CN107151259A - The method that a kind of solid residue after extraction to citrus pectin is comprehensively utilized - Google Patents
The method that a kind of solid residue after extraction to citrus pectin is comprehensively utilized Download PDFInfo
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Abstract
The invention discloses the method that the solid residue after a kind of extraction to citrus pectin is comprehensively utilized, comprise the following steps：(1) aurantiamarin is rough, (2) aurantiamarin is refined, the acquisition of (3) tangeritin extract, the acquisition of (4) citrus feed addictive and the acquisition of (5) alkaline extract solution.The present invention has technique simple, mild condition, environment-friendly and the characteristics of be easy to industrialized production, realizes the complete utilization that citrus pectin extracts solid residue, making the remarkable in economical benefits of orange peel deep processing increases, and belongs to the production technology of environmental protection.
Description
Technical field
The invention belongs to field of deep processing of farm products, it is related to the solid residue after a kind of extraction to citrus pectin and integrates
The method utilized.
Background technology
China is citrus fruit producing country the biggest in the world, and total output is up to 36,000,000 tons.Orange peel is citrus fruit
Pectin content in the Main By product of processing, orange peel is up to 20~30%, far above other fruit peels.Carried 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 carrying for environmental consciousness
Reduction production cost and environmental protection treatment pressure are badly in need of in height, pectin production enterprise.It is worth noting that, containing quite in orange peel
Flavone compound (aurantiamarin, narirutin, naringin etc.) and substantial amounts of dietary fiber are (cellulose, hemicellulose, oligomeric
Sugar etc.) and crude protein, various vitamins, trace element etc. (iron, manganese, zinc, copper, selenium), with 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.
The orange peel to extracting pectin announced at present integrate the patent of extraction and application it has been reported that such as patent
201410195428.6 disclose a kind of method 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, and the pectin in residue is then extracted again, and because pectin extraction is rear, extraction is deposited
In mass transfer barrier, cause the recovery rate of aurantiamarin relatively low (＜ 3%), and easily add impurities in aurantiamarin crude product, because
This also needs to be dissolved with alkaline ethanol solution when refined, and carries out that quadratic acid is heavy can just to obtain the aurantiamarin of high-purity, in addition should
Patent is not carried out to the residue after extraction to be comprehensively utilized.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 is returned while pectin is extracted
Orange peel fiber has been received, but flavone compound not higher to added value in orange peel is extracted.
The method that the solid residue developed as can be seen here after a kind of extraction to citrus pectin is comprehensively utilized, can not only show
The problem of writing the economic benefit of raising orange peel deep processing, and advantageously account for the sector wasting of resources and a large amount of discharge waste residues,
Have important practical significance.
The content of the invention
The solid residue that the technical problems to be solved by the invention are to provide after a kind of extraction to citrus pectin is integrated
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 a kind of solid residue after extraction to citrus pectin is comprehensively utilized, comprises the following steps：
(1) aurantiamarin is rough：The raw material residue extracted after citrus pectin is washed with water to pH >=6, alkalescence is subsequently added
The aqueous solution is extracted to residue, is obtained alkaline extract solution and is slightly carried residue；Ultrafiltration removal of impurities is carried out to the alkaline extract solution, will
Obtained ultrafiltration permeate concentration, obtains evaporation water and concentrate, by the concentrate acid precipitation, the precipitation is washed with water
To water colorless is gone out, aurantiamarin crude product is obtained；
(2) aurantiamarin is refined：After the aurantiamarin crude product obtained in step (1) is extracted with hot ethanol, filter while hot, will
Filtered after the extract solution crystallisation by cooling arrived, obtained crystal is obtained into aurantiamarin finished product by vacuum drying；Ethanol in mother liquor
It is distilled to recover, obtains medicinal extract；
(3) acquisition of tangeritin extract：The residue obtained in step (1) is washed with water to pH≤8, ethanol is added
Aqueous solution heating and refluxing extraction, is filtered while hot, filtrate ultra-filtration and separation, obtains solid residue and ultrafiltration permeate, by the ultrafiltration
After ethanol distillation in permeate is reclaimed, vacuum distillation is carried out to the slurry of residual, residue is obtained, by the residue and
The medicinal extract obtained in step (2) is dried in vacuo after merging, or is dried in vacuo respectively, obtains tangeritin extract；
(4) acquisition of citrus feed addictive：The solid residue obtained in step (3) is cleaned to without ethanol with water and remained
Dry, crush afterwards, obtain citrus feed addictive；
(5) acquisition of alkaline extract solution：The alkalescence that the evaporation water obtained in step (1) is used in preparation steps (1) is carried
Take liquid.
