CN108409813A - A method of continuously extracting flaxseed gum and flax lignan from flaxseed meal - Google Patents
A method of continuously extracting flaxseed gum and flax lignan from flaxseed meal Download PDFInfo
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- CN108409813A CN108409813A CN201810274730.9A CN201810274730A CN108409813A CN 108409813 A CN108409813 A CN 108409813A CN 201810274730 A CN201810274730 A CN 201810274730A CN 108409813 A CN108409813 A CN 108409813A
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- flax
- lignan
- flaxseed
- linseed
- extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/18—Acyclic radicals, substituted by carbocyclic rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Abstract
The present invention relates to the methods that flaxseed gum and flax lignan are continuously extracted from flaxseed meal, and this approach includes the following steps：1) linseed separation of hull from kernel：Flaxseed meal pulverizes and sieves, and collects upper layer flax seed husk and lower layer's linseed kernel after sieving respectively；2) extraction of flaxseed gum：Using flax seed husk as raw material, microwave radiation technology hot water extraction flaxseed gum；3) extraction of flax lignan：Degummed flax seeds shell is mixed into extraction with ethanolic sodium hydroxide solution, obtains hurds lignan；4) purifying of flax lignan：Using macroporous resin purification flax lignan crude product, the flax lignan of high-purity is obtained.The present invention continuously extracts flaxseed gum and flax lignan from flaxseed meal; provide a kind of new way making full use of flaxseed meal; simultaneously efficiently method is provided a convenient to prepare a variety of linseed active ingredients; it is effectively utilized linseed liquefaction by-product; reduce target product production cost; with low energy consumption, product recovery rate height, high financial profit, the advantages such as low in the pollution of the environment, it is suitable for scale production.
Description
Technical field
The present invention relates to the method for the effective component extracting from flaxseed meal, more particularly to one kind is continuous from flaxseed meal
The method for extracting flaxseed gum and flax lignan.
Background technology
Flax is a kind of ancient and important oil crops.About 400,000 tons of the linseed yield in China in 2013, is only second to
Canada occupies second place of the world.It has been investigated that containing multiple nutritional components in linseed, (not rich in ω -3 such as linseed oil
Saturated fatty acid), protein, dietary fiber etc., linseed also contains that there are many biologically active active ingredients, including flax
Seed glue, flax lignan, ring flax peptide etc..
Flaxseed gum is present in flax seed husk, accounts for about the 8-10% of linseed weight, and main ingredient is polysaccharide.Flax glue
With very strong emulsification, thickening function, food additives are can be used as applied in refrigerated products, meat products, Flour product, also may be used
Applied to fields such as cosmetics, pharmacy, papermaking.In addition, flaxseed gum is as a kind of soluble dietary fiber, to certain heavy metals
Poisoning symptom has detoxifying effect, the work(such as incidence also with beauty, weight-reducing, reduction diabetes and coronary heart disease
Effect.Lignan is the diphenol chemical combination that the higher plant to be formed is coupled by two coniferyl alcohol residues being present in plant cell wall
Object, majority exist in the form of dimer, also there is a small number of tripolymers and the tetramer.Lignan is widely present in a variety of wholefoods
In, such as cereal, water fruits and vegetables, the lignan content highest wherein in linseed, content be higher by 75 than other 66 kinds of food
~80 times.Flax lignan is present in flax seed husk, and the content in linseed is 1%~4%, and main component is that open loop is different
Larch turpentine phenol (secoisolariciresinol, SECO).Studies have shown that the precursor of SECO is the different larch turpentine phenol of open loop two
Glucoside (secoisolariciresinol diglucoside, SDG), is usually also considered as the component of flax lignan
One of.In recent years, lignan has been proved by numerous scientific researchers athero- with anti-oxidant, anticancer, prevention diabetes and artery
Many potential physiological activity such as hardening.
Flaxseed gum and linseed lignan all have multiple biological activities and a health-care efficacy, and linseed is in China master at present
It is used to prepare linseed oil, as the linseed oil processing byproduct of high added value, by flaxseed gum and linseed lignan
Effectively successive extract out has huge economic benefit and social benefit from flaxseed meal.Outside Current Domestic
Research focuses primarily upon the respective independent extraction purification of the two, and is mostly extracted from the full seed of flax, such as Chinese patent
CN101838406B reports the method that flaxseed gum and flax lignan are continuously extracted from the full seed of flax；Chinese patent
CN102850414B reports the method that flaxseed gum and lignan are continuously extracted from flax seed peel；Still lack about from flax
The report of successive extract flaxseed gum and flax lignan in the seed dregs of rice.
