered while hot at 65 DEG C, and the filtrate of collection is 100,000 dalton using molecular cut off
Ceramic membrane carry out ultra-filtration and separation, collect ultrafiltration permeate.The ethyl alcohol being distilled to recover in ultrafiltration permeate, 77 DEG C of vapo(u)rizing temperature,
After recycling ethyl alcohol, remaining slurry is evaporated under reduced pressure, vacuum degree 2Kpa, vapo(u)rizing temperature is 60 DEG C, and residue is leaching
Cream.It is merged with the medicinal extract obtained before and is dried in vacuo, vacuum degree 2Kpa, 60 DEG C, dry 6h, i.e. acquisition citrus is yellow
Ketone extract.The recovery rate of tangeritin extract is 5.3%, and wherein general flavone content is 63.4%.
The solid residue obtained after extraction tangeritin, which is cleaned with tap water to no ethyl alcohol, to be remained, powder after being dehydrated, being dried
It is broken to become citrus feed addictive, recovery rate 75.8%.
Embodiment 3
It is the extraction that raw material carries out aurantiamarin, solid-to-liquid ratio 1:4, with reality to extract the orange peel after pectin (water content 88%)
The evaporation water collected when alkali extracting solution is concentrated in example 1 to be applied as extractant, is adjusted to pH=12.5, extraction time is 60 minutes,
Extracting temperature is 20 DEG C, and mixing speed 50rpm obtains filtrate after filtering, extracts 2 times by this condition, merges all filtrates and obtain
To alkaline extracting solution.Alkaline extracting solution uses molecular cut off for the ultrafiltration membrane ultrafiltration of 8000 dalton, collects ultrafiltration permeate.
The vacuum distillation of ultrafiltration permeate is concentrated into the 1/8 of original volume, condition is concentrated are as follows: vacuum degree 3Kpa, temperature are
65℃.Concentrate is adjusted to pH 4.0 with hydrochloric acid, and keeps 12h at 10 DEG C, is precipitated after filtering, and with 4 DEG C go from
Sub- water washing is precipitated to out water colorless, as aurantiamarin crude product, and wherein the content of aurantiamarin is 83%, and the recovery rate of aurantiamarin is
5.3%.
Aurantiamarin crude product is refined, aurantiamarin crude product is mixed according to the solid-to-liquid ratio of 1:15 with 95% ethanol solution, and 70
Heating and refluxing extraction 80 minutes, are filtered while hot at DEG C, collect filtrate and undissolved solid respectively, undissolved solid is pressed more than
Condition heating and refluxing extraction 2 times simultaneously filters.Merge the above filtrate and obtain extracting solution, extracting solution is cooled to 8 DEG C, growing the grain 8h, shape
At crystal, the crystal being collected by filtration is dried in vacuo, and vacuum degree 3Kpa, 58 DEG C, dry 5h obtains aurantiamarin finished product.It is right
Crystalline mother solution carries out ethanol distillation recycling, and 77 DEG C of vapo(u)rizing temperature, the solid of precipitation is as medicinal extract.Aurantiamarin in aurantiamarin finished product
Content is 95.0%, and the aurantiamarin recovery rate after refinement treatment is 4.1%.
Using 90% ethanol solution, heating and refluxing extraction citrus general flavone, solid-to-liquid ratio are from the residue after aurantiamarin extraction
1:4, heating and refluxing extraction 100 minutes, are filtered while hot at 65 DEG C, and the filtrate of collection is 150,000 dalton using molecular cut off
Ceramic membrane carry out ultra-filtration and separation, collect ultrafiltration permeate.The ethyl alcohol being distilled to recover in ultrafiltration permeate, 79 DEG C of vapo(u)rizing temperature,
After recycling ethyl alcohol, remaining slurry is evaporated under reduced pressure, vacuum degree 3Kpa, vapo(u)rizing temperature is 60 DEG C, and residue is leaching
Cream.It is merged with the medicinal extract obtained before and is dried in vacuo, vacuum degree 3Kpa, 58 DEG C, dry 5h, i.e. acquisition citrus is yellow
Ketone extract.The recovery rate of tangeritin extract is 4.5%, and wherein general flavone content is 62.0%.
