CN101696381A - 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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- CN101696381A CN101696381A CN200910117532A CN200910117532A CN101696381A CN 101696381 A CN101696381 A CN 101696381A CN 200910117532 A CN200910117532 A CN 200910117532A CN 200910117532 A CN200910117532 A CN 200910117532A CN 101696381 A CN101696381 A CN 101696381A
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- barley flavone
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- 235000007340 Hordeum vulgare Nutrition 0.000 title claims abstract description 66
- 239000000284 extract Substances 0.000 title claims abstract description 49
- 229930003944 flavone Natural products 0.000 title claims abstract description 46
- 235000011949 flavones Nutrition 0.000 title claims abstract description 46
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 39
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 39
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 240000005979 Hordeum vulgare Species 0.000 title description 3
- 241000209219 Hordeum Species 0.000 claims abstract description 64
- 239000012528 membrane Substances 0.000 claims abstract description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001728 nano-filtration Methods 0.000 claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 24
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 238000005352 clarification Methods 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 238000010612 desalination reaction Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 45
- 238000000108 ultra-filtration Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 14
- 239000005416 organic matter Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 12
- 230000001476 alcoholic effect Effects 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000005304 joining Methods 0.000 claims description 7
- 230000001737 promoting effect Effects 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 150000002215 flavonoids Chemical group 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000002994 raw material Substances 0.000 description 10
- OQKYVRDRDIXQMK-KETMJRJWSA-N 2-(3,4-dihydroxyphenyl)-5-hydroxy-6-[(2s,3r,4r,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]-7-[(2s,3r,4r,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxychromen-4-one Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC(C(=C1O)[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)=CC2=C1C(=O)C=C(C=1C=C(O)C(O)=CC=1)O2 OQKYVRDRDIXQMK-KETMJRJWSA-N 0.000 description 9
- NXXWLQYGFANBST-UHFFFAOYSA-N Isoorientin-7-O-glucosid Natural products OCC1OC(Oc2cc3OC(=CC(=O)c3cc2C4OC(CO)C(O)C(O)C4O)c5ccc(O)c(O)c5)C(O)C(O)C1O NXXWLQYGFANBST-UHFFFAOYSA-N 0.000 description 9
- SLJVIWCEWPUMET-UHFFFAOYSA-N lutonarin Natural products OCC1OC(Oc2cc3OC(=CC(=O)c3c(O)c2OC4OC(CO)C(O)C(O)C4O)c5ccc(O)c(O)c5)C(O)C(O)C1O SLJVIWCEWPUMET-UHFFFAOYSA-N 0.000 description 9
- UBORTCNDUKBEOP-UHFFFAOYSA-N L-xanthosine Natural products OC1C(O)C(CO)OC1N1C(NC(=O)NC2=O)=C2N=C1 UBORTCNDUKBEOP-UHFFFAOYSA-N 0.000 description 8
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- UBORTCNDUKBEOP-HAVMAKPUSA-N Xanthosine Natural products O[C@@H]1[C@H](O)[C@H](CO)O[C@H]1N1C(NC(=O)NC2=O)=C2N=C1 UBORTCNDUKBEOP-HAVMAKPUSA-N 0.000 description 8
- UBORTCNDUKBEOP-UUOKFMHZSA-N xanthosine Chemical compound O[C@@H]1[C@H](O)[C@@H](CO)O[C@H]1N1C(NC(=O)NC2=O)=C2N=C1 UBORTCNDUKBEOP-UUOKFMHZSA-N 0.000 description 8
- 150000002213 flavones Chemical class 0.000 description 7
- 230000000740 bleeding effect Effects 0.000 description 5
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- 238000011033 desalting Methods 0.000 description 5
- 239000000428 dust Substances 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 235000012054 meals Nutrition 0.000 description 5
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- 239000012141 concentrate Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
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- 206010021143 Hypoxia Diseases 0.000 description 2
- 230000002929 anti-fatigue Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- FYGDTMLNYKFZSV-URKRLVJHSA-N (2s,3r,4s,5s,6r)-2-[(2r,4r,5r,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5r,6s)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1[C@@H](CO)O[C@@H](OC2[C@H](O[C@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-URKRLVJHSA-N 0.000 description 1
- HGUVPEBGCAVWID-KETMJRJWSA-N 7-O-(beta-D-glucosyl)isovitexin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC(C(=C1O)[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)=CC2=C1C(=O)C=C(C=1C=CC(O)=CC=1)O2 HGUVPEBGCAVWID-KETMJRJWSA-N 0.000 description 1
- 206010002660 Anoxia Diseases 0.000 description 1
- 241000976983 Anoxia Species 0.000 description 1
- 229920002498 Beta-glucan Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- 230000001142 anti-diarrhea Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
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- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000007954 hypoxia Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 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
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
Landscapes
- 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 for the treatment of 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 as follows:
The chemical structure of the chemical structure Saponaria officinalis xanthosine of lutonarin
Ergonomy studies show that the antifatigue of highland barley seedling extractive of general flavone and hypoxia tolerance 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 a kind of good separating effect, yield height, highland barley flavone extract that 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) highland barley seedling dry, after pulverizing is added aqueous ethanol solution and extracts, filters with conventional refluxing extraction method, extracting solution, reclaim ethanol in the extracting solution to determining alcohol＜below 5%, get concentrated solution;
(2) with concentrated solution through the dilution, centrifugal after, centrifugate;
(3) centrifugate is adopted successively the membrane sepn mode of ceramic membrane clarification, ultra-filtration membrane separation and nanofiltration membrane desalination and concentration carry out purifies and separates, obtain the nanofiltration concentrated solution at last;
(4) after drying, promptly get highland barley flavone extract with the nanofiltration concentrated solution.
Refluxing extraction condition in the described 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 described step (3) is 50nm～200nm.
The organic matter molecular mass of holding back of ultra-filtration membrane is 20000～50000Dalton in the described step (3).
The organic matter molecular mass of holding back of nanofiltration membrane is 300～1000Dalton in the described step (3).
Drying in the described 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 extracting method, 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 2, the highland barley flavone extract that 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 nanofiltration membrane desalination and concentration is carried out purifies and separates, therefore, good separating effect, working substance yield height, 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 infiltration 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 saved 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, it with raw material weight 10 times of amounts, concentration 10% ethanolic soln, extracting unit at 70 ℃ of TQ-300 small-size multifunctions of producing with Wuhan sunshine roc pharmaceutical machine equipment company limited down of temperature extracts 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 is reclaimed ethanol in the extracting solution to determining alcohol＜5%, must concentrated solution 30Kg.
After concentrated solution 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 company limited 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 limited liability company production to filter, and gets clear liquor 100Kg (process of the test is added water 20Kg, surplus ceramic membrane filter debris 10Kg).The SJM-DGN-060 type that clear liquor is produced with the outstanding film engineering of Hefei generation limited liability company, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 50000Dalton carries out ultrafiltration 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).The SJM-DGN-060 type that ultra-filtration and separation liquid is produced with the outstanding film engineering of Hefei generation limited liability company again, to hold back organic matter molecular mass be that the nanofiltration membrane of 300Dalton is carried out desalting and dewatering and concentrated, nanofiltration concentrated solution 36Kg.
After the R2002K type 20L Rotary Evaporators that the nanofiltration concentrated solution is produced with Wuxi Xing Hai king's biochemical equipment company limited further concentrates, the KMZ-2006 type microwave vacuum dryer that adopts Wenzhou City health board pharmaceutical machine company limited 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, after adopting the KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min of Kunshan Ultrasonic Instruments Co., Ltd.'s production, 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, it with raw material weight 20 times of amounts, concentration 60% ethanolic soln, extracting unit with small-size multifunction under 80 ℃ of temperature extracts 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 in the extracting solution to determining alcohol＜5%, concentrated solution 25Kg.
After concentrated solution 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 with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 30000Dalton carries out ultrafiltration 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 is that the nanofiltration membrane of 500Dalton is carried out desalting and dewatering and concentrated with holding back organic matter molecular mass again, nanofiltration concentrated solution 40Kg.
After the nanofiltration concentrated solution 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, after adopting KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min, 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, it with raw material weight 25 times of amounts, concentration 40% ethanolic soln, extracting unit with the TQ-300 small-size multifunction down for 90 ℃ in temperature extracts 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 in the extracting solution to determining alcohol＜5%, concentrated solution 28Kg.