It is presently disclosed to have with the relevant patent of Linseed pigment extraction：Chinese patent application publication No.
CN101759731B, CN101838406A, the content that these patents are related to are relatively low to the recovery rate of flaxseed gum, and are extracting
Cheng Zhonghui destroys the acidic polysaccharose in flaxseed gum.So far, domestic about the continuously and efficiently extraction point from flaxseed meal
There is not been reported for method from flaxseed gum and flax lignan.
Invention content
To solve the disadvantage that the prior art and shortcoming, the primary purpose of the present invention is that providing a kind of from flaxseed meal
In continuously extract the method for flaxseed gum and lignan.It is obtained it is another object of the present invention to provide above-mentioned preparation method
Flaxseed gum and flax lignan.
The object of the invention is achieved through the following technical solutions：
A method of it continuously extracting flaxseed gum and flax lignan from flaxseed meal, includes the following steps：
1) linseed separation of hull from kernel：Flaxseed meal after oil expression collects upper layer flax respectively through pulverizer grinding and sieving
Seed shell and lower layer's linseed kernel；
2) extraction of flaxseed gum：The flax seed husk obtained using step 1) is sub- using microwave radiation technology hot water extraction as raw material
Numb seed glue collects upper layer mucus and lower layer's degummed flax seeds shell respectively after 3500~5000r/min centrifuges 20~30min；It will
Upper layer mucus is concentrated under reduced pressure, and 50%~90% ethanol solution precipitation is stood, and 3500~5000r/min centrifuges 20~30min,
Precipitation is taken, flaxseed gum is obtained after vacuum freeze drying after washing；
3) extraction of flax lignan：The degummed flax seeds shell that step 2) is obtained presses matter with ethyl alcohol-sodium hydroxide solution
The ratio between amount 1:10~20 mix, and 2~8h is extracted under conditions of 40 DEG C~70 DEG C, and 2500~3500r/min centrifuges 10~30min,
Supernatant is taken, supernatant pH value is adjusted to neutrality with hydrochloric acid；Supernatant is concentrated under reduced pressure, and hurds wood is obtained after vacuum freeze drying
Phenol element；
4) purifying of flax lignan：By the hurds lignan of step 3) acquisition and 50%~80% ethanol water
It is made into the solution of a concentration of 4~8mg/mL, with macroporous resin purification, stripping liquid is collected, is concentrated under reduced pressure, after vacuum freeze drying
To the flax lignan of high-purity.
A kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal as described above, step 1) institute
The linseed separation of hull from kernel stated is to realize efficiently separating for flax seed husk benevolence according to flax seed husk benevolence toughness and the difference of grain size, sub-
Numb seed smashes it through 20~30 mesh sieve.
A kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal as described above, step 2) institute
The condition for the microwave radiation technology hot water extraction stated is：The mass ratio of flax seed husk and water is 1:20~30, extraction temperature 60~100
DEG C, 40~60min of extraction time, 600~800W of output power, 600~900r/min of mixing speed.
A kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal as described above, step 3) institute
The ethyl alcohol stated-sodium hydroxide solution parameter is：The content of ethyl alcohol be 40%~90%, concentration of sodium hydroxide solution be 0.2~
2mol/L。
A kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal as described above, step 4) institute
In the flax lignan purification process stated, big pore resin be AB-8 macroreticular resins, at room temperature adsorption time be 4~for 24 hours, solution
Inhale the time be 2~for 24 hours, stripping liquid be 30%~70% ethanol water.
The invention has the advantages that：
(1) present invention continuously extracts flaxseed gum and flax lignan from flaxseed meal, provides one kind and makes full use of
The new way of flaxseed meal, while being provided a convenient and efficient method to prepare a variety of linseed active ingredients, effectively drop
Low production cost, have low energy consumption, product recovery rate height, high financial profit, the advantages such as low in the pollution of the environment, proper scale metaplasia
Production.
(2) present invention provides convenience linseed separation of hull from kernel for the extraction purification of different linseed active ingredients, and
Linseed source of the present invention derives from a wealth of sources, and method is simple and reliable, to expand the application range of linseed, improving its economic and society
Benefit is laid a good foundation.
