CN101696381B - Novel process for preparing highland barley flavone extract and application thereof in health wine - Google Patents
Novel process for preparing highland barley flavone extract and application thereof in health wine Download PDFInfo
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- CN101696381B CN101696381B CN2009101175322A CN200910117532A CN101696381B CN 101696381 B CN101696381 B CN 101696381B CN 2009101175322 A CN2009101175322 A CN 2009101175322A CN 200910117532 A CN200910117532 A CN 200910117532A CN 101696381 B CN101696381 B CN 101696381B
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- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 34
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- 238000000108 ultra-filtration Methods 0.000 claims description 25
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- HGUVPEBGCAVWID-UHFFFAOYSA-N saponarin Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)C2C(C(O)C(O)C(CO)O2)O)=CC2=C1C(=O)C=C(C=1C=CC(O)=CC=1)O2 HGUVPEBGCAVWID-UHFFFAOYSA-N 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a novel process for preparing highland barley flavone extract, comprising the following steps of extracting flavonoids form highland barley seedlings by a normal hydrous alcohol solvent reflux extraction method; removing particular impurities such as dusts by a tubular centrifuge; carrying out the procedures of filtering for clarification through a ceramic membrane, interception for separation through anultrfiltration membrane, desalination for concentration through a nanofiltration membrane and the like; and finally drying by spraying or microwave to obtain the highland barley flavone extract containing 8.1-14.9 percent of total flavone . Meanwhile, the invention also discloses the application of the highland barley flavone extract prepared by the process in health wine. In the invention, purification and separation are carried out in a combined membrane separation mode, so that the invention has the advantages of good separation effect, high yield of effective substances and good stability of the product.
Description
Technical field
The present invention relates to a kind of new preparation process of highland barley flavone extract and the application in health promoting wine thereof.
Background technology
Highland barley (Hordeum vulgare L.var.nudum Hook.f.) is a kind of cereal crop of Gramineae Hordeum (Hordeumvulgare), and because of coetonium shell in it separates, seed is exposed, so claim hull-less barley, Mi Damai, highland barley again.Highland barley has abundant nutritive value and outstanding medicines and health protection effect.Put down in writing according to supplement to the Herbal: highland barley, during the therapeutic method to keep the adverse qi flowing downward is wide, strong lean power, dehumidifying sweating, antidiarrheal.Tibetan medicine's ancient books and records " brilliant pearl book on Chinese herbal medicine " more highland barley as a kind of important drugs, be used to treat multiple disease.
In recent years, the development research of highland barley mainly concentrated on the functional component beta-glucan aspect in the seed, and the activeconstituents development research of flavonoid is less relatively in the relevant highland barley seedling.Lutonarin (Lutonarin) and Saponaria officinalis xanthosine (Saponarin) are the main flavones ingredients in the highland barley seedling, and its chemical structure is following:
The chemical structure of the chemical structure Saponaria officinalis xanthosine of lutonarin
Ergonomy research shows that the antifatigue of highland barley seedling extractive of general flavone and anoxia efficacy effect are obvious.
At present, the existing extracting and preparing technique of highland barley flavone extract is that conventional aqueous ethanolic solution extracts, macroporous resin adsorption is separated and the solvent stage treatment.Shortcomings such as this technology exists that product yield is low, organic substance residues is high, separates poor reproducibility, stage treatment technology trouble and production process energy consumption height.
Summary of the invention
Technical problem to be solved by this invention provides the new preparation process of the highland barley flavone extract that a kind of good separating effect, yield are high, product stability is good.
Another technical problem to be solved by this invention provides the application art of a kind of this highland barley flavone extract in health promoting wine.
For addressing the above problem, the new preparation process of a kind of highland barley flavone extract of the present invention may further comprise the steps:
(1) the highland barley seedling after drying, the pulverizing is added aqueous ethanol solution and extract, filter, get extracting solution, ethanol to the determining alcohol in the recovery extracting solution＜below 5%, get liquid concentrator with conventional refluxing extraction method;
(2) with liquid concentrator through the dilution, centrifugal after, centrifugate;
(3) adopt the membrane sepn mode of ceramic membrane clarification, ultra-filtration membrane separation and nf membrane desalination and concentration to carry out purifies and separates successively centrifugate, obtain the nanofiltration liquid concentrator at last;
(4) with the nanofiltration liquid concentrator after drying, promptly get highland barley flavone extract.
