CN102308987B - Production method for extracting glucoside type seabuckthorn flavones from sea-buckthorn leaf - Google Patents
Production method for extracting glucoside type seabuckthorn flavones from sea-buckthorn leaf Download PDFInfo
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Abstract
The invention discloses a production method for extracting glucoside type seabuckthorn flavones from sea-buckthorn leaves and the method comprises the following steps: carrying out pre-processed machining, such as cleaning, jordaning and the like to fresh sea-buckthorn leaves or picked fallen leaves; taking ethanol as solvent; and under the action of ultrasonic wave, further breaking plant cells to release glucoside type seabuckthorn flavones-Isorhamnetin, wherein the extraction ratio is 95.6%. Compared with the traditional method, the production method disclosed by the invention has the advantages of low temperature, constant pressure, no toxic solvent residue, low energy consumption, short extraction period and high extraction efficiency, does not damage or degrade effective ingredients and is suitable for mass production; and the additional value of agricultural products is improved.
Description
Technical field
The present invention relates to the technical field of the processing extracting method of International Classification of Patents A23L food or foodstuff, especially from the sea-buckthorn leaf, extract the production method of glucosides type Hippophate flavone.
Background technology
Sea-buckthorn has another name called vinegar willow, acid thorn.Fruit juice contains multivitamin, amino acid, trace element and flavone compound.The fruit of sea-buckthorn can be treated burn, telephium, frostbite, lacerated wound, skin surface ulcer, telephium, extract and hippophae rhamnoides patch, medicinal extract etc. also can be treated gastric ulcer, tracheitis, bedsore etc., and prevention and professional venereal diseases such as treatment lead, phosphorus, benzene, indigestion, subcutaneous hemorrhage, irregular menstruation etc. all there are certain curative effect.Prescription or decoction control also that cough, phlegm are many, pulmonary abscess, pulmonary tuberculosis etc.Seed can be made cathartic.Fructus hippophae syrup treatment chronic bronchitis, expectorant effect is relatively good.
Sea-buckthorn has multiple product, and as sea-buckthorn electuary, sea-buckthorn ketone sheet, sea-buckthorn essence, sea-buckthorn wet goods, these products all have good effect to chronic bronchitis, cough, indigestion, ischemic cardiomyopathy, allevating angina pectoris etc.The function of sea-buckthorn electuary is cough-relieving apophlegmatic, relieving dyspepsia, promoting blood circulation to remove blood stasis, tonifying spleen stomach invigorating.
Seabuckthorm Seed Oil has protective effect to the carbon tetrachloride liver damage, there is no acute and chronic toxic reaction.Seabuckthorn Oil lipopenicillinase experiment shows to have the effect of the exogenous high fat experimental rat serum total cholesterol of obvious reduction, can increase rat blood serum HDL-C, and the liver lipid content is increased.The ability that protection is arranged and accelerate to repair gastric mucosa helps to strengthen the therapeutic action of antineoplastic.Contain A family, B family vitamin and a large amount of unrighted acid in the Seabuckthorn Oil, feed every part to hen and contain 0.5～1.0% Seabuckthorn Oil, can improve the adipochrome of yolk and chicken body.Seabuckthorn Oil has anesthesia character, once be used for the treatment of totally 72 people such as burn, vitamin A shortage, acute erosion eczema, chronic eczema, mycotic eczema, seborrheic eczema, infantile eczema, scales of skin that peel off shape rash, pyodermia, cutaneous tuberculosis, total effective rate 62/72.Seabuckthorn Oil treatment wound can be made into various formulations, as dripping pill or emulsion etc.Seabuckthorn Oil treatment burn effect is remarkable, the fat-soluble solution of sea-buckthorn that Qinghai Medicine College provides with the northwest plateau biological study, and treatment burn 100 examples, efficient more than 90%.Soak the cotton yarn flap coverage with seabuckthorn preparation, purulence is oozed out obvious minimizing, and the growth of epithelium granulation tissue is accelerated, and wound healing all improved about a week.
