CN1528130A - Method for extracting functional ingredient of bee glue by ultrasonic wave process - Google Patents
Method for extracting functional ingredient of bee glue by ultrasonic wave process Download PDFInfo
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- CN1528130A CN1528130A CNA031350917A CN03135091A CN1528130A CN 1528130 A CN1528130 A CN 1528130A CN A031350917 A CNA031350917 A CN A031350917A CN 03135091 A CN03135091 A CN 03135091A CN 1528130 A CN1528130 A CN 1528130A
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Abstract
The present invention relates to a method for extracting functional components of propolis by utilizing ultrasonic wave technology, belonging to the field of propolis extract technology. Said invention uses ethyl alcohol as solvent, and adopts the following steps: freezing crude propolis, pulverizing and dissolving the crude propolis in ethyl alcohol, extracting by using ultrasonic technique, filtering, vacuum concentrating filtrate so as to obtain the finished product propolis. At the same time of vacuum concentration the ethyl alcohol can be synchronously recovered. It can raise extraction rate, shorten extraction time and can prepare high-quality propolis product.
Description
Technical field
A kind of ultrasonic technology extracts the method for propolis functional ingredient, belongs to the propolis extract technology field.
Background technology
Propolis (propolis) is described as " purple gold ", is the natural gum of honeybee from plant gemma and trunk collection, and sneaks into a kind of colloidal solid thing with aromatic odor of honeybee mandibular gland secretion and beeswax.The resinae, the aromatic oil that wherein contain 50-55%, the beeswax of 30-40%, the pollen of 5-10% also has alkyl acid oil, grease, amino acid, organic acid, iron, copper, manganese, zinc, phytocide, vitamin B group, vitamin E, C, H, provitamin A, antibiotic, enzyme etc.From compound, mainly contain flavonoids, organic acid compound, ester, aldehyde, alcohol compound and alkene, hydrocarbon, obedient compounds etc.Flavonoids is the main bioactivator of propolis, and kind more than 20 is arranged approximately, comprises flavonoids, flavonols and flavanone class.
The report about the aspect research of propolis pharmacological increases gradually in the document in recent years.Propolis product is widely used clinically, mainly contain antitumor, resisting pathogenic microbes, protection liver, can play immunoregulation effect, anti-oxidant, improve cardiovascular system, anti-inflammatory and antiallergic action, radioresistance, antiulcer.
Bee product is that the Nature is given the whole mankind common treasure, the whole world has many countries all being engaged in the R and D of bee product, especially Germany, Japan, Romania, New Zealand, Australia etc., annual research paper about propolis reaches a hundreds of piece of writing, especially more deep to Pharmacological action study, propolis is developed to series of products by external many countries, is the product great reputation particularly of development of raw materials with Brazilian propolis, and price is also very expensive.Be cosmetics, the bactericide that raw material is made with propolis, widely known in many countries, especially be proved when many cancer cells are had toxic action when propolis, propolis product is more praised highly.
Propolis must be through the processing leaching process before becoming medicine, and process extracts its useful factor exactly.The useful factor in the propolis is a lot, and flavones is wherein most important composition.Flavones is to have the natural activity compound that valuable pharmacological is worth, and has anti-ageing, nourishing, regulates immunization.
At present, the method of extracting functional components in the propolis both at home and abroad all is to utilize it can be dissolved in the characteristic of alcohol well, and adopt alcohol to extract, but because its extraction time is long, recovery rate is low, and finding that a kind of new method can improve the recovery rate of propolis and shorten extraction time becomes current much-talked-about topic.