In step (1), it is described extract citrus pectin after raw material residue water content be 75~85%, size be 3~
10mm；Described 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, pH are 11.5~12.5, temperature
Spend for 20~30 DEG C, mixing speed is 30~60rpm, filtered after extracting 40~90 minutes, collect 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 extract solution and
Slightly carry residue.
The ultrafiltration retaining molecular weight that ultrafiltration is used described in step (1) is 3000~8000 dalton, described ultrafiltration
The condition of the concentration of permeate is：Vacuum is 1~3Kpa, and thickening temperature is 60~65 DEG C, is concentrated into ultrafiltration permeate original
The 1/5~1/10 of volume.
In step (1), the condition of the acid precipitation is：With sulfuric acid or aqueous hydrochloric acid solution by concentrate adjust to pH 3~
4.5,6~12h is kept at 4~10 DEG C, is precipitated after filtering.
In step (2), the method that the aurantiamarin crude product is extracted with hot ethanol is：By aurantiamarin crude product according to 1:10~1:
20g/mL solid-liquid mass volume ratio is mixed with ethanol, is heated to reflux at 65~75 DEG C 60~100 minutes, filtrate is collected respectively
With undissolved solid, undissolved solid is extracted again with same process, total extraction time is 2~3 times, and merging filtrate is obtained
To extract solution；The crystallisation by cooling condition is：The extract solution is cooled to 4~10 DEG C, white crystal is formed, growing the grain 6~
12h。
In step (3), the condition of the addition ethanol water heating and refluxing extraction is：Use 70~95%v/v second
Alcohol solution, solid-liquid mass volume ratio is 1:2~1:5g/mL, is heated to reflux 60~100 minutes at 60~80 DEG C；It is described super
Filter separation is carried out using molecular cut off for the ceramic membrane of 5~150,000 dalton, it is preferred that ultrafiltrate temperature is 40 DEG C.
In step (2) and (3), ethanol distillation reclaim condition be, 77~79 DEG C of vapo(u)rizing temperature.
In step (3), the vacuum of the vacuum distillation is 1~3Kpa, and the temperature of vacuum distillation is 55~60 DEG C；It is described
Vacuum drying vacuum is 1~3Kpa, and 55~60 DEG C, the vacuum drying time is 4~6h.
In step (4), the drying is：Flowed after removing the moisture in solid residue with screw extrusion dewaterer with belt
Dryer is dehydrated, it is preferred that drying temperature is 80 DEG C, and the water content of residue is down into below 10wt%；After drying
Residue be ground into it is powdered.
Beneficial effect：Compared with prior art, present invention process is simple, mild condition, and citrus pectin life is being greatly decreased
While producing the waste residue of discharge, can produce high pure hesperidin (coarse extraction rate up to more than 5%, the extraction rate reached after refining
More than 3.5%, content of hesperidin in finished product is up to more than 95%), (extraction rate reached more than 4%, general flavone content reaches tangeritin
More than 60%), the product such as citrus feed addictive (extraction rate reached more than 75%), is avoiding the loss of orange peel functional component
Meanwhile, eliminate the discharge of solid residue.On the other hand, the water that steams formed in aurantiamarin concentration process is back to extraction,
Avoid a large amount of discharges of waste water.It can be seen that, the present invention improves the utilization rate of orange peel raw material, in the same of increase economic benefit
When, it is thus also avoided that extract pollution of the waste residue to environment.
Brief description of the drawings
Fig. 1 is the flow chart that the solid residue after being extracted to citrus pectin is comprehensively utilized.
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
Apply the content described by example and be merely to illustrate the present invention, without should be also without limitation on sheet described in detail in claims
Invention.
The recovery rate of product refers to target product obtained in 100g over dry citrus peel raw materials in embodiment.
Pectin extraction residue involved in the present invention be using document (research of orange peel pectous extracting method, grain with
Food industry, 2012,19 (5)) obtain after the acidity extraction pectin that is provided, the concrete technology condition used for：With hydrochloric acid
Sour, 85 DEG C of the extraction temperature as extracting, and 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 peels of 100g (water content 75~80%) can obtain the wet pericarps of 90~220g by above method
(water content 75%~90%), these residues are used in following examples.