Specific implementation mode
The present invention is further described below by way of specific embodiment, but the invention does not limit the present invention in any way
The range of patent protection.
Embodiment 1
The flaxseed meal after oil expression is taken, is crushed, 20 mesh sieve is crossed, the upper layer flax seed husk after sieving is collected respectively and lower layer is sub-
Numb seed benevolence；By mass ratio it is 1 by flax seed husk and water:20 by mixing, and it is 60 DEG C, microwave output power to keep extraction temperature
600W, mixing speed 600r/min, microwave radiation technology hot water extraction flaxseed gum, after extracting 40min, extraction mixture is packed into centrifugation
Cylinder centrifuges 20min after slightly cooling down under 3500r/min, collects upper layer mucus and lower layer's flax seed husk respectively；Upper layer mucus is subtracted
Pressure concentration, controls the addition of absolute ethyl alcohol, until ethanol solution concentration is 50% in solution, stirs alcohol precipitation, 2h is stood, by alcohol precipitation
Liquid centrifuges 20min under 3500r/min, and precipitation, washing is taken to remove ethyl alcohol, flaxseed gum is obtained after vacuum freeze drying.This
Flaxseed gum yield is 28.6% (opposite flax seed husk) under part.
By degummed flax seeds shell and ethyl alcohol-sodium hydroxide solution, (content of ethyl alcohol is 40%, and concentration of sodium hydroxide solution is
0.2mol/L) press mass ratio 1:10 mix, and 2h is extracted under conditions of 40 DEG C.Mixed liquor is centrifuged in 2500r/min later
10min takes supernatant, and supernatant pH value is adjusted to neutrality with hydrochloric acid solution.Supernatant is concentrated under reduced pressure, after vacuum freeze drying
To hurds lignan；The ethanol water of hurds lignan and 50% is made into the solution of a concentration of 4mg/mL, uses AB-8
Macroreticular resin is purified：Oscillation absorption 4h at room temperature filters off adsorption liquid after resin adsorption saturation；30% ethanol water is added
Solution, oscillation desorption 2h, is filtered at room temperature.Stripping liquid is collected, is concentrated under reduced pressure, flax of high-purity is obtained after vacuum freeze drying
Lignan, gained flax lignan purity are 75.8%.
Embodiment 2
The flaxseed meal after oil expression is taken, is crushed, 30 mesh sieve is crossed, the upper layer flax seed husk after sieving is collected respectively and lower layer is sub-
Numb seed benevolence；By mass ratio it is 1 by flax seed husk and water:30 by mixing, and it is 100 DEG C, microwave output power to keep extraction temperature
800W, mixing speed 900r/min, microwave radiation technology hot water extraction flaxseed gum, after extracting 60min, extraction mixture is packed into centrifugation
Cylinder centrifuges 30min after slightly cooling down under 5000r/min, collects upper layer mucus and lower layer's flax seed husk respectively；Upper layer mucus is subtracted
Pressure concentration, controls the addition of absolute ethyl alcohol, until ethanol solution concentration is 90% in solution, stirs alcohol precipitation, 2h is stood, by alcohol precipitation
Liquid centrifuges 30min under 5000r/min, and precipitation, washing is taken to remove ethyl alcohol, flaxseed gum is obtained after vacuum freeze drying.This
Flaxseed gum yield is 29.5% (opposite flax seed husk) under part.
By degummed flax seeds shell and ethyl alcohol-sodium hydroxide solution, (content of ethyl alcohol is 90%, and concentration of sodium hydroxide solution is
2mol/L) press mass ratio 1:20 mix, and 8h is extracted under conditions of 70 DEG C.Mixed liquor is centrifuged in 3500r/min later
30min takes supernatant, and supernatant pH value is adjusted to neutrality with hydrochloric acid solution.Supernatant is concentrated under reduced pressure, after vacuum freeze drying
To hurds lignan；The ethanol water of hurds lignan and 80% is made into the solution of a concentration of 8mg/mL, uses AB-8
Macroreticular resin is purified：Oscillation absorption for 24 hours, after resin adsorption saturation, filters off adsorption liquid at room temperature；70% ethanol water is added
Solution, at room temperature oscillation desorption for 24 hours, are filtered.Stripping liquid is collected, is concentrated under reduced pressure, the Asia of high-purity is obtained after vacuum freeze drying
Numb lignan, gained flax lignan purity are 78.6%.
