CN101361932B - Preparation method of high-assay highland barley flavones and use thereof in preparing healthcare products - Google Patents
Preparation method of high-assay highland barley flavones and use thereof in preparing healthcare products Download PDFInfo
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Abstract
The invention relates to a preparation method of a high content extract of naked oat fruit flavone. In the method, a reflux extraction method of a water-containing alcohol-soluble medium is adopted to extract flavonoid compound from naked oat fruit seedlings, and then the macroporous resin absorption method is adopted to enrich the flavonoid compound in the extracting liquid, and the extract is eluted by ethanol solution, condensed and dried, and finally the extract of naked oat fruit flavone containing 20 to 45 percent of total flavone is prepared. The extract has the functions of fatigue resistance and anoxia resistance, and can be used for preparing healthcare products with fatigue resistance and anoxia resistance.
Description
Technical field
The present invention relates to the preparation method of highland barley flavone extract, relate in particular to a kind of preparation method of high-assay highland barley flavones and the application in health product thereof.
Background technology
Live in the high altitude localities or to highland tour's people, the distinct issues the most that run into be exactly be easy to generate fatigue and because of high originality anoxia brought uncomfortable, because under very abominable environment of low oxygen plateau condition, bigger change takes place in the normal physiological metabolism of human body, therefore body immunity descends, a series of body anoxia symptoms such as headache, dizzy, weak, insomnia occur, had a strong impact on people's work efficiency and healthy.
Semen avenae nudae (Hordeum vulgare L.var.nudum Hook.f.) is a kind of cereal crop of grass family Hordeum (Hordeumvulgare), and because of coetonium shell in it separates, seed is exposed, so claim hull-less barley, Mi Damai, Semen avenae nudae again.Semen avenae nudae has long cultivation history in the Qinghai-Tibet Platean, apart from modern existing 3500, mainly be distributed in the Qinghai-Tibet extremely frigid zones of 4200～4500 meters of ground height above sea level such as Tibet, Qinghai, Ganzi, Sichuan Province and Aba Tibetan Autonomous Prefecture, Tibetan Autonomous Prefecture of Gannan, Gansu Province and Yunnan, Guizhou, being the primary raw material of Zanba first of four treasured of Tibet, also is the symbol of Qinghai-Tibet agricultural Culture simultaneously.
Semen avenae nudae has abundant nutritive value and outstanding medicines and health protection effect.Put down in writing according to supplement to the Herbal: Semen avenae nudae, therapeutic method to keep the adverse QI flowing downwards alleviating distention in middle-JIAO, strong lean power, dehumidifying diaphoresis, antidiarrheal.Tibetan medicine's ancient books and records " brilliant pearl book on Chinese herbal medicine " more Semen avenae nudae as a kind of important drugs, be used for the treatment of multiple disease.
In recent years, the developmental research of Semen avenae nudae mainly concentrated on the functional component beta glucan aspect in the seed, and the active component developmental research of flavonoid is less relatively in the relevant Semen avenae nudae seedling.According to statistics, the research paper of delivering both at home and abroad about highland barley flavone class material mainly concentrates on the pharmacodynamic studies such as mensuration, qualitative and quantitative analysis and removing free radical of its chemical constitution, and result of study shows, the Flavonoid substances (main component is lutonarin Lutonarin and ZAOCAO xanthosine Saponarin) that contains high activity, structure uniqueness in the Semen avenae nudae seedling, the resisting fatigue of extractive of general flavone and anoxia enduring efficacy effect are obvious, but relevant its production technology, high-load flavone health promoting product and preparation process thereof there is no report.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of high-assay highland barley flavones of high-load flavone.
Another technical problem to be solved by this invention provides the application of a kind of high-assay highland barley flavones in health product.
For addressing the above problem, a kind of high-assay highland barley flavones of the present invention is characterized in that: content of total flavone is 20%～45% in the described extract; Effective ingredient lutonarin content is 12%～25%, and ZAOCAO xanthosine content is 8%～20%.
The chemical constitution of described lutonarin is as follows:
The chemical structural formula of described ZAOCAO xanthosine is as follows:
A kind of preparation method of aforesaid high-assay highland barley flavones may further comprise the steps:
(1) Semen avenae nudae seedling dry, after pulverizing is added aquiferous ethanol solution with conventional reflux, extract, method extract extracting solution, reclaim ethanol in the extracting solution to determining alcohol＜below 10%, filter, get filtrate;
(2) adsorption column of filtrate flow through being filled with adsorbing material adsorbs;
(3) extremely colourless with the water wash adsorption column;
(4) with the alcoholic solution eluting of concentration 20%～60%, collect eluent;
(5) concentrate the recovery eluent, get thick paste;
(6) with the Ethanol Treatment of concentration 80%～95%, separate out precipitate, be drying to obtain extract.
