CN1628703A - Method for extracting propolis effective component under high pressure - Google Patents
Method for extracting propolis effective component under high pressure Download PDFInfo
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- CN1628703A CN1628703A CNA2004100110775A CN200410011077A CN1628703A CN 1628703 A CN1628703 A CN 1628703A CN A2004100110775 A CNA2004100110775 A CN A2004100110775A CN 200410011077 A CN200410011077 A CN 200410011077A CN 1628703 A CN1628703 A CN 1628703A
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Abstract
The invention provides a method for extracting propolis effective component under high pressure, which comprises, (1) cooling the bee glue at below -20 deg. C for 6-12 hours, then comminuting, (2) passing the disintegrated material through 20-60 mesh sieve, (3) mixing the sieved material with solvent, (4) placing the mixture in a high-pressure vessel, carrying out heavy pressure extraction at normal temperature, the pressure is 100-600 MPa, the pressure sustaining time is 1-15 minutes, (5) filtering the raffinate in a filter.
Description
Technical field:
The present invention relates to a kind of process of under normal temperature condition, extracting effective ingredient in the propolis.
Background technology
Propolis is the natural gum of Apis from plant sprout bud and trunk collection, and sneaks into a kind of gluey solid content with aromatic odor that Apis mandibular gland secretions and Cera Flava etc. process.That propolis has is antibiotic, suppress virus, opposing toxoid and regulate effects such as body immunity.Propolis contains a large amount of flavonoid (flavone, flavonol and flavanone), aromatic acid, aliphatic acid and ester thereof, and terpenes, have biology and pharmacological actions such as antibiotic, antifungal, antiviral, antitumor, antioxidation, antiinflammatory, anesthesia, be subjected to the extensive attention and the further investigation of medical circle.The major function composition of propolis is a total flavones, and flavone is to have the natural activity chemical compound that valuable pharmacological is worth, and has defying age, nourishing, adjusting immunization.Here said effective ingredient is meant flavone compound.
The extracting method of propolis mainly contains: traditional ethanol extraction is a most popular method of extracting effective ingredient in the propolis; The research that the supercritical carbon dioxide extraction technology is extracted effective ingredient in the propolis is in exploration and key stage; Water-bath circumfluence method, microwave extraction and ultrasound assisted extraction technique also are in conceptual phase at present.
Tradition ethanol extraction: the process conditions that what is discussed well with reference to bee product quality supervision and test test center of the Ministry of Agriculture: 75% and 95% alcoholic solution, 4 ℃ were soaked 14 days.This method is simple to operate, and is temperature required not high, and some volatile and effective flavonoid inactivation is difficult for losing, but the production cycle is long, and extraction ratio is not high.
The supercritical carbon dioxide extraction technology: extract with this technology that flavone compound has lot of advantages in propolis,, no solvent residue, safety and Health yellowish as color and luster, impurity is few, content of beary metal is low, technological process is simple etc.But when adopting supercritical liquid extraction technique, because flavone compound, lactone and the dissolubility of material in supercritical fluid CO2 such as polysaccharide, protein and tannin are extremely low, therefore need to add the phase behavior that an amount of entrainer changes the shooting flow system, to increase its dissolubility.Though entrainer brings benefit to supercritical liquid extraction technique, can increase some equipment and energy consumption to separation that extracts miscellaneous entrainer in the matter and the recovery that is present in the entrainer in the residue.
Water-bath circumfluence method: turn round and look at the blue or green process conditions of discussing with reference to Hangzhou Commercial College: 95% alcoholic solution, 85 ℃ of water-baths refluxed 6 hours.The not only required temperature of this method is higher, and can produce a large amount of Cera Flavas, has increased the difficulty of later separation and purification.
The microwave extraction technology: this technology is that 24.5 hundred million hyperfrequencies of per second that produce by magnetron shake fast, make molecule, especially polarizable medium (as: water, ethanol), concussion at a high speed, spin taking place, has increased the ability that solvent enters solute inside, and because intermolecular friction generates heat mutually, also promoted the leaching of effective ingredient in the propolis, made whole extraction time shorten, extraction ratio increases.But, increased the difficulty of isolation and purification operation because the heat effect of microwave may make some that heat sensitive flavone compound is lost activity, and can produce a large amount of Cera Flavas.
Ultrasonic wave extraction: ultrasound wave is a kind of elastic mechanical vibration wave, is the sonic vibration beyond the audition.Because ultrasonic have special roles such as cavitation, pulverizing, stirring, the cell of medical material there is breakoff phenomenon, solvent is penetrated in the cell of medical material, thereby the chemical constituent in the medical material is dissolved among the solvent.It is simple, easy to operate that ultrasound assisted extraction technique has equipment, and extraction time is short, and the extraction ratio height need not advantages such as heating.But because the destruction of ultrasound wave pair cell, make the crude drug cell fragmentation, increased the difficulty of later separation and purification procedures.