The solid residue obtained after extraction tangeritin, which is cleaned with tap water to no ethyl alcohol, to be remained, powder after being dehydrated, being dried
It is broken to become citrus feed addictive, recovery rate 76.5%.
Embodiment 4
It is the extraction that raw material carries out aurantiamarin, solid-to-liquid ratio 1:4, with reality to extract the orange peel after pectin (water content 75%)
The evaporation water collected when alkali extracting solution is concentrated in example 2 to be applied as extractant, is adjusted to pH=12.0, extraction time is 50 minutes,
Extracting temperature is 25 DEG C, and mixing speed 60rpm obtains filtrate after filtering, extracts 3 times by this condition, merges all filtrates and obtain
To alkaline extracting solution.Alkaline extracting solution uses molecular cut off for the ultrafiltration membrane ultrafiltration of 5000 dalton, collects ultrafiltration permeate.
The vacuum distillation of ultrafiltration permeate is concentrated into the 1/10 of original volume, condition is concentrated are as follows: vacuum degree 1Kpa, temperature are
65℃.Concentrate is adjusted to pH 3.5 with hydrochloric acid, and keeps 8h at 4 DEG C, is precipitated after filtering, and with 4 DEG C of deionizations
Water washing is precipitated to out water colorless, as aurantiamarin crude product, and wherein the content of aurantiamarin is 87.3%, and the recovery rate of aurantiamarin is
6.1%.
Aurantiamarin crude product is refined, aurantiamarin crude product is mixed according to the solid-to-liquid ratio of 1:18 with 95% ethanol solution, and 70
Heating and refluxing extraction 100 minutes, are filtered while hot at DEG C, collect filtrate and undissolved solid respectively, to undissolved solid press with
Upper condition heating and refluxing extraction 3 times simultaneously filters.Merge the above filtrate and obtain extracting solution, extracting solution is cooled to 5 DEG C, growing the grain 12h,
Crystal is formed, the crystal being collected by filtration is dried in vacuo, and vacuum degree 1Kpa, 60 DEG C, dry 4h obtains aurantiamarin finished product.
Ethanol distillation recycling is carried out to crystalline mother solution, 78 DEG C of vapo(u)rizing temperature, the solid of precipitation is as medicinal extract.Orange peel in aurantiamarin finished product
Glycosides content is 95.8%, and the aurantiamarin recovery rate after refinement treatment is 4.8%.
Using 95% ethanol solution, heating and refluxing extraction citrus general flavone, solid-to-liquid ratio are from the residue after aurantiamarin extraction
1:5, heating and refluxing extraction 90 minutes, are filtered while hot at 65 DEG C, and the filtrate of collection is 80,000 dalton using molecular cut off
Ceramic membrane carries out ultra-filtration and separation, collects ultrafiltration permeate.The ethyl alcohol being distilled to recover in ultrafiltration permeate, returns by 78 DEG C of vapo(u)rizing temperature
After receiving ethyl alcohol, remaining slurry is evaporated under reduced pressure, vacuum degree 1Kpa, vapo(u)rizing temperature is 55 DEG C, and residue is medicinal extract.
It is merged with the medicinal extract obtained before and is dried in vacuo, vacuum degree 1Kpa, 60 DEG C, dry 4h, i.e. acquisition tangeritin
Extract.The recovery rate of tangeritin extract is 5.1%, and wherein general flavone content is 64.4%.
The solid residue obtained after extraction tangeritin, which is cleaned with tap water to no ethyl alcohol, to be remained, powder after being dehydrated, being dried
It is broken to become citrus feed addictive, recovery rate 73.0%.