Embodiment 3
The flaxseed meal after oil expression is taken, is crushed, 20 mesh sieve is crossed, the upper layer flax seed husk after sieving is collected respectively and lower layer is sub-
Numb seed benevolence；By mass ratio it is 1 by flax seed husk and water:25 by mixing, and it is 80 DEG C, microwave output power to keep extraction temperature
700W, mixing speed 700r/min, microwave radiation technology hot water extraction flaxseed gum, after extracting 50min, extraction mixture is packed into centrifugation
Cylinder centrifuges 25min after slightly cooling down under 4000r/min, collects upper layer mucus and lower layer's flax seed husk respectively；Upper layer mucus is subtracted
Pressure concentration, controls the addition of absolute ethyl alcohol, until ethanol solution concentration is 70% in solution, stirs alcohol precipitation, 2h is stood, by alcohol precipitation
Liquid centrifuges 25min under 4000r/min, and precipitation, washing is taken to remove ethyl alcohol, flaxseed gum is obtained after vacuum freeze drying.This
Flaxseed gum yield is 30.7% (opposite flax seed husk) under part.
By degummed flax seeds shell and ethyl alcohol-sodium hydroxide solution, (content of ethyl alcohol is 70%, and concentration of sodium hydroxide solution is
1mol/L) press mass ratio 1:15 mix, and 5h is extracted under conditions of 55 DEG C.Mixed liquor is centrifuged in 3500r/min later
20min takes supernatant, and supernatant pH value is adjusted to neutrality with hydrochloric acid solution；Supernatant is concentrated under reduced pressure, after vacuum freeze drying
To hurds lignan.The ethanol water of hurds lignan and 65% is made into the solution of a concentration of 6mg/mL, uses AB-8
Macroreticular resin is purified：Oscillation absorption 14h at room temperature filters off adsorption liquid after resin adsorption saturation；50% ethanol water is added
Solution, oscillation desorption 13h, is filtered at room temperature.Stripping liquid is collected, is concentrated under reduced pressure, the Asia of high-purity is obtained after vacuum freeze drying
Numb lignan, gained flax lignan purity are 80.9%.
Claims (5)
1. a kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal, which is characterized in that including following
Step：
1) linseed separation of hull from kernel：Flaxseed meal after oil expression collects the upper layer after sieving respectively through pulverizer grinding and sieving
Flax seed husk and lower layer's linseed kernel；
2) extraction of flaxseed gum：The flax seed husk obtained using step 1) is raw material, using microwave radiation technology hot water extraction linseed
Glue, mixed liquor centrifuge 20~30min through 3500~5000r/min, collect upper layer mucus and lower layer's degummed flax seeds shell respectively；
Upper layer mucus is concentrated under reduced pressure, 50%~90% ethanol solution alcohol precipitation, is stood, 3500~5000r/min centrifugations 20~
30min takes precipitation, flaxseed gum is obtained after vacuum freeze drying after washing；
3) extraction of flax lignan：Degummed flax seeds shell and the ethyl alcohol-sodium hydroxide solution that step 2) is obtained by quality it
Than 1:10~20 mix, and 2~8h is extracted under conditions of 40 DEG C~70 DEG C, and 2500~3500r/min centrifuges 10~30min, takes
Clear liquid adjusts supernatant pH value to neutrality with hydrochloric acid；Supernatant is concentrated under reduced pressure, and hurds wood phenol is obtained after vacuum freeze drying
Element；
4) purifying of flax lignan：The hurds lignan that step 3) obtains is made into 50%~80% ethanol water
The solution of a concentration of 4~8mg/mL collects stripping liquid with macroporous resin purification, is concentrated under reduced pressure, and height is obtained after vacuum freeze drying
The flax lignan of purity.
2. a kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal according to claim 1,
It is characterized in that, the linseed separation of hull from kernel described in step 1) is to realize flax according to the difference of flax seed husk benevolence toughness and grain size
Seed shell benevolence efficiently separates, and linseed smashes it through 20~30 mesh sieve.