Summary of the invention
The objective of the invention is to extract the above-mentioned shortcoming that effective bee glue components exists, propose a kind of effective bee glue components high pressure extract method, with further raising extraction ratio and simplification extraction process for overcoming present habitual process.
Extracting method of the present invention is being raw material, making solvent with water or ethanol, methanol, ether, acetic acid, acetone, benzene and aqueous solution thereof without removing mellisic thick propolis, and its processing step is as follows:
A. propolis is pulverized after cooling off 6～12 hours under-20 ℃ of temperature;
B. pulverize and expected 20～60 mesh sieves;
C. will go up preface minus mesh and solvent, its charge ratio is a propolis: solvent=1 gram: 5～45 milliliters;
D. said mixture is put into high-pressure bottle, apply high pressure extract at normal temperatures, its pressure is 100～600MPa, and pressurize is 1～15 minute time;
E. after said extracted liquid filters, be the effective bee glue components extracting solution in filter.
For the effective ingredient in the propolis is as far as possible all extracted, can carry out repeatedly high pressure extract repeatedly, the filtering residue after extracting of soon last time exerting pressure is with the extraction of exerting pressure once more of same process condition.Experimental results show that when extraction time is 1～3 time, the effective ingredient in the propolis all can be extracted.
Because propolis when temperature is 20～40 ℃, has strong viscosity and plasticity, therefore in order can successfully to pulverize, result of the test pre-cooling under-20 ℃ of conditions was spent the night 6～12 hours, can realize crushing effect preferably.
The particulate granularity of propolis is more little, and its surface area is big more, and is big more with the contact surface of solvent, thereby the media table area is big more, has accelerated the extraction rate of effective ingredient.If but granularity is too little, then can increase the isolating difficulty of extracting liquid filtering.Through a large amount of experimentatioies, when granularity was 20～60 mesh sieves, the effect of experiment was best.
The extracting solution that is obtained also can pass through the one matter that operations such as separation, purification obtain various compositions, perhaps multiple mixture of ingredients, for example, propolis dropping liquid, bee glue soft capsule, propolis tablet, propolis extractum; Also can operate and directly use without separation, purification etc., for example, propolis liquid etc.
The maximum characteristics of effective bee glue components high pressure extract method of the present invention are to finish under room temperature, condition of high voltage, have the following advantages:
(1) the extraction yield of high pressure extract method is very high, increases by 8% than traditional ethanol extraction, increases by 17% than water-bath circumfluence method;
(2) extraction time of high pressure extract method is very short.This has illustrated that fully the high pressure extract technology has high efficient in the effective bee glue components leaching process, be present any extracting method can not compare;
(3) Cera Flava content is lower in the extracting solution of high pressure extract, so not only can reduce the consumption of the used medicines of operation such as separation and purification in a large number, and has shortened the time that operations such as separation and purification take equipment.
(4) high pressure extract is carried out in room temperature, and extraction time is very short, can avoid some that heat sensitive flavone compound is lost activity like this.
The specific embodiment
In the whole technology, pressure is core and key, and therefore, the specific embodiment that effective bee glue components extracts and the main difference of other method are also just in the HIGH PRESSURE TREATMENT stage.The selection of HIGH PRESSURE TREATMENT parameter is relevant with the physics and the factors such as chemical property, solvent and concentration thereof of effective ingredient in the propolis.
Embodiment 1
From thick propolis, extract effective bee glue components by following processing step and process conditions:
A. propolis is pulverized after 6-12 hour in cooling under-20 ℃ of temperature;
B. pulverize and expected 20～60 mesh sieves;
C. make solvent with 95% concentration ethanol, will go up preface minus mesh and solvent, its charge ratio is a propolis: solvent=1 gram: 35 milliliters;
D. said mixture is put into high-pressure bottle, apply high pressure extract at normal temperatures, its pressure is 500MPa, and the dwell time is 1 minute,
E. said extracted liquid filters in filter, is the effective bee glue components extracting solution,
F. the filtering residue that unloads behind the press filtration carries out 2 extractions of exerting pressure repeatedly under the identical condition again.
Under these process conditions, effective bee glue components total flavones extraction ratio is 5.1%.
Embodiment 2
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
With the distillation water as solvent, the ratio of propolis and solvent is 1g: 5ml, and extraction pressure is 100MPa, and the dwell time is 5min, and extraction time is 3 times, and the total flavones extraction ratio is 3.9%.