Claims (10)
1. the method that the solid residue after a kind of pair of citrus pectin extraction is comprehensively utilized, which is characterized in that including following step
It is rapid:
(1) aurantiamarin is crude: the raw material residue after extraction citrus pectin being washed with water to pH >=6, it is water-soluble that alkalinity is then added
Liquid extracts residue, obtains alkaline extracting solution and slightly mentions residue；Ultrafiltration removal of impurities is carried out to the alkaline extracting solution, will be obtained
The concentration of ultrafiltration permeate, obtain evaporation water and concentrate, by the concentrate acid precipitation, described be precipitated to out be washed with water
Water colorless obtains aurantiamarin crude product；
(2) aurantiamarin refines: after aurantiamarin crude product obtained in step (1) is extracted with hot ethanol, filtering while hot, by what is obtained
It is filtered after extracting solution crystallisation by cooling, obtained crystal is obtained into aurantiamarin finished product by vacuum drying；Ethanol distillation in mother liquor
Recycling, obtains medicinal extract；
(3) acquisition of tangeritin extract: residue will be slightly mentioned obtained in step (1) and is washed with water to pH≤8, ethyl alcohol is added
Aqueous solution heating and refluxing extraction, is filtered while hot, and filtrate ultra-filtration and separation obtains solid residue and ultrafiltration permeate, by the ultrafiltration
After ethanol distillation recycling in permeate, remaining slurry is evaporated under reduced pressure, residue is obtained, by the residue and
Medicinal extract obtained in step (2) is dried in vacuo after merging, or is dried in vacuo respectively, and tangeritin extract is obtained；
(4) acquisition of citrus feed addictive: the solid residue obtained in step (3) is washed with water to no ethyl alcohol and is done after remaining
Dry, crushing, obtains citrus feed addictive；
(5) acquisition of alkaline extracting solution: by evaporation water obtained in step (1) for the alkaline extracting solution in preparation steps (1).
2. the method according to claim 1, wherein the raw material after the extraction citrus pectin is residual in step (1)
The water content of slag is 75~85%, having a size of 3~10mm；The alkaline aqueous solution is sodium hydrate aqueous solution.
3. the method according to claim 1, wherein in step (1), the mass volume ratio of the solid-liquid of the extraction
It is 11.5~12.5 for 1:2~1:5g/mL, pH, temperature is 20~30 DEG C, and mixing speed is 30~60rpm, extracts 40~90 points
It is filtered after clock, collects filtrate and filter residue, filter residue are extracted again with same process, total extraction time is 2~3 times, merges institute respectively
There are filtrate and all filter residues to obtain alkaline extracting solution and slightly mentions residue.
4. the method according to claim 1, wherein the ultrafiltration membrane retention point that ultrafiltration described in step (1) uses
Son amount is 3000~8000 dalton, the condition of the concentration of the ultrafiltration permeate are as follows: vacuum degree is 1~3Kpa, concentration temperature
Degree is 60~65 DEG C, is concentrated into the 1/5~1/10 of ultrafiltration permeate initial volume.
5. the method according to claim 1, wherein in step (1), the condition of the acid precipitation are as follows: use sulphur
Concentrate is adjusted to pH 3~4.5 by sour or hydrochloric acid, and 6~12h is kept at 4~10 DEG C, is precipitated after filtering.
6. the method according to claim 1, wherein the aurantiamarin crude product is extracted with hot ethanol in step (2)
Method are as follows: aurantiamarin crude product is mixed according to the solid-liquid mass volume ratio of 1:10~1:20g/mL with ethyl alcohol, at 65~75 DEG C
Under be heated to reflux 60~100 minutes, collect filtrate and undissolved solid respectively, undissolved solid mentioned again with same process
It takes, total extraction time is 2~3 times, and merging filtrate obtains extracting solution；The crystallisation by cooling condition are as follows: the extracting solution cools down
To 4~10 DEG C, white crystal, 6~12h of growing the grain are formed.
7. the method according to claim 1, wherein the addition ethanol water is heated to reflux in step (3)
The condition of extraction are as follows: using the ethanol water of 70~95%v/v, the mass volume ratio of solid-liquid is 1:2~1:5g/mL, 60
It is heated to reflux at~80 DEG C 60~100 minutes；The ultra-filtration and separation is the ceramic membrane of 5~150,000 dalton using molecular cut off
It carries out.
8. the method according to claim 1, wherein in step (2) and (3), the condition of ethanol distillation recycling is,
77~79 DEG C of vapo(u)rizing temperature.
9. the method according to claim 1, wherein in step (3), the vacuum degree of the vacuum distillation is 1~
3Kpa, the temperature of vacuum distillation are 55~60 DEG C；The vacuum drying vacuum degree is 1~3Kpa, 55~60 DEG C, is dried in vacuo
Time be 4~6h.
10. the method according to claim 1, wherein in step (4), the drying are as follows: be dehydrated with screw extrusion
It is dehydrated after moisture in machine removing solid residue with belt percolation dryer, the water content of residue is down to 10wt%
Below；Residue after drying is pulverized into powder.
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