Embodiment 1
To extract the extraction that the orange peel after pectin (water content 83%) carries out aurantiamarin for raw material, solid-to-liquid ratio is 1：2, regulation
To pH=12.5, extraction time is 90 minutes, and Extracting temperature is 30 DEG C, and mixing speed is to obtain filtrate after 60rpm, filtering, is pressed
This condition is extracted 2 times, is merged all filtrates and is obtained alkaline extract solution.Alkaline extract solution uses molecular cut off for 3000 dalton
Milipore filter ultrafiltration, collect ultrafiltration permeate.
Ultrafiltration permeate vacuum distillation is concentrated into the 1/10 of original volume, concentration condition is：Vacuum is 1Kpa, and temperature is
65℃.Concentrate is adjusted to pH 3 with sulfuric acid, and precipitated after keeping 6h, filtering at 4 DEG C, and with 4 DEG C of deionized waters
Washing is precipitated to out water colorless, as aurantiamarin crude product, and the wherein content of aurantiamarin is 83.6%, and the recovery rate of aurantiamarin is
5.2%.
Aurantiamarin crude product is refined, aurantiamarin crude product is according to 1:20 solid-to-liquid ratio is mixed with 95% ethanol water,
Heating and refluxing extraction 60 minutes, are filtered while hot at 65 DEG C, and filtrate and undissolved solid are collected respectively, undissolved solid is pressed with
Upper condition heating and refluxing extraction 2 times is simultaneously filtered.Merge above filtrate and obtain extract solution, extract solution is cooled to 4 DEG C, growing the grain 6h,
Form crystal, the crystal being collected by filtration is dried in vacuo, vacuum is 1~3Kpa, 55 DEG C, dry 4h, acquisition aurantiamarin into
Product.To crystalline mother solution progress ethanol distillation recovery, 78 DEG C of vapo(u)rizing temperature, the solid of precipitation is used 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 uses molecular cut off to be 50,000 dalton
Ceramic membrane carry out ultra-filtration and separation, collect ultrafiltration permeate.Ethanol in distillation recovery ultrafiltration permeate, 78 DEG C of vapo(u)rizing temperature,
Reclaim after ethanol, vacuum distillation is carried out to the slurry of residual, vacuum is 1Kpa, and 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 is 1Kpa, 55 DEG C, dries 4h, that is, obtains citrus 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 is cleaned to without ethanol with running water to be remained, the powder after being dehydrated, drying
Broken to become citrus feed addictive, recovery rate is 77.3%.
Embodiment 2
To extract the extraction that the orange peel after pectin (water content 81%) carries out aurantiamarin for raw material, solid-to-liquid ratio is 1：3, regulation
To pH=12.0, extraction time is 40 minutes, and Extracting temperature is 25 DEG C, and mixing speed is to obtain filtrate after 30rpm, filtering, is pressed
This condition is extracted 2 times, is merged all filtrates and is obtained alkaline extract solution.Alkaline extract solution uses molecular cut off for 5000 dalton
Milipore filter ultrafiltration, collect ultrafiltration permeate.
Ultrafiltration permeate vacuum distillation is concentrated into the 1/5 of original volume, concentration condition is：Vacuum is 2Kpa, and temperature is
60℃.Concentrate is adjusted to pH 3.5 with sulfuric acid, and precipitated after keeping 8h, filtering at 8 DEG C, and with 4 DEG C of deionizations
Water washing is precipitated to out water colorless, as aurantiamarin crude product, and the wherein content of aurantiamarin is 81.2%, and the recovery rate of aurantiamarin is
5.1%.
Aurantiamarin crude product is refined, aurantiamarin crude product is according to 1:10 solid-to-liquid ratio is mixed with 95% ethanol solution, and 70
Heating and refluxing extraction 80 minutes, are filtered while hot at DEG C, and filtrate and undissolved solid are collected respectively, undissolved solid is pressed more than
Condition heating and refluxing extraction 3 times is simultaneously filtered.Merge above filtrate and obtain extract solution, extract solution is cooled to 8 DEG C, growing the grain 8h, shape
Into crystal, the crystal being collected by filtration is dried in vacuo, and vacuum is 2Kpa, 60 DEG C, dries 6h, obtains aurantiamarin finished product.It is right
Crystalline mother solution progress ethanol distillation recovery, 77 DEG C of vapo(u)rizing temperature, the solid of precipitation is used 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 from the residue after aurantiamarin extraction heating and refluxing extraction citrus general flavone, solid-to-liquid ratio is
1:5, heating and refluxing extraction 80 minutes, are filtered while hot at 65 DEG C, and the filtrate of collection uses molecular cut off to be 100,000 dalton
Ceramic membrane carry out ultra-filtration and separation, collect ultrafiltration permeate.Ethanol in distillation recovery ultrafiltration permeate, 77 DEG C of vapo(u)rizing temperature,
Reclaim after ethanol, vacuum distillation is carried out to the slurry of residual, vacuum is 2Kpa, and 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 is 2Kpa, 60 DEG C, dries 6h, that is, obtains citrus 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 is cleaned to without ethanol with running water to be remained, the powder after being dehydrated, drying
Broken to become citrus feed addictive, recovery rate is 75.8%.