Embodiment 3
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Methanol aqueous solution with 75% is made solvent, and the ratio of propolis and solvent is 1g: 45ml, and extraction pressure is 200MPa, and the dwell time is 10min, and extraction time is 2 times, and the total flavones extraction ratio is 4.4%.
Embodiment 4
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Methanol aqueous solution with 50% is made solvent, and the ratio of propolis and solvent is 1g: 30ml, and extraction pressure is 300MPa, and the dwell time is 15min, and extraction time is 1 time, and the total flavones extraction ratio is 4.8%.
Embodiment 5
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Make solvent with absolute methanol, the ratio of propolis and solvent is 1g: 35ml, and extraction pressure is 400MPa, and the dwell time is 10min, and extraction time is 2 times, and the total flavones extraction ratio is 5%.
Embodiment 6
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ethanol water with 50% is made solvent, and the ratio of propolis and solvent is 1g: 20ml, and extraction pressure is 500MPa, and the dwell time is 1min, and extraction time is 2 times, and the total flavones extraction ratio is 4.4%.
Embodiment 7
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ethanol water with 75% is made solvent, and the ratio of propolis and solvent is 1g: 10ml, and extraction pressure is 600MPa, and the dwell time is 5min, and extraction time is 3 times, and the total flavones extraction ratio is 5.2%.
Embodiment 8
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Alcoholic solution with 100% is made solvent, and the ratio of propolis and solvent is 1g: 15ml, and extraction pressure is 400MPa, and the dwell time is 15min, and extraction time is 2 times, and the total flavones extraction ratio is 5.1%.
Embodiment 9
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Acetone soln with 100% is made solvent, and the ratio of propolis and solvent is 1g: 35ml, and extraction pressure is 500MPa, and the dwell time is 5min, and extraction time is 1 time, and the total flavones extraction ratio is 5.3%.
Embodiment 10
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Acetone soln with 50% is made solvent, and the ratio of propolis and solvent is 1g: 25ml, and extraction pressure is 100MPa, and the dwell time is 10min, and extraction time is 3 times, and the total flavones extraction ratio is 4.6%.
Embodiment 11
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Acetone soln with 5% is made solvent, and the ratio of propolis and solvent is 1g: 15ml, and extraction pressure is 600MPa, and the dwell time is 15min, and extraction time is 2 times, and the total flavones extraction ratio is 4.9%.
Embodiment 12
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Diethyl ether solution with 100% is made solvent, and the ratio of propolis and solvent is 1g: 40ml, and extraction pressure is 100MPa, and the dwell time is 1min, and extraction time is 2 times, and the total flavones extraction ratio is 5.2%.
Embodiment 13
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Diethyl ether solution with 50% is made solvent, and the ratio of propolis and solvent is 1g: 10ml, and extraction pressure is 200MPa, and the dwell time is 15min, and extraction time is 2 times, and the total flavones extraction ratio is 4.5%.
Embodiment 14
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Diethyl ether solution with 25% is made solvent, and the ratio of propolis and solvent is 1g: 20ml, and extraction pressure is 300MPa, and the dwell time is 15min, and extraction time is 3 times, and the total flavones extraction ratio is 4.4%.
Embodiment 15
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Diethyl ether solution with 100% is made solvent, and the ratio of propolis and solvent is 1g: 35ml, and extraction pressure is 500MPa, and the dwell time is 5min, and extraction time is 2 times, and the total flavones extraction ratio is 5.3%.
Embodiment 16
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ethylene glycol solution with 50% is made solvent, and the ratio of propolis and solvent is 1g: 25ml, and extraction pressure is 300MPa, and the dwell time is 15min, and extraction time is 3 times, and the total flavones extraction ratio is 4.5%.
Embodiment 17
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ethylene glycol solution with 15% is made solvent, and the ratio of propolis and solvent is 1g: 45ml, and extraction pressure is 400MPa, and the dwell time is 1min, and extraction time is 2 times, and the total flavones extraction ratio is 4.3%.
Embodiment 18
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Benzole soln with 100% is made solvent, and the ratio of propolis and solvent is 1g: 15ml, and extraction pressure is 400MPa, and the dwell time is 10min, and extraction time is 1 time, and the total flavones extraction ratio is 5.4%.
Embodiment 19
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Benzole soln with 50% is made solvent, and the ratio of propolis and solvent is 1g: 25ml, and extraction pressure is 200MPa, and the dwell time is 5min, and extraction time is 2 times, and the total flavones extraction ratio is 4.6%.
Embodiment 20
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Benzole soln with 15% is made solvent, and the ratio of propolis and solvent is 1g: 5ml, and extraction pressure is 150MPa, and the dwell time is 1min, and extraction time is 2 times, and the total flavones extraction ratio is 4.9%.