Contain abundant vitamin C in the sea-buckthorn essence, to improving sportsman's ability, improving the cardiovascular system function and the good influence that dispelled fatigue quickly, contained potassium, magnesium, calcium, sodium, iron, zinc, copper etc. are to guaranteeing the significance that is supplemented with of element that sportsman's large amount of exercise consumes and trace element.The sea-buckthorn essence is coughed, breathed heavily chronic bronchitis all curative effect preferably.Through treating 61 examples, cardinal symptoms such as coughing, cough up phlegm, pant, breathe hard is all had obvious curative effects, simultaneously to sleep, promote digestion, eliminate abdominal fullness and distention certain curative effect is also arranged that rheopneumogram is had in various degree improvement.
Sea-buckthorn (H ipp op hae rham noid es L.) is the inferior arbor of the shrub of Elaeangnaceae Hippophne, is rich in flavone compound in the sea-buckthorn leaf.The extraction of general flavone mainly contains water extract method, buck extraction and solvent refluxing extraction method, and these method complex operations, recovery rate are low.Ultrasonic wave can make micro-bubble compression, the explosion of extracting in the medium, and the cell membrane of broken raw material accelerates stripping, the diffusion of active ingredient, can shorten extraction time greatly, improves extraction efficiency.Ultrasonic technique be applied in the extraction research of natural products, and ultrasonic circulation technique is to apply ultrasonic wave in the process that feed liquid circulates, and is a kind of new technology of extracting natural products as a kind of effective extracting method.
Total seabuckthorn flavone has antagonism to the multiple room of animal and VA model, increases the myocardial nutritional flow amount of being tried mouse, improves myocardium microcirculation, reduces the MCO effect.Clinical proof can be improved the myocardial blood supply state, improves microcirculation, allevating angina pectoris, improve palpitaition, uncomfortable in chest, breathe hard, reduce serum cholesterol and triglycerides, to experimental chronic hepatitis due to the carbon tetrachloride.Antiviral, anti-sclerosis, anti-inflammatory are arranged and strengthen effect capillaceous.Disclosed sea-buckthorn processing method is less.Mainly from dried plant sea-buckthorn pulp, extract Hippophate flavone.Because fructus hippophae is direct-edible, or is easy to as multiple deep processing raw material, and price is higher, make existing technology obtain Hippophate flavone cost costliness, influence further application and development.
For example: aspect production technology, and for example: the refinement method of number of patent application CN86108906 Seabuckthorn Oil is raw material with hippophae rhamnoides seed, pulp, pomace, fruit juice floating thing, has fully utilized various light wood material processed.For retentive activity composition as much as possible, adopt mixed solvent or the single fat hydrocarbon solvent of aliphatic hydrocarbon and ketone to leach, with the film-type evaporation precipitation, again with the gained crude oil in same container come unstuck under the condition of 15～25 ℃ of temperature, depickling, dewaxing and then be lower than decolouring under 65 ℃ the condition, deodorization namely gets refining Seabuckthorn Oil processed.
In addition, research and analyse and think, flavones content is comparatively approaching in the flavones in the sea-buckthorn blade and the sea-buckthorn pulp, is generally 0.9-1.3%.Its difference only is, aglycon type flavones large percentage in the sea-buckthorn pulp, and in the blade based on the Hippophate flavone of glucosides type, be that the method that raw material extracts flavones is not seen open as yet with the sea-buckthorn blade.
Summary of the invention
The purpose of this invention is to provide a kind of is that raw material extracts flavones processing treatment technology with the sea-buckthorn blade, and this technology is carried out preliminary treatment and extraction at the characteristic of sea-buckthorn blade, in the hope of obtaining dna purity and recovery rate preferably.
Goal of the invention of the present invention realizes by following technical measures: the sea-buckthorn leaf adds ethanol through behind the ultrasonic extraction through after comprising the preliminary treatment of defibrination, extract is carried out cryogenic separation, ethanol reclaim, the working substance drying makes.