Reflux, extract, condition in the described step (1) is: 70～100 ℃ of temperature, feed liquid weight ratio are 1:40～1:80, concentration of alcohol 20%～50%.
Adsorbing material in the described step (2) is a macroporous adsorbent resin.
Eluent concentration of alcohol in the described step (4) is 20%～60%.
The application of a kind of aforesaid high-assay highland barley flavones in health product is characterized in that: highland barley flavone extract is pulverized, added conventional pharmaceutic adjuvant behind 200～400 mesh sieves excessively, mix, be processed into oral formulations.
Described oral formulations is tablet, hard capsule, soft capsule, granule or oral liquid.
The present invention compared with prior art has the following advantages:
1, adopt the character of the highland barley flavone extract that the inventive method makes to be yellow powder, peat-reek is arranged, the total flavones amount reaches 20%～45%, and wherein the effective ingredient lutonarin reaches 12%～25%, and the ZAOCAO xanthosine reaches 8%～20%.
2, through being carried out Ergonomy, the made extract of the present invention studies show that this extract has significant resisting fatigue, oxygen lack resistant function.
A. highland barley flavone extract animal resisting fatigue pole-jump test:
Choose 50 of Kunming mouses, body weight 18 ± 2g is divided into blank group and administration group.High, medium and low three the dosage groups of administration component, positive controls is the VE capsule, the blank group gives the distilled water of equal volume, once a day, continuous 7 days, half an hour after the last administration, carries out the pole-climbing experiment.The length of pole-climbing experiment can be reacted the degree of fatigue when animal is quiet to exert oneself.The results are shown in Table 1:
The antifatigue effect of table 1 highland barley flavone extract (animal pole-jump test)
| Group | Dosage | Number of animals | The pole-climbing time (second) |
| High dose | 3.0g/kg | 8 | 467.42±215.84 * |
| Middle dosage | 2.5g/kg | 7 | 220.66±71.37 * |
| Low dosage | 1.5g/kg | 8 | 183.85±47.55 |
| VE | 2.0g/kg | 8 | 384.16±183.57 * |
| Blank group | 15ml/kg | 8 | 103.28±117.49 |
Compare with blank::
*P＜0.05
Drawn by table 1, there were significant differences with blank group for administration height, middle dosage group and positive group, and high, medium and low dosage extract group all has significant antifatigue effect.
B. highland barley flavone extract animal resisting fatigue swimming test:
Choose 50 of Kunming mouses, body weight 18 ± 2g is divided into blank group and administration group.Administration component 1.5g/kg, 2.5g/kg, 3.0g/kg, positive controls is the VE capsule, the blank group gives the distilled water of equal volume, once a day, continuous 7 days, half an hour after the last administration, the load screw of 5% body weight of Mus root of the tail portion carried out the swimming with a load attached to the body experiment.The results are shown in Table 2:
The antifatigue effect of table 2 highland barley flavone extract (animal swimming with a load attached to the body test)
| Group | Dosage | Number of animals | Swimming time (branch) |
| High dose | 3.0g/kg | 9 | 336.7±26.5 *** |
| Middle dosage | 2.5g/kg | 10 | 309.6±31.8 *** |
| Low dosage | 1.5g/kg | 8 | 237.7±59.7 * |
| VE | 2.0g/kg | 10 | 229.0±45.0 * |
| Blank group | 15ml/kg | 10 | 183.3±33.5 |
Compare with blank:
*P＜0.05;
*P＜0.01;
* *P＜0.005
Drawn by table 2, there were significant differences with blank group for high, medium and low dosage group of administration and positive group; High, medium and low dosage extract group all has significant antifatigue effect.