Refluxing extraction condition in the said step (1) is: 70～100 ℃ of temperature, feed liquid weight ratio are 1: 10～1: 30, alcohol concn 10%～70%.
Ceramic membrane membrane pore size in the said step (3) is 50nm～200nm.
The organic matter molecular mass of holding back of ultra-filtration membrane is 20000～50000Dalton in the said step (3).
The organic matter molecular mass of holding back of nf membrane is 300～1000Dalton in the said step (3).
Drying in the said step (4) is spraying drying or microwave drying.
A kind of application of highland barley flavone extract in health promoting wine of adopting the new preparation process extraction of aforesaid highland barley flavone extract; It is characterized in that: highland barley flavone extract is pulverized; Crossing behind 200～400 mesh sieves and joining alcoholic strength in 1: 40～1: 80 by the feed liquid weight ratio is in 30 °～60 ° the liquor; Behind the ceramic micro filter membrane filtration of ultrasonic dissolution, 50nm～200nm, canned getting final product.
The present invention compared with prior art has the following advantages:
1, the present invention on the basis of conventional process for extracting, the highland barley flavone extract that utilizes membrane separation technique to make is brown ceramic powder; Special aroma is arranged; Content of total flavone is 8.1%～14.9%; Wherein effective constituent lutonarin content is 5.1%～9.2%, and Saponaria officinalis xanthosine content is 3.0%～5.7%.
When the highland barley flavone extract that 2, adopts the inventive method to make was used to prepare health promoting wine, flavones content can reach 0.15%～0.3% in this health promoting wine, has antifatigue and anoxia tolerance function.
3, because the present invention adopts ceramic membrane clarification, ultra-filtration membrane to separate and the membrane sepn array mode of nf membrane desalination and concentration is carried out purifies and separates, therefore, good separating effect, the working substance yield is high, and product stability is good.
4, because the present invention has avoided the use regenerating resin, thereby reduce a large amount of acid and alkali consumptions, do not had steam consumption at concentration process simultaneously; And the wet water after concentrating is got back in the production line as process water; Therefore, the present invention is energy-conserving and environment-protective not only, and have practiced thrift spending.
5, technological operation of the present invention is easy, with short production cycle.
Embodiment
Embodiment 1 gets exsiccant highland barley seedling raw material 10Kg; Be cut into the segment of 1～2cm or be ground into meal; Use raw material weight 10 times of amounts, concentration are 10% ethanolic soln; Extract unit at 70 ℃ of TQ-300 small-size multifunctions of producing with Wuhan sunshine roc pharmaceutical machine equipment ltd down of temperature and extract 1～4 time, each 0.5～4 hour, the screen filtration post precipitation got extracting solution through multi-functional extraction unit extractor bottom; The SHB-C type vacuum pump that adopts Zhengzhou Greatwall Scientific Industrial & Trading Co., Ltd. to produce the then decompression of bleeding, reclaim ethanol to determining alcohol＜5% in the extracting solution after, must liquid concentrator 30Kg.
After liquid concentrator added 2 times of amounts and be 60Kg pure water dilution, the GQ75 type tubular-bowl centrifuge of producing with sky, PVG this centrifugal machine ltd must centrifugate 90Kg with the centrifugal suspended particle shape impurity such as dust of removing of 20000 rev/mins speed.
Centrifugate adopts the ceramic micro filter film device of the SJM-FHM-10 type 200nm of the outstanding film engineering of Hefei generation Ltd production to filter, and gets clear liquor 100Kg (process of the test is added water 20Kg, surplus ceramic membrane filter debris 10Kg).Clear liquor uses SJM-DGN-060 type that the outstanding film engineering of Hefei generation Ltd produces, hold back organic matter molecular mass carries out ultrafiltration as the multifunctional membrane equipment of 50000Dalton and holds back separations (it is the 300Kg pure water that process of the test is added 3 times of amounts), ultra-filtration and separation liquid 370Kg (remaining ultra-filtration membrane debris 28Kg).Ultra-filtration and separation liquid uses SJM-DGN-060 type that the outstanding film engineering of Hefei generation Ltd produces again, hold back organic matter molecular mass carries out desalting and dewatering as the nf membrane of 300Dalton and concentrates, nanofiltration liquid concentrator 36Kg.
After the R2002K type 20L Rotary Evaporators that the nanofiltration liquid concentrator is produced with Wuxi Xing Hai king's biochemical equipment ltd further concentrates; The KMZ-2006 type microwave vacuum dryer that adopts Wenzhou City health board pharmaceutical machine ltd to produce carries out microwave drying; Get brown highland barley flavone extract 1.36Kg, yield 13.6%.