After concentrated solution 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 with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 30000Dalton carries out ultrafiltration 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 is that the nanofiltration membrane of 500Dalton is carried out desalting and dewatering and concentrated with holding back organic matter molecular mass again, nanofiltration concentrated solution 42Kg.
The nanofiltration concentrated solution 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, after adopting KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min, 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, it with raw material weight 15 times of amounts, concentration 30% ethanolic soln, extracting unit with the TQ-300 small-size multifunction down for 80 ℃ in temperature extracts 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 in the extracting solution to determining alcohol＜5%, concentrated solution 30Kg.
After concentrated solution 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 with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 20000Dalton carries out ultrafiltration 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 is that the nanofiltration membrane of 800Dalton is carried out desalting and dewatering and concentrated with holding back organic matter molecular mass again, nanofiltration concentrated solution 38Kg.
The nanofiltration concentrated solution 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, after adopting KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min, 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, it with raw material weight 30 times of amounts, concentration 70% ethanolic soln, extracting unit with the TQ-300 small-size multifunction down for 100 ℃ in temperature extracts 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 in the extracting solution to determining alcohol＜5%, concentrated solution 25Kg.
After concentrated solution 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 with the SJM-DGN-060 type, to hold back organic matter molecular mass be that the multifunctional membrane equipment of 20000Dalton carries out ultrafiltration 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 is that the nanofiltration membrane of 1000Dalton is carried out desalting and dewatering and concentrated with holding back organic matter molecular mass again, nanofiltration concentrated solution 35Kg.
After the nanofiltration concentrated solution 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, after adopting KQ500E ultrasonic cleaner ultrasonic dissolution 10～30min, the ceramic micro filter film device of crossing 150nm filters clarification, canned, promptly get highland barley health care wine.
Claims (7)
1. the new preparation process of a highland barley flavone extract may further comprise the steps:
(1) highland barley seedling dry, after pulverizing is added aqueous ethanol solution and extracts, filters with conventional refluxing extraction method, extracting solution, reclaim ethanol in the extracting solution to determining alcohol＜below 5%, get concentrated solution;
(2) with concentrated solution through the dilution, centrifugal after, centrifugate;
(3) centrifugate is adopted successively the membrane sepn mode of ceramic membrane clarification, ultra-filtration membrane separation and nanofiltration membrane desalination and concentration carry out purifies and separates, obtain the nanofiltration concentrated solution at last;
(4) after drying, promptly get highland barley flavone extract with the nanofiltration concentrated solution.
2. the new preparation process of highland barley flavone extract as claimed in claim 1, it is characterized in that: the refluxing extraction condition in the described step (1) is: 70～100 ℃ of temperature, feed liquid weight ratio are 1: 10～1: 30, alcohol concn 10%～70%.
3. the new preparation process of highland barley flavone extract as claimed in claim 1, it is characterized in that: the ceramic membrane membrane pore size in the described step (3) is 50nm～200nm.
4. the new preparation process of highland barley flavone extract as claimed in claim 1 is characterized in that: the organic matter molecular mass of holding back of ultra-filtration membrane is 20000～50000Dalton in the described step (3).
5. the new preparation process of highland barley flavone extract as claimed in claim 1 is characterized in that: the organic matter molecular mass of holding back of nanofiltration membrane is 300～1000Dalton in the described step (3).
6. the new preparation process of highland barley flavone extract as claimed in claim 1, it is characterized in that: the drying in the described step (4) is spraying drying or microwave drying.
7. the application of highland barley flavone extract in health promoting wine of adopting the new preparation process 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115251383A (en) * | 2022-07-27 | 2022-11-01 | 劲牌持正堂药业有限公司 | Method for continuously preparing highland barley flavone extracts with two different purposes from highland barley and application |
-
2009
- 2009-10-23 CN CN2009101175322A patent/CN101696381B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115251383A (en) * | 2022-07-27 | 2022-11-01 | 劲牌持正堂药业有限公司 | Method for continuously preparing highland barley flavone extracts with two different purposes from highland barley and application |
| 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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| Publication number | Publication date |
|---|---|
| CN101696381B (en) | 2012-06-27 |
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