Embodiment 3
To extract the extraction that the orange peel after pectin (water content 88%) carries out aurantiamarin for raw material, solid-to-liquid ratio is 1：4, with reality
The evaporation water collected when alkali extracting solution is concentrated in example 1 is applied as extractant, regulation to pH=12.5, extraction time is 60 minutes,
Extracting temperature is 20 DEG C, and mixing speed is to obtain filtrate after 50rpm, filtering, is extracted 2 times by this condition, merges all filtrates and obtains
To alkaline extract solution.Alkaline extract solution uses molecular cut off for the milipore filter ultrafiltration of 8000 dalton, collects ultrafiltration permeate.
Ultrafiltration permeate vacuum distillation is concentrated into the 1/8 of original volume, concentration condition is：Vacuum is 3Kpa, and temperature is
65℃.Concentrate is adjusted to pH 4.0 with hydrochloric acid, and precipitated after keeping 12h, filtering at 10 DEG C, and with 4 DEG C go from
Sub- water washing is precipitated to out water colorless, as aurantiamarin crude product, and the wherein content of aurantiamarin is 83%, and the recovery rate of aurantiamarin is
5.3%.
Aurantiamarin crude product is refined, aurantiamarin crude product is according to 1:15 solid-to-liquid ratio is mixed with 95% ethanol solution, and 70
Heating and refluxing extraction 80 minutes, are filtered while hot at DEG C, and filtrate and undissolved solid are collected respectively, undissolved solid is pressed more than
Condition heating and refluxing extraction 2 times is simultaneously filtered.Merge above filtrate and obtain extract solution, extract solution is cooled to 8 DEG C, growing the grain 8h, shape
Into crystal, the crystal being collected by filtration is dried in vacuo, and vacuum is 3Kpa, 58 DEG C, dries 5h, obtains aurantiamarin finished product.It is right
Crystalline mother solution progress ethanol distillation recovery, 77 DEG C of vapo(u)rizing temperature, the solid of precipitation is used 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 from the residue after aurantiamarin extraction heating and refluxing extraction citrus general flavone, solid-to-liquid ratio is
1:4, heating and refluxing extraction 100 minutes, are filtered while hot at 65 DEG C, and the filtrate of collection uses molecular cut off to be 150,000 dalton
Ceramic membrane carry out ultra-filtration and separation, collect ultrafiltration permeate.Ethanol in distillation recovery ultrafiltration permeate, 79 DEG C of vapo(u)rizing temperature,
Reclaim after ethanol, vacuum distillation is carried out to the slurry of residual, vacuum is 3Kpa, and 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 is 3Kpa, 58 DEG C, dries 5h, that is, obtains citrus 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 is cleaned to without ethanol with running water to be remained, the powder after being dehydrated, drying
Broken to become citrus feed addictive, recovery rate is 76.5%.
Embodiment 4
To extract the extraction that the orange peel after pectin (water content 75%) carries out aurantiamarin for raw material, solid-to-liquid ratio is 1：4, with reality
The evaporation water collected when alkali extracting solution is concentrated in example 2 is applied as extractant, regulation to pH=12.0, extraction time is 50 minutes,
Extracting temperature is 25 DEG C, and mixing speed is to obtain filtrate after 60rpm, filtering, is extracted 3 times by this condition, merges all filtrates and obtains
To alkaline extract solution.Alkaline extract solution uses molecular cut off for the milipore filter ultrafiltration of 5000 dalton, collects ultrafiltration permeate.