The Agilent 1200 type high-efficient liquid phase chromatogram HPLCs that this extract is produced through U.S. Agilent company are measured and are contained lutonarin 5.1% and Saponaria officinalis xanthosine 3.0%, add up to flavones content 8.1%.
Getting above highland barley flavone extract 0.5Kg pulverizes; After crossing 200～400 mesh sieves; Joining alcoholic strength in 1: 40 ratio is in 40 ° the 20Kg highland barley liquor in bulk, adopt KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min that Kunshan Ultrasonic Instruments Co., Ltd. produces after, the ceramic micro filter film device of crossing 50nm filters clarification; Canned, promptly get highland barley health care wine.
Embodiment 2 gets exsiccant highland barley seedling raw material 10Kg; Be cut into the segment of 1～2cm or be ground into meal; Use raw material weight 20 times of amounts, concentration are 60% ethanolic soln; Under 80 ℃ of temperature, extract unit with small-size multifunction and extract 1～4 time, each 0.5～4 hour, the screen filtration post precipitation got extracting solution through multi-functional extraction unit extractor bottom; Adopt the decompression of bleeding of SHB-C type vacuum pump then, reclaim ethanol to determining alcohol＜5% in the extracting solution after, liquid concentrator 25Kg.
After liquid concentrator added 2 times of amounts and be 50Kg pure water dilution, with GQ75 type tubular-bowl centrifuge with the centrifugal suspended particle shape impurity such as dust of removing of 20000 rev/mins speed, must centrifugate 75Kg.
Centrifugate adopts the ceramic micro filter film device of SJM-FHM-10 type 100nm to filter, and gets clear liquor 100Kg (process of the test is added water 40Kg, surplus ceramic membrane filter debris 14Kg).Clear liquor uses the SJM-DGN-060 type, hold back organic matter molecular mass carries out ultrafiltration as the multifunctional membrane equipment of 30000Dalton and holds back separation (it is the 300Kg pure water that process of the test is added 3 times of amounts), ultra-filtration and separation liquid 360Kg (surplus ultra-filtration membrane debris 35Kg).Ultra-filtration and separation liquid uses again to be held back organic matter molecular mass and carries out desalting and dewatering as the nf membrane of 500Dalton and concentrate, nanofiltration liquid concentrator 40Kg.
After the nanofiltration liquid concentrator further concentrates with R2002K type 20L Rotary Evaporators; The Mini Spray Dryer B-29 type spray-dryer that adopts Switzerland BUCHI to produce carries out spraying drying; To set tower wind-warm syndrome degree be 160 ℃, go out the tower wind-warm syndrome is that 80 ℃, airshed are 20m/h; Get brown highland barley flavone extract 0.96Kg, yield 9.6%.
This extract is measured through HPLC and is contained lutonarin 7.3% and Saponaria officinalis xanthosine 4.6%, adds up to flavones content 11.9%.
Getting above highland barley flavone extract 0.5Kg pulverizes; After crossing 200～400 mesh sieves; Joining alcoholic strength in 1: 50 ratio is in 30 ° the 25Kg highland barley liquor in bulk, adopt KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min after, the ceramic micro filter film device of crossing 100nm filters clarification; Canned, promptly get highland barley health care wine.
Embodiment 3 gets exsiccant highland barley seedling raw material 10Kg; Be cut into the segment of 1～2cm or be ground into meal; Use raw material weight 25 times of amounts, concentration are 40% ethanolic soln; Extract unit with the TQ-300 small-size multifunction down for 90 ℃ in temperature and extract 1～4 time, each 0.5～4 hour, the screen filtration post precipitation got extracting solution through multi-functional extraction unit extractor bottom; Adopt the decompression of bleeding of SHB-C type vacuum pump then, reclaim ethanol to determining alcohol＜5% in the extracting solution after, liquid concentrator 28Kg.
After liquid concentrator added 2 times of amounts and be 56Kg pure water dilution, with GQ75 type tubular-bowl centrifuge with the centrifugal suspended particle shape impurity such as dust of removing of 20000 rev/mins speed, must centrifugate 83Kg.