C. highland barley flavone extract animal anti-hypoxia test:
Choose 50 of Kunming mouses, body weight 18 ± 2g is divided into blank group and administration group.Administration component 1.5g/kg, 2.5g/kg, 3g/kg, positive controls is a Rhodiola rosea capsules, and dosage is 2g/kg, and the blank group gives the distilled water of equal volume, once a day, continuous 7 days, half an hour after the last administration, carries out the anoxia enduring experiment.The results are shown in Table 3:
The oxygen lack resistant function of table 3 highland barley flavone extract
| Group | Dosage | Number of animals | Hypoxia endurance time (branch) |
| High dose | 3.0g/kg | 10 | 21.1±7.7 * |
| Middle dosage | 2.5g/kg | 10 | 19.1±5.7 * |
| Low dosage | 1.5g/kg | 10 | 15.6±2.7 |
| Rhodiola rosea capsules | 3.0g/kg | 10 | 18.9±4.8 |
| Blank group | 15ml/kg | 10 | 18.0±4.0 |
Compare with blank:
*P＜0.05;
*P＜0.01
Drawn by table 3, there were significant differences with blank group for administration height, middle dosage group, and high, middle dosage extract group all has oxygen lack resistant function.
3, in the highland barley flavone extract that the inventive method makes, add conventional pharmaceutic adjuvant, as filler, binding agent, disintegrating agent, lubricant and coating material thereof and the plant oil, the fats filler that are used for soft capsule, can be made into have resisting fatigue, the preparation of oxygen lack resistant function.
The specific embodiment
A kind of high-assay highland barley flavones, its content of total flavone are 20%～45%, and effective ingredient lutonarin (Lutonarin) content is 12%～25%, and ZAOCAO xanthosine (Saponarin) content is 8%～20%.
The chemical constitution of Lutonarin and Saponarin is as follows:
Embodiment 1 gets exsiccant Semen avenae nudae seedling raw material 2Kg, being cut into the segment of 1～2cm or being ground into coarse powder, is 20%～50% alcoholic solution with raw material weight 40～80 times of amounts, concentration, extracts 1～4 time down for 70～100 ℃ in temperature, each 0.5～4 hour, get extracting solution; 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＜10%, and room temperature leaves standstill 0.5～1h, with the filtration of 200～400 order filter clothes, and must filtrate.
With 300～350L filtrate flow through (source: Chemical Plant of Nankai Univ.) 10 centimetres of the diameters of Tian Chonging, high 120 centimetres glass adsorption column are that the water wash of 10～15 times of amounts of packing material is to colourless with volume earlier with macroporous resin AB-8; The reuse volume is that packing material 20～30 times of amounts, concentration are behind 20%～60% the ethanol elution, and the R2002K type 20L Rotary Evaporators of producing with Wuxi Xing Hai king's biochemical equipment company limited concentrates and reclaims eluent, thick paste; Be cooled to room temperature again with 80%～95% ethanol elder generation thermosol at last, separate out precipitate, rotating speed centrifugal filtration with 4000～5000 rev/mins, put into 101-1A type baking oven (temperature is controlled at 80～90 ℃) inner drying that Tianjin Tai Site Instr Ltd. produces then, promptly get high-assay highland barley flavones.
The heavy 18.6g of this extract, yield 0.93%, extract through high-efficient liquid phase chromatogram HPLC (source: U.S. Agilent company, Agilent1100) measure and contain Lutonarin28%; Saponarin17%, the total flavones amount is 45%.
Embodiment 2 gets exsiccant Semen avenae nudae seedling raw material 2Kg, being cut into the segment of 1～2cm or being ground into coarse powder, is 20%～50% alcoholic solution with raw material weight 40～80 times of amounts, concentration, extracts 1～4 time down for 70～100 ℃ in temperature, each 0.5～4 hour, get extracting solution; Adopt the vacuum pump decompression of bleeding then, reclaim ethanol in the extracting solution to determining alcohol＜10%, room temperature leaves standstill 0.5～1h, filters with 200～400 order filter clothes, must filtrate.
With 300～350L filtrate flow through (source: the glass adsorption column of Tian Chonging Chemical Plant of Nankai Univ.) is that the water wash of 10～15 times of amounts of packing material is to colourless with volume earlier with macroporous resin D101; The reuse volume is that packing material 20～30 times of amounts, concentration are behind 20%～60% the ethanol elution, concentrate with the 20L Rotary Evaporators and reclaim eluent, thick paste; Be cooled to room temperature again with 80%～95% ethanol elder generation thermosol at last, separate out precipitate,, put into 80～90 ℃ of baking oven inner dryings then, promptly get high-assay highland barley flavones with 4000～5000 rev/mins rotating speed centrifugal filtration.
The heavy 12.4g of this extract, yield 0.62%, extract measure through HPLC and contain Lutonarin12%; Saponarin8%, the total flavones amount is 20%.