3. a kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal according to claim 1,
It is characterized in that, the condition of the microwave radiation technology hot water extraction described in step 2) is：The mass ratio of flax seed husk and water is 1:20
~30,60~100 DEG C, 40~60min of extraction time, 600~800W of output power of extraction temperature, 600~900r/ of mixing speed
min。
4. a kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal according to claim 1,
It is characterized in that, concentration of alcohol is 40%~90% in ethyl alcohol-sodium hydroxide solution described in step 3), naoh concentration is
0.2~2mol/L.
5. a kind of method for continuously extracting flaxseed gum and flax lignan from flaxseed meal according to claim 1,
It is characterized in that, in flax lignan purification process described in step 4), big pore resin is AB-8 macroreticular resins, at room temperature
Adsorption time be 4~for 24 hours, desorption time be 2~for 24 hours, stripping liquid be 30%-70% ethanol water.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109490292A (en) * | 2018-11-23 | 2019-03-19 | 北京倍肯恒业科技发展股份有限公司 | The rapid detection method of biguanide compound in a kind of health care product |
| CN109535276A (en) * | 2018-12-28 | 2019-03-29 | 呼和浩特市蒙谷香生物科技有限公司 | The extracting method of flax glue and lignan in a kind of linseed meal |
| CN110463567A (en) * | 2019-08-12 | 2019-11-19 | 亿利资源集团有限公司 | A kind of soil cultivation agent and preparation method thereof |
| CN110663774A (en) * | 2019-11-01 | 2020-01-10 | 辽宁晟麦实业股份有限公司 | High-dietary-fiber linseed powder with good reconstitution property and preparation method thereof |
| CN111671077A (en) * | 2020-03-24 | 2020-09-18 | 宁夏君星坊食品科技有限公司 | Total nutrient meal replacement powder containing secoisolariciresinol diglucoside and preparation method thereof |
| CN113080476A (en) * | 2021-04-19 | 2021-07-09 | 浙江中科中创功能食品有限公司 | Resource-saving type comprehensive utilization and processing technology for flaxseeds |
| CN114539436A (en) * | 2022-03-21 | 2022-05-27 | 青岛德慧海洋生物科技有限公司 | Extraction process of flaxseed gum and flaxseed gum |
| CN115067417A (en) * | 2022-06-08 | 2022-09-20 | 丁兰浦 | Preparation method for comprehensive processing and utilization of linseed oil meal |
| WO2023011102A1 (en) * | 2021-08-04 | 2023-02-09 | 暨南大学 | Subcritical composite solvent extraction and separation method for multiple components in flaxseed meal |
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| CN102850414A (en) * | 2012-08-16 | 2013-01-02 | 山西省农业科学院农产品加工研究所 | Method for continuously extracting flaxseed gum and lignan from flaxseed husks |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109490292A (en) * | 2018-11-23 | 2019-03-19 | 北京倍肯恒业科技发展股份有限公司 | The rapid detection method of biguanide compound in a kind of health care product |
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| CN109535276A (en) * | 2018-12-28 | 2019-03-29 | 呼和浩特市蒙谷香生物科技有限公司 | The extracting method of flax glue and lignan in a kind of linseed meal |
| CN110463567A (en) * | 2019-08-12 | 2019-11-19 | 亿利资源集团有限公司 | A kind of soil cultivation agent and preparation method thereof |
| CN110663774A (en) * | 2019-11-01 | 2020-01-10 | 辽宁晟麦实业股份有限公司 | High-dietary-fiber linseed powder with good reconstitution property and preparation method thereof |
| CN111671077A (en) * | 2020-03-24 | 2020-09-18 | 宁夏君星坊食品科技有限公司 | Total nutrient meal replacement powder containing secoisolariciresinol diglucoside and preparation method thereof |
| CN113080476A (en) * | 2021-04-19 | 2021-07-09 | 浙江中科中创功能食品有限公司 | Resource-saving type comprehensive utilization and processing technology for flaxseeds |
| WO2023011102A1 (en) * | 2021-08-04 | 2023-02-09 | 暨南大学 | Subcritical composite solvent extraction and separation method for multiple components in flaxseed meal |
| CN114539436A (en) * | 2022-03-21 | 2022-05-27 | 青岛德慧海洋生物科技有限公司 | Extraction process of flaxseed gum and flaxseed gum |
| CN115067417A (en) * | 2022-06-08 | 2022-09-20 | 丁兰浦 | Preparation method for comprehensive processing and utilization of linseed oil meal |
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Application publication date: 20180817 |