Ultrafiltration permeate vacuum distillation is concentrated into the 1/10 of original volume, concentration condition is：Vacuum is 1Kpa, and temperature is
65℃.Concentrate is adjusted to pH 3.5 with hydrochloric acid, and precipitated after keeping 8h, filtering at 4 DEG C, and with 4 DEG C of deionizations
Water washing is precipitated to out water colorless, as aurantiamarin crude product, and the wherein content of aurantiamarin is 87.3%, and the recovery rate of aurantiamarin is
6.1%.
Aurantiamarin crude product is refined, aurantiamarin crude product is according to 1:18 solid-to-liquid ratio is mixed with 95% ethanol solution, and 70
Heating and refluxing extraction 100 minutes, are filtered while hot at DEG C, and filtrate and undissolved solid are collected respectively, undissolved solid is pressed with
Upper condition heating and refluxing extraction 3 times is simultaneously filtered.Merge above filtrate and obtain extract solution, extract solution is cooled to 5 DEG C, growing the grain 12h,
Crystal is formed, the crystal being collected by filtration is dried in vacuo, vacuum is 1Kpa, 60 DEG C, dries 4h, obtains aurantiamarin finished product.
To crystalline mother solution progress ethanol distillation recovery, 78 DEG C of vapo(u)rizing temperature, the solid of precipitation is used as medicinal extract.Orange peel in aurantiamarin finished product
Glycosides content is that the aurantiamarin recovery rate after 95.8%, refinement treatment is 4.8%.
Using 95% ethanol solution from the residue after aurantiamarin extraction heating and refluxing extraction citrus general flavone, solid-to-liquid ratio is
1:5, heating and refluxing extraction 90 minutes, are filtered while hot at 65 DEG C, and the filtrate of collection uses molecular cut off to be 80,000 dalton
Ceramic membrane carries out ultra-filtration and separation, collects ultrafiltration permeate.The ethanol in ultrafiltration permeate is distilled to recover, 78 DEG C of vapo(u)rizing temperature is returned
Receive after ethanol, vacuum distillation is carried out to the slurry of residual, vacuum is 1Kpa, and 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 is 1Kpa, 60 DEG C, dries 4h, that is, obtains 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 is cleaned to without ethanol with running water to be remained, the powder after being dehydrated, drying
Broken to become citrus feed addictive, recovery rate is 73.0%.
Claims (10)
1. the method that the solid residue after a kind of extraction to citrus pectin is comprehensively utilized, it is characterised in that including following step
Suddenly：
(1) aurantiamarin is rough：The raw material residue extracted after citrus pectin is washed with water to pH >=6, alkalescence is subsequently added water-soluble
Liquid is extracted to residue, is obtained alkaline extract solution and is slightly carried residue；Ultrafiltration removal of impurities is carried out to the alkaline extract 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 is refined：After the aurantiamarin crude product obtained in step (1) is extracted with hot ethanol, filter while hot, by what is obtained
Filtered after extract solution crystallisation by cooling, obtained crystal is obtained into aurantiamarin finished product by vacuum drying；Ethanol distillation in mother liquor
Reclaim, obtain medicinal extract；
(3) acquisition of tangeritin extract：The residue obtained in step (1) is washed with water to pH≤8, ethanol is added water-soluble
Liquid heating and refluxing extraction, is filtered while hot, filtrate ultra-filtration and separation, obtains solid residue and ultrafiltration permeate, and the ultrafiltration is passed through
After ethanol distillation in liquid is reclaimed, vacuum distillation is carried out to the slurry of residual, residue is obtained, by the residue and step
(2) medicinal extract obtained in is dried in vacuo after merging, or is dried in vacuo respectively, obtains tangeritin extract；
(4) acquisition of citrus feed addictive：The solid residue obtained in step (3) is cleaned to after being remained without ethanol dry with water
Dry, crushing, obtains citrus feed addictive；
(5) acquisition of alkaline extract solution：The alkaline extract solution that the evaporation water obtained in step (1) is used in preparation steps (1).
2. according to the method described in claim 1, it is characterised in that in step (1), the raw material extracted after citrus pectin is residual
The water content of slag is 75~85%, and size is 3~10mm；Described alkaline aqueous solution is sodium hydrate aqueous solution.
3. according to the method described in claim 1, it is characterised in that in step (1), the mass volume ratio of the solid-liquid of the extraction
For 1：2~1：5g/mL, pH are 11.5~12.5, and temperature is 20~30 DEG C, and mixing speed is 30~60rpm, extracts 40~90 points
Filtered after clock, collect filtrate and filter residue, filter residue is extracted again with same process, total extraction time is 2~3 times, and institute is merged respectively
There are filtrate and all filter residues to obtain alkaline extract solution and slightly carry residue.