Embodiment 3 gets exsiccant Semen avenae nudae seedling raw material 2Kg, being cut into the segment of 1～2cm or being ground into coarse powder, is 20%～50% alcoholic solution with raw material weight 40～80 times of amounts, concentration, extracts 1～4 time down for 70～100 ℃ in temperature, each 0.5～4 hour, get extracting solution; Adopt the vacuum pump decompression of bleeding then, reclaim ethanol in the extracting solution to determining alcohol＜10%, room temperature leaves standstill 0.5～1h, filters with 200～400 order filter clothes, must filtrate.
With 300～350L filtrate flow through (source: the glass adsorption column of Tian Chonging Sichuan morning twilight engineering designing institute) is that the water wash of 10～15 times of amounts of packing material is to colourless with volume earlier with macroporous resin D140; The reuse volume is that packing material 20～30 times of amounts, concentration are behind 20%～60% the ethanol elution, concentrate with the 20L Rotary Evaporators and reclaim eluent, thick paste; Be cooled to room temperature again with 80%～95% ethanol elder generation thermosol at last, separate out precipitate,, put into 80～90 ℃ of baking oven inner dryings then, promptly get high-assay highland barley flavones with 4000～5000 rev/mins rotating speed centrifugal filtration.
The heavy 16.5g of this extract, yield 0.82%, extract measure through HPLC and contain Lutonarin22%; Saponarin14%, the total flavones amount is 36%.
Embodiment 4 gets exsiccant Semen avenae nudae seedling raw material 2Kg, being cut into the segment of 1～2cm or being ground into coarse powder, is 20%～50% alcoholic solution with raw material weight 40～80 times of amounts, concentration, extracts 1～4 time down for 70～100 ℃ in temperature, each 0.5～4 hour, get extracting solution; Adopt the vacuum pump decompression of bleeding then, reclaim ethanol in the extracting solution to determining alcohol＜10%, room temperature leaves standstill 0.5～1h, filters with 200～400 order filter clothes, must filtrate.
With the glass adsorption column of 450～500L filtrate flow, be that the water wash of 10～15 times of amounts of packing material is to colourless with volume earlier through filling with macroporous resin AB-8; The reuse volume is that packing material 20～30 times of amounts, concentration are behind 20%～60% the ethanol elution, concentrate with the 20L Rotary Evaporators and reclaim eluent, thick paste; Be cooled to room temperature again with 80%～95% ethanol elder generation thermosol at last, separate out precipitate,, put into 80～90 ℃ of baking oven inner dryings then, promptly get high-assay highland barley flavones with 4000～5000 rev/mins rotating speed centrifugal filtration.
The heavy 20.4g of this extract, yield 1.02%, extract measure through HPLC and contain Lutonarin25%; Saponarin20%, the total flavones amount is 45%.
Embodiment 5 contains producing of highland barley flavone extract tablet.
Write out a prescription every: highland barley flavone extract 50mg
Microcrystalline cellulose 60mg
Starch 85mg
Magnesium stearate 5mg
Method for making: highland barley flavone extract is pulverized, pressed the formula proportion mix homogeneously with various adjuvants behind 200～400 mesh sieves excessively; Use 80% alcohol granulation, granulate, compacting is in blocks, every 200mg.
Embodiment 6 contains producing of highland barley flavone extract hard capsule.
Write out a prescription every: highland barley flavone extract 50mg
Starch 140mg
Polyethylene Glycol 10mg
Method for making: highland barley flavone extract is pulverized, pressed the formula proportion mix homogeneously with various adjuvants behind 200～400 mesh sieves excessively; Press the formula proportion mix homogeneously with various adjuvants, encapsulated, every 200mg.
Embodiment 7 contains producing of highland barley flavone extract soft capsule.
Write out a prescription every: highland barley flavone extract 50mg
Cera Flava 10mg
Edible vegetable oil 140mg
Method for making: highland barley flavone extract is pulverized, crossed 200～400 mesh sieves; Get edible vegetable oil by formula proportion and be heated to 80 ℃, add the suspending agent Cera Flava, it is dissolved, cool to 30～40 ℃, add extract powder, mixing is crossed the SMA-0.75 type colloid mill that Shanghai Suowei Electromechanical Equipment Co., Ltd. produces, and is pressed into soft capsule.
Embodiment 8 contains producing of highland barley flavone extract granule.