Embodiment 21
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ethylene glycol solution with 100% is made solvent, and the ratio of propolis and solvent is 1g: 15ml, and extraction pressure is 600MPa, and the dwell time is 15min, and extraction time is 3 times, and the total flavones extraction ratio is 5.4%.
Embodiment 22
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows: the ethylene glycol solution with 50% is made solvent, and the ratio of propolis and solvent is 1g: 25ml, extraction pressure is 500MPa, dwell time is 5min, and extraction time is 2 times, and the total flavones extraction ratio is 4.9%.
Embodiment 23
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ethylene glycol solution with 10% is made solvent, and the ratio of propolis and solvent is 1g: 25ml, and extraction pressure is 200MPa, and the dwell time is 10min, and extraction time is 1 time, and the total flavones extraction ratio is 4.6%.
Embodiment 24
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Sodium hydroxide solution with 2% is made solvent, and the ratio of propolis and solvent is 1g: 35ml, and extraction pressure is 400MPa, and the dwell time is 15min, and extraction time is 3 times, and the total flavones extraction ratio is 4.3%.
Embodiment 25
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ammonia spirit with 5% is made solvent, and the ratio of propolis and solvent is 1g: 15ml, and extraction pressure is 300MPa, and the dwell time is 5min, and extraction time is 2 times, and the total flavones extraction ratio is 4.2%.
Embodiment 26
Press embodiment 1 same process step and extract effective bee glue components, its process conditions are as follows:
Ammonia spirit with 25% is made solvent, and the ratio of propolis and solvent is 1g: 25ml, and extraction pressure is 400MPa, and the dwell time is 15min, and extraction time is 2 times, and the total flavones extraction ratio is 4.9%.
The selection principle of HIGH PRESSURE TREATMENT parameter is: guaranteeing under the product quality premise, selecting lower pressure and short dwell time as far as possible, to boost productivity, reducing energy resource consumption.
Claims (2)
1. effective bee glue components high pressure extract method being raw material, making solvent with water or ethanol, methanol, ether, acetic acid, acetone, benzene and aqueous solution thereof without removing mellisic thick propolis, is characterized in that comprising following processing step:
A. propolis is pulverized after cooling off 6～12 hours under-20 ℃ of temperature;
B. pulverize and expected 20～60 mesh sieves;
C. will go up preface minus mesh and solvent, its charge ratio is a propolis: solvent=1 gram: 5～45 milliliters;
D. said mixture is put into high-pressure bottle, apply high pressure extract at normal temperatures, its pressure is 100～600MPa, and pressurize is 1～15 minute time;
E. after said extracted liquid filters, be the effective bee glue components extracting solution in filter.
2. effective bee glue components high pressure extract method according to claim 1 is characterized in that also can repeatedly applying repeatedly high pressure extract to improve extraction ratio, and the filtering residue after the extraction of soon last time exerting pressure is with the extraction of exerting pressure once more of same process condition.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2004100110775A CN1628703A (en) | 2004-09-03 | 2004-09-03 | Method for extracting propolis effective component under high pressure |
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| CNA2004100110775A CN1628703A (en) | 2004-09-03 | 2004-09-03 | Method for extracting propolis effective component under high pressure |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103054907A (en) * | 2012-12-05 | 2013-04-24 | 天津隆顺榕发展制药有限公司 | Propolis flavonoid extractive and preparation method thereof |
| CN103520213A (en) * | 2013-10-15 | 2014-01-22 | 武汉瑞博科技发展有限责任公司 | Preparation method for propolis flavoid extract and application of propolis flavoid extract |
| CN105363030A (en) * | 2015-12-07 | 2016-03-02 | 山东华宏生物工程有限公司 | Preparation method of propolis ethanol extract |
| CN107320500A (en) * | 2017-07-10 | 2017-11-07 | 张松波 | A kind of method of purification of propolis |
-
2004
- 2004-09-03 CN CNA2004100110775A patent/CN1628703A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103054907A (en) * | 2012-12-05 | 2013-04-24 | 天津隆顺榕发展制药有限公司 | Propolis flavonoid extractive and preparation method thereof |
| CN103054907B (en) * | 2012-12-05 | 2014-10-15 | 天津隆顺榕发展制药有限公司 | Propolis flavonoid extractive and preparation method thereof |
| CN103520213A (en) * | 2013-10-15 | 2014-01-22 | 武汉瑞博科技发展有限责任公司 | Preparation method for propolis flavoid extract and application of propolis flavoid extract |
| CN105363030A (en) * | 2015-12-07 | 2016-03-02 | 山东华宏生物工程有限公司 | Preparation method of propolis ethanol extract |
| CN107320500A (en) * | 2017-07-10 | 2017-11-07 | 张松波 | A kind of method of purification of propolis |
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