After preliminary treatment such as the defibrination processing, make solvent with ethanol, under action of ultrasonic waves, further broken plant cell discharges glucosides type Hippophate flavone---Isorhamnetin, and recovery rate can reach 95.6%.Relatively conventional method have that low temperature, normal pressure, no toxic solvent are residual, low energy consumption, extraction cycle weak point, the effective ingredient of not destroying and degrade, advantage that recovery rate is high, suitable large-scale production has promoted additional value of farm products.
The invention has the beneficial effects as follows: utilize fresh sea-buckthorn blade or the fallen leaves selected after preliminary treatment such as cleaning, defibrination processing, make solvent with ethanol, under action of ultrasonic waves, further broken plant cell, discharge glucosides type Hippophate flavone---Isorhamnetin, recovery rate can reach 95.6%.Relatively conventional method have that low temperature, normal pressure, no toxic solvent are residual, low energy consumption, extraction cycle weak point, the effective ingredient of not destroying and degrade, advantage that recovery rate is high, suitable large-scale production has promoted additional value of farm products.
Description of drawings:
Fig. 1 is technological process simplified schematic diagram of the present invention
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.
The sea-buckthorn leaf adds ethanol through behind the ultrasonic extraction through after comprising the preliminary treatment of defibrination, extract is carried out cryogenic separation, ethanol reclaim, the working substance drying makes.
Specifically, sea-buckthorn fallen leaves through letter sorting, are soaked 20min and clean 3 times with running water, again with the drying chamber of putting into 60 ℃ behind the centrifuge dewatering, 24h is standby in oven dry.Get the dry blade of 10kg and pulverize with pulverizer, with the 20kg running water powder is soaked 20min, send into fiberizer under stirring and carry out the defibrination preliminary treatment; Again the liquid slurry is injected in the ultrasonic response still, and add 95% edible ethanol 150kg, and input power is the ultrasonic wave of 200W, 25kHz service intermittent mode, work and dwell time all are set at 2min, temperature of reaction kettle keeps 45 ℃, and the whole ultrasonic ripple extraction time is 20min.Again extract is put into cold catch pot, temperature keeps 10 ℃, leaves standstill 12h, gets supernatant and sends in the decompression distillation still after whizzer filters, and is warming up to 50 ℃, is decompressed to 0.08MPa, reclaims ethanol.Elimination water when extract is cooled to room temperature at the bottom of the still, and spend deionised water 4 times, filter is put into vacuum refrigeration case inner drying 12h after doing, and product obtains glucosides type Hippophate flavone-Isorhamnetin 94.65g, extraction rate reached 95.6% after testing.
Use the sea-buckthorn blade as raw material, key is after cleaning, dirt and residues of pesticides on the blade are removed fully, has guaranteed the avirulence of product.
The material that soaked is carried out the defibrination preliminary treatment, make material refinement more, granularity is easy to reach 0.3-1 μ m.
When ultrasonic wave acts on vegetable slurries, because the high-pressure spray that the cavity that the shock wave that dither produces forms forms when collapse, can produce powerful shear action to plant cell, plant cell is broken, accelerate intracellular active principle and fully discharged.
Under 45-50 degree temperature conditions, the characteristic of utilizing flavones to be soluble in ethanol extracts, and whole extraction process needs 10-30min.
As preferred embodiments, better with the low-frequency ultrasonic waves effect, frequency of ultrasonic and power output are chosen to be 20-30KHz, and power is 100-500w.
The of short duration service intermittent mode that adopts, and the work dwell time all is set at 2min.Adopt of short duration service intermittent mode, in cell, produce the heat energy cumulative effect to prevent ultrasonic wave.
Material is soaking defibrination under the wetting state in the present embodiment, when guaranteeing large-scale production, can not destroy effective ingredient because pulverizing the localized hyperthermia that produces again, reduces dust simultaneously.
Extraction solvent adopts 95% edible ethanol, the water yield joint account that adds during with immersion, and average ethanol content has satisfied the valid density of ethanol when extracting at 60-70%.