Centrifugate adopts the ceramic micro filter film device of SJM-FHM-10 type 50nm to filter, and gets clear liquor 100Kg (process of the test is added water 30Kg, surplus ceramic membrane filter debris 12Kg).Clear liquor uses the SJM-DGN-060 type, hold back organic matter molecular mass carries out ultrafiltration as the multifunctional membrane equipment of 30000Dalton and holds back separation (it is the 300Kg pure water that process of the test is added 3 times of amounts), ultra-filtration and separation liquid 360Kg (surplus ultra-filtration membrane debris 35Kg).Ultra-filtration and separation liquid uses again to be held back organic matter molecular mass and carries out desalting and dewatering as the nf membrane of 500Dalton and concentrate, nanofiltration liquid concentrator 42Kg.
The nanofiltration liquid concentrator adopts KMZ-2006 type microwave vacuum dryer to carry out microwave drying after further concentrating with R2002K type 20L Rotary Evaporators, gets brown highland barley flavone extract 0.98Kg, yield 9.8%.
This extract is measured through HPLC and is contained lutonarin 7.1% and Saponaria officinalis xanthosine 4.5%, adds up to flavones content 11.6%.
Getting above highland barley flavone extract 0.5Kg pulverizes; After crossing 200～400 mesh sieves; Joining alcoholic strength in 1: 50 ratio is in 45 ° the 25Kg highland barley liquor in bulk, adopt KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min after, the ceramic micro filter film device of crossing 150nm filters clarification; Canned, promptly get highland barley health care wine.
Embodiment 4 gets exsiccant highland barley seedling raw material 10Kg; Be cut into the segment of 1～2cm or be ground into meal; Use raw material weight 15 times of amounts, concentration are 30% ethanolic soln; Extract unit with the TQ-300 small-size multifunction down for 80 ℃ in temperature and extract 1～4 time, each 0.5～4 hour, the screen filtration post precipitation got extracting solution through multi-functional extraction unit extractor bottom; Adopt the decompression of bleeding of SHB-C type vacuum pump then, reclaim ethanol to determining alcohol＜5% in the extracting solution after, liquid concentrator 30Kg.
After liquid concentrator added 2 times of amounts and be 60Kg pure water dilution, with GQ75 type tubular-bowl centrifuge with the centrifugal suspended particle shape impurity such as dust of removing of 20000 rev/mins speed, must centrifugate 89Kg.
Centrifugate adopts the ceramic micro filter film device of SJM-FHM-10 type 100nm to filter, and gets clear liquor 102Kg (process of the test is added water 25Kg, surplus ceramic membrane filter debris 11Kg).Clear liquor uses the SJM-DGN-060 type, hold back organic matter molecular mass carries out ultrafiltration as the multifunctional membrane equipment of 20000Dalton and holds back separation (it is the 306Kg pure water that process of the test is added 3 times of amounts), ultra-filtration and separation liquid 370Kg (surplus ultra-filtration membrane debris 30Kg).Ultra-filtration and separation liquid uses again to be held back organic matter molecular mass and carries out desalting and dewatering as the nf membrane of 800Dalton and concentrate, nanofiltration liquid concentrator 38Kg.
The nanofiltration liquid concentrator adopts KMZ-2006 type microwave vacuum dryer to carry out microwave drying after further concentrating with R2002K type 20L Rotary Evaporators, gets brown highland barley flavone extract 0.65Kg, yield 6.5%.
This extract is measured through HPLC and is contained lutonarin 9.2% and Saponaria officinalis xanthosine 5.7%, adds up to flavones content 14.9%.
Getting above highland barley flavone extract 0.3Kg pulverizes; After crossing 200～400 mesh sieves; Joining alcoholic strength in 1: 80 ratio is in 50 ° the 24Kg highland barley liquor in bulk, adopt KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min after, the ceramic micro filter film device of crossing 200nm filters clarification; Canned, promptly get highland barley health care wine.
Embodiment 5 gets exsiccant highland barley seedling raw material 10Kg; Be cut into the segment of 1～2cm or be ground into meal; Use raw material weight 30 times of amounts, concentration are 70% ethanolic soln; Extract unit with the TQ-300 small-size multifunction down for 100 ℃ in temperature and extract 1～4 time, each 0.5～4 hour, the screen filtration post precipitation got extracting solution through multi-functional extraction unit extractor bottom; Adopt the decompression of bleeding of SHB-C type vacuum pump then, reclaim ethanol to determining alcohol＜5% in the extracting solution after, liquid concentrator 25Kg.
After liquid concentrator added 3 times of amounts and be 75Kg pure water dilution, with GQ75 type tubular-bowl centrifuge with the centrifugal suspended particle shape impurity such as dust of removing of 20000 rev/mins speed, must centrifugate 98Kg.