4. according to the method described in claim 1, it is characterised in that the milipore filter retention point that ultrafiltration is used described in step (1)
Son amount is 3000~8000 dalton, and the condition of the concentration of described ultrafiltration permeate is：Vacuum is 1~3Kpa, concentration temperature
Spend for 60~65 DEG C, be concentrated into the 1/5~1/10 of ultrafiltration permeate initial volume.
5. according to the method described in claim 1, it is characterised in that in step (1), the condition of the acid precipitation is：Use sulphur
Acid or hydrochloric acid adjust concentrate to pH 3~4.5, and 6~12h is kept at 4~10 DEG C, is precipitated after filtering.
6. according to the method described in claim 1, it is characterised in that in step (2), the aurantiamarin crude product is extracted with hot ethanol
Method be：By aurantiamarin crude product according to 1:10~1:20g/mL solid-liquid mass volume ratio is mixed with ethanol, at 65~75 DEG C
Under be heated to reflux 60~100 minutes, filtrate and undissolved solid are collected respectively, undissolved solid is carried again with same process
Take, total extraction time is 2~3 times, and merging filtrate obtains extract solution；The crystallisation by cooling condition is：The extract solution is cooled
To 4~10 DEG C, white crystal, 6~12h of growing the grain are formed.
7. according to the method described in claim 1, it is characterised in that in step (3), the addition ethanol water is heated to reflux
The condition of extraction is：Using 70~95%v/v ethanol water, 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 uses the ceramic membrane that molecular cut off is 5~150,000 dalton
Carry out.
8. the condition that according to the method described in claim 1, it is characterised in that in step (2) and (3), ethanol distillation is reclaimed is,
77~79 DEG C of vapo(u)rizing temperature.
9. according to the method described in claim 1, it is characterised in that in step (3), the vacuum of the vacuum distillation be 1~
3Kpa, the temperature of vacuum distillation is 55~60 DEG C；The vacuum drying vacuum is 1~3Kpa, 55~60 DEG C, vacuum drying
Time be 4~6h.
10. according to the method described in claim 1, it is characterised in that in step (4), the drying is：It is dehydrated with screw extrusion
Dehydrated after moisture in machine removing solid residue with belt percolation dryer, the water content of residue is down to 10wt%
Below；Dried residue is ground into powdered.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129584A (en) * | 2017-12-27 | 2018-06-08 | 中国农业科学院农产品加工研究所 | It is a kind of to realize pectin and flavones while the method for extraction in citrus peel residue |
| CN115746164A (en) * | 2022-10-24 | 2023-03-07 | 梅州市飞龙果业有限公司 | Method for extracting active ingredients from orange peel residues |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3536138B2 (en) * | 1994-09-12 | 2004-06-07 | 江崎グリコ株式会社 | Prevention of crystal precipitation of hesperidin and prevention of white turbidity in liquid foods containing tangerines or tangerine juice |
| CN1810819A (en) * | 2006-03-03 | 2006-08-02 | 华东理工大学 | Process of preparing tangeritin from orange peel |
| CN105669800A (en) * | 2016-03-03 | 2016-06-15 | 湖南省农产品加工研究所 | Method of combined extraction of essential oil, pectin, hesperidin, synephrine and limonin from citrus |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3536138B2 (en) * | 1994-09-12 | 2004-06-07 | 江崎グリコ株式会社 | Prevention of crystal precipitation of hesperidin and prevention of white turbidity in liquid foods containing tangerines or tangerine juice |
| CN1810819A (en) * | 2006-03-03 | 2006-08-02 | 华东理工大学 | Process of preparing tangeritin from orange peel |
| CN105669800A (en) * | 2016-03-03 | 2016-06-15 | 湖南省农产品加工研究所 | Method of combined extraction of essential oil, pectin, hesperidin, synephrine and limonin from citrus |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129584A (en) * | 2017-12-27 | 2018-06-08 | 中国农业科学院农产品加工研究所 | It is a kind of to realize pectin and flavones while the method for extraction in citrus peel residue |
| CN115746164A (en) * | 2022-10-24 | 2023-03-07 | 梅州市飞龙果业有限公司 | Method for extracting active ingredients from orange peel residues |
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