The sea-buckthorn blade, particularly fallen leaves are a kind of discarded objects originally, and the exploitation blade extracts active principle, and lifting additional value of farm products that can be bigger descends production cost significantly.
Claims (2)
1. extract the production method of glucosides type Hippophate flavone from the sea-buckthorn leaf, it is characterized in that: the sea-buckthorn leaf adds ethanol through behind the ultrasonic extraction through after comprising the preliminary treatment of defibrination, extract is carried out cryogenic separation, ethanol reclaim, the working substance drying makes; Sea-buckthorn is fallen leaves through letter sorting, soak 20min and clean 3 times with running water, again with the drying chamber of putting into 60 ℃ behind the centrifuge dewatering, 24h is standby in oven dry, getting the dry blade of 10kg pulverizes with pulverizer, with the 20kg running water powder is soaked 20min, send into fiberizer under stirring and carry out the defibrination preliminary treatment; Again the liquid slurry is injected in the ultrasonic response still, and add 95% edible ethanol 150kg, input power is 200W, the ultrasonic wave of 25kHz service intermittent mode, work and dwell time all are set at 2min, temperature of reaction kettle keeps 45 ℃, the whole ultrasonic ripple extraction time is 20min, again extract is put into cold catch pot, temperature keeps 10 ℃, leaves standstill 12h, gets supernatant and sends in the decompression distillation still after whizzer filters, be warming up to 50 ℃, be decompressed to 0.08MPa, reclaim ethanol, elimination water when extract is cooled to room temperature at the bottom of the still, and spend deionised water 4 times, filter is put into vacuum refrigeration case inner drying 12h after doing, and product obtains glucosides type Hippophate flavone-Isorhamnetin 94.65g, extraction rate reached 95.6% after testing.
2. the production method of extracting glucosides type Hippophate flavone from the sea-buckthorn leaf as claimed in claim 1 is characterized in that the material that soaked is carried out defibrination, and granularity reaches 0.3-1 μ m.
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| CN103211761A (en) * | 2013-04-07 | 2013-07-24 | 史小军 | Seabuckthorn seed oil oral emulsion with gastric mucosa protective effect and preparation method and use thereof |
| CN104490956B (en) * | 2014-12-25 | 2017-12-29 | 上海交通大学 | A kind of total seabuckthorn flavone purifying technique |
| CN105982369B (en) * | 2016-06-12 | 2017-07-21 | 浙江梦娜袜业股份有限公司 | A kind of preparation method of the mosquito-proof quilted stockings of plants essential oil |
| CN108553559B (en) * | 2018-06-22 | 2021-03-23 | 南昌糖友安健康科技有限公司 | Formula and preparation method of vegetable and fruit extract for preventing and treating type II diabetes |
| CN109082723B (en) * | 2018-08-28 | 2021-02-09 | 山西恒义生物集团有限公司 | Sea buckthorn leaf cellulose fiber |
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Denomination of invention: Method for extracting glycosidic seabuckthorn flavone from seabuckthorn leaves Effective date of registration: 20220530 Granted publication date: 20130821 Pledgee: Bank of Urumqi Co.,Ltd. Urumqi high tech Zone sub branch Pledgor: XINJIANG KEYU TECHNOLOGY Co.,Ltd. Registration number: Y2022650000021 |
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Denomination of invention: Production Method of Extracting Glycoside Type Seabuckthorn Flavonoids from Seabuckthorn Leaves Effective date of registration: 20230308 Granted publication date: 20130821 Pledgee: Bank of Urumqi Co.,Ltd. Urumqi high tech Zone sub branch Pledgor: XINJIANG KEYU TECHNOLOGY Co.,Ltd. Registration number: Y2023980034361 |
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Denomination of invention: Production method for extracting glycosidic seabuckthorn flavonoids from seabuckthorn leaves Granted publication date: 20130821 Pledgee: Bank of Urumqi Co.,Ltd. Urumqi high tech Zone sub branch Pledgor: XINJIANG KEYU TECHNOLOGY Co.,Ltd. Registration number: Y2024650000007 |