Highland barley flavone extract 50mg
Lactose 950mg
Method for making: highland barley flavone extract is pulverized, pressed formula proportion and lactose mix homogeneously behind 200～400 mesh sieves excessively, use 70% alcohol granulation, granulate, packing (every pouch 1g) gets final product.
Embodiment 9 contains producing of highland barley flavone extract oral liquid.
Highland barley flavone extract 2.5g
Potassium sorbate 0.3g
White sugar 60g
Pure water 1000g
Method for making: highland barley flavone extract is adopted pulverizing, put into 80～90 ℃ of pure water thermosols after crossing 200～400 mesh sieves, adopt the GQ75 type tube centrifuge of sky, PVG this centrifugal machine company limited production to cross the filtering insoluble matter again with 20000 rev/mins speed, add potassium sorbate, white sugar then, mixing carries out canned (every 20ml) behind ultraviolet disinfection.
Claims (3)
1. high-assay highland barley flavones, it is characterized in that: content of total flavone is 20%～45% in the described extract; Effective ingredient lutonarin content is 12%～25%, and ZAOCAO xanthosine content is 8%～20%; This preparation method of extract may further comprise the steps:
(1) Semen avenae nudae seedling dry, after pulverizing is added aquiferous ethanol solution with conventional reflux, extract, method extract extracting solution, reclaim ethanol in the extracting solution to determining alcohol＜below 10%, filter, get filtrate; Described reflux, extract, condition is 70～100 ℃ of temperature, and the feed liquid weight ratio is 1: 40～1: 80, concentration of alcohol 20%～50%;
(2) adsorption column of filtrate flow through being filled with adsorbing material adsorbs; Described adsorbing material is a macroporous adsorbent resin, and this macroporous resin is a kind of among AB-8, D101 or the D140;
(3) extremely colourless with the water wash adsorption column;
(4) with volume be the alcoholic solution eluting of 20～30 times of amounts of packing material, concentration 20%～60%, collect eluent;
(5) concentrate the recovery eluent, get thick paste;
(6) ethanol with concentration 80%～95% is cooled to room temperature again to thick paste elder generation thermosol, separates out precipitate, with 4000～5000 rev/mins rotating speed centrifugal filtration, promptly gets extract at 80～90 ℃ of baking oven inner dryings then.
2. the application of high-assay highland barley flavones as claimed in claim 1 in the preparation health product is characterized in that: highland barley flavone extract is pulverized, added conventional pharmaceutic adjuvant behind 200～400 mesh sieves excessively, mix, be processed into oral formulations.
3. the application of high-assay highland barley flavones as claimed in claim 2 in the preparation health product, it is characterized in that: described oral formulations is tablet, hard capsule, soft capsule, granule or oral liquid.
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| CN102060825A (en) * | 2009-11-13 | 2011-05-18 | 天津市食品研究所有限公司 | Method for extracting flavone from young barley grass |
| CN101829284B (en) * | 2010-03-19 | 2012-01-11 | 陈元涛 | Process for extracting and refining flavone in highland barley seedlings by enzymolysis-membrane ultrafiltration |
| CN107242353A (en) * | 2016-07-27 | 2017-10-13 | 江西中成人药业有限公司 | Stress crude granule and preparation method thereof |
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| CN1907433A (en) * | 2005-08-01 | 2007-02-07 | 王文敦 | Process for extracting physiologically active substance from highland barley tender leaf |
| JP3937188B2 (en) * | 1996-03-01 | 2007-06-27 | 日本薬品開発株式会社 | Lutonalin production method |
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| JP3937188B2 (en) * | 1996-03-01 | 2007-06-27 | 日本薬品開発株式会社 | Lutonalin production method |
| CN1907433A (en) * | 2005-08-01 | 2007-02-07 | 王文敦 | Process for extracting physiologically active substance from highland barley tender leaf |
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| 张立武.青稞麦绿素的制备及其抗疲劳和耐缺氧功能评价.《青稞麦绿素的制备及其抗疲劳和耐缺氧功能评价》.2005,全文. * |
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Effective date of registration: 20200514 Address after: 810000 room 12002, building 1, No. 7, jingsan Road, Qinghai Biotechnology Industrial Park, Xining City, Qinghai Province Patentee after: QINGDAO JINMAIQI BIOTECHNOLOGY Co.,Ltd. Address before: 810001 Qinghai province Xining City West Street No. 59 Patentee before: Northwest Institute of Plateau Biology, Chinese Academy of Sciences |