Ultrasonic is meant that the per second vibration frequency is higher than 20000 times people's the inaudible high-frequency sound of ear.Hyperacoustic facilitation is mainly derived from its cavitation phenomenon.Ultrasonic cavitation is acoustochemical energy source, can relate to effects such as phonochemistry, photochemistry in the ultrasonic reaction process, produces huge energy.Utilize cavitation effect of ultrasonic waves, can improve the reaction velocity of many chemical reactions.A series of experimental results show that: ultrasonic wave energy changes the assembled state of material, and material is disperseed and emulsification, changes material diffusion, crystallization and dissolution velocity; Accelerated reaction and some technical process of reinforcement.Ultrasonic wave energy is quickened acting in the light industry of heterogeneous diffusion and is most widely used, and heterogeneous diffusion generally is a procedure the most slowly in the various process.Ultrasonic technology is applied to propolis extract this industry, the relevant bibliographical information of Shang Weijian.
Summary of the invention
The purpose of this invention is to provide the method that a kind of ultrasonic technology extracts propolis functional ingredient,, improve recovery rate, shorten extraction time, prepare high-quality propolis product with the extraction process of intensified by ultrasonic wave propolis.
Technical solution of the present invention is to adopt ultrasonic extracting process, is solvent with ethanol, will be dissolved in the ethanol after the freezing pulverizing of thick propolis, and Extraction by Ultrasound, filtration, filtrate is carried out vacuum concentration, makes the product propolis.During vacuum concentration, reclaim ethanol synchronously, the solid-liquid ratio of thick propolis and ethanol is 1: 5-25 (w/v).Ultrasonic treatment time is 10-60min, and the processing ultrasonic power is 500-1000w.Its preferably process conditions be: the solid-liquid ratio of thick propolis and ethanol is 1: 15 (w/V), and ultrasonic treatment time is 25min, and power is 750w.
Natural propolis is sneaked into impurity such as a large amount of beeswaxs, honeybee corpse, wood chip and earth in gatherer process.Therefore, when producing propolis product, need purify to thick propolis.
Propolis is water-soluble hardly, be soluble in methyl alcohol, ethanol, the acetone and other organic solvent, methyl alcohol, ethanol and ethyl acetate etc. all are the better solvents that extracts propolis, the three is to the recovery rate of propolis and the stripping quantity no significant difference of flavones, but the stripping quantity to beeswax has nothing in common with each other, no significant difference between methyl alcohol and ethanol wherein, but have significant difference between methyl alcohol, ethanol and ethyl acetate.So ethanol is optimal solvent at present.
Traditional ethanol extraction method is that the ethanol of already pulverised thick propolis sample with finite concentration, certain solid-liquid ratio is mixed, main component in the thick propolis is dissolved out, through behind the certain hour, the various compositions in the propolis will be dissolved in the ethanol to some extent and go.
Generally speaking, the rising temperature can both improve the dissolution characteristics of material greatly, therefore can be applied to the Soxhlet extraction process of present classics the ethanol extraction method of propolis.Pretreated propolis sample is extracted as the solvent high temperature reflux with 95% ethanol, the Flavonoid substances in the sample is entered in the solvent, reclaim that the product of gained is exquisite propolis behind the solvent.This method can extract the Flavonoid substances in the propolis more completely, but required time is longer, and solvent-oil ratio is big, and the stripping quantity of beeswax is also bigger, has hindered normally carrying out of extracting, and needs special Soxhlet extractor.
The typical process flow of Extraction by Ultrasound as shown in Figure 2.
Ethanol extraction method:
Table 1 ethanol extraction method gained general flavone content and recovery rate
| Tested number | General flavone content (%) | Recovery rate (%) |
| ????1 | ????8.10 | ????18.56 |
| ????2 | ????8.85 | ????19.29 |
| Mean value | ????8.475 | ????18.91 |
The method required extraction time is grown (needing 32 hours at least) very much, and recovery rate is not high.
The method is very simple, and temperature is not high, and some volatile and effective flavonoids inactivation is difficult for losing, but recovery rate is subjected to time restriction, and industrial large-scale production efficient is extremely low.
The Soxhlet extraction process:
Table 2 Soxhlet extraction process gained general flavone content
| Tested number | General flavone content (%) |
| ????1 | ????9.46 |
| ????2 | ????9.65 |
| Mean value | ????9.555 |
The Soxhlet extracting is after 8 hours, and as seen the Flavonoid substances major part stripping of propolis sample, heats up and can shorten extraction time really.But this method equipment needed thereby input is bigger, so also be not suitable in industrial large-scale application.