Centrifugate adopts the ceramic micro filter film device of SJM-FHM-10 type 200nm to filter, and gets clear liquor 102Kg (process of the test is added water 15Kg, surplus ceramic membrane filter debris 11Kg).Clear liquor uses the SJM-DGN-060 type, hold back organic matter molecular mass carries out ultrafiltration as the multifunctional membrane equipment of 20000Dalton and holds back separation (it is the 306Kg pure water that process of the test is added 3 times of amounts), ultra-filtration and separation liquid 380Kg (surplus ultra-filtration membrane debris 26Kg).Ultra-filtration and separation liquid uses again to be held back organic matter molecular mass and carries out desalting and dewatering as the nf membrane of 1000Dalton and concentrate, nanofiltration liquid concentrator 35Kg.
After the nanofiltration liquid concentrator further concentrates with R2002K type 20L Rotary Evaporators; Adopt Mini SprayDryer B-29 type spray-dryer to carry out spraying drying; To set tower wind-warm syndrome degree be 160 ℃, go out the tower wind-warm syndrome is that 80 ℃, airshed are 20m/h; Get brown highland barley flavone extract 0.96Kg, yield 9.6%.
This extract is measured through HPLC and is contained lutonarin 8.3% and Saponaria officinalis xanthosine 5.3%, adds up to flavones content 13.6%.
Getting above highland barley flavone extract 0.5Kg pulverizes; After crossing 200～400 mesh sieves; Joining alcoholic strength in 1: 40 ratio is in 60 ° the 20Kg highland barley liquor in bulk, adopt KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min after, the ceramic micro filter film device of crossing 150nm filters clarification; Canned, promptly get highland barley health care wine.
Claims (2)
1. the preparation technology of a highland barley flavone extract may further comprise the steps:
(1) the highland barley seedling after drying, the pulverizing is added aqueous ethanol solution and extract, filter, get extracting solution, ethanol to the determining alcohol in the recovery extracting solution＜below 5%, get liquid concentrator with conventional refluxing extraction method; The refluxing extraction condition is: 70～100 ℃ of temperature, feed liquid weight ratio are 1: 10～1: 30, alcohol concn 10%～70%;
(2) with liquid concentrator through the dilution, centrifugal after, centrifugate;
(3) adopt the membrane sepn mode of ceramic membrane clarification, ultra-filtration membrane separation and nf membrane desalination and concentration to carry out purifies and separates successively centrifugate, obtain the nanofiltration liquid concentrator at last; Said ceramic membrane membrane pore size is 50nm～200nm; The organic matter molecular mass of holding back of ultra-filtration membrane is 20000～50000Dalton; The organic matter molecular mass of holding back of nf membrane is 300～1000Dalton;
(4) the nanofiltration liquid concentrator after the spray-dried or microwave drying, is promptly got highland barley flavone extract.
2. the application of highland barley flavone extract in health promoting wine of adopting preparation technology's extraction of highland barley flavone extract as claimed in claim 1; It is characterized in that: highland barley flavone extract is pulverized; Crossing behind 200～400 mesh sieves and joining alcoholic strength in 1: 40～1: 80 by the feed liquid weight ratio is in 30 °～60 ° the liquor; Behind the ceramic micro filter membrane filtration of ultrasonic dissolution, 50nm～200nm, canned getting final product.
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| CN2009101175322A CN101696381B (en) | 2009-10-23 | 2009-10-23 | Novel process for preparing highland barley flavone extract and application thereof in health wine |
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| CN2009101175322A CN101696381B (en) | 2009-10-23 | 2009-10-23 | Novel process for preparing highland barley flavone extract and application thereof in health wine |
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| CN101696381A CN101696381A (en) | 2010-04-21 |
| CN101696381B true CN101696381B (en) | 2012-06-27 |
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| CN102492007A (en) * | 2011-12-08 | 2012-06-13 | 中国农业大学 | Method for extracting flavones compounds and total phenol from hot pepper residue |
| CN104745423A (en) * | 2015-03-30 | 2015-07-01 | 李滋星 | Liquor-based drink and preparation method thereof |
| CN107007526A (en) * | 2017-05-09 | 2017-08-04 | 上海绰然生物科技有限公司 | A kind of Preparation method and use of highland barley bran extract |
| CN115251383B (en) * | 2022-07-27 | 2024-05-10 | 劲牌持正堂药业有限公司 | Method for continuously preparing two highland barley flavone extracts with different purposes from highland barley and application |
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