Ultrasonic extraction:
By research, can determine the process conditions preferably of Extraction by Ultrasound propolis, solid-liquid ratio 1: 15, processing time 25min handles ultrasonic power 750w.Experimental result sees the following form:
Table 7 Different Extraction Method result relatively
| Experimental technique | Conventional extraction method | The Soxhlet extraction process | Ultrasonic |
| Time | ????32h | ????8h | ????25min |
| Solid-liquid ratio | ????1∶15 | ????1∶15 | ????1∶15 |
| Power | ????500w | ????500w | ????750w |
| General flavone content (%) | ????8.475 | ????9.555 | ????10.02 |
| Recovery rate (%) | ????18.91 | ????* | ????34.26 |
*Because beeswax separates out when temperature is higher in a large number, when measuring recovery rate influence bigger, so when the Soxhlet extracting, fail accurately to measure recovery rate.
As seen from the above table, ultrasonic has greater advantage in the extraction application facet of propolis.
Beneficial effect of the present invention:
Tradition ethanol extraction method required time is longer, and recovery rate is low.It is too high that the Soxhlet extraction process extracts temperature, and some other compositions have also been put forward, and influence the extraction process, and the equipment input is bigger.Ultrasonic is compared preceding two kinds of methods and is greatly increased aspect extraction time and recovery rate, only need a 25min just the alcohol soluble substance major part in the propolis to be put forward, for the extraction of functional components in the propolis provides a kind of effective method.
Can find out significantly that ultrasonic is having huge advantage aspect extraction time and the recovery rate, so the extraction that the using ultrasound ripple quickens propolis is very effective.This explanation, Extraction by Ultrasound has huge future, and is suitable for industrial applications.
Ultrasonic has quickened material Transfer, under lower temperature, just can obtain effect preferably, natural flavour mountaineous, the color and the heat-sensitive substance that have kept raw material effectively, and ultrasonic has continuation to the invigoration effect of propolis, after promptly stopping the ultrasonic effect, its effect of quickening extraction propolis process still can continue for some time.Therefore it will have more wide development space in food industry.
Description of drawings
Fig. 1 ultrasonic response device schematic diagram
1, reaction bench, 2, supersonic generator, 3, metallic support, 4, transformer.
Fig. 2 Extraction by Ultrasound typical process flow figure
Specific embodiments
Embodiment 1:
With the thick propolis of dissolve with ethanol, solid-liquid ratio 1: 15 (w/v), handle 25min with the 750w ultrasonic, general flavone content reaches 10.02% in the solution, and recovery rate is 34.26%.
Claims (2)
1, a kind of ultrasonic technology extracts the method for propolis functional ingredient, it is characterized in that adopting ultrasonic extracting process, is solvent with ethanol, will be dissolved in the ethanol after the freezing pulverizing of thick propolis, Extraction by Ultrasound, filtration, filtrate is carried out vacuum concentration, makes the product propolis, during vacuum concentration, reclaim ethanol synchronously, the feed liquid by weight/volume of thick propolis and ethanol is 1: 5-25, ultrasonic treatment time are 10-60min, and the processing ultrasonic power is 500-1000w.
2, method according to claim 1, the feed liquid by weight/volume that it is characterized in that thick propolis and ethanol is 1: 15, and ultrasonic treatment time is 25 minutes, and the processing ultrasonic power is 750w.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA031350917A CN1528130A (en) | 2003-09-30 | 2003-09-30 | Method for extracting functional ingredient of bee glue by ultrasonic wave process |
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| CNA031350917A CN1528130A (en) | 2003-09-30 | 2003-09-30 | Method for extracting functional ingredient of bee glue by ultrasonic wave process |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2070543A1 (en) * | 2007-12-12 | 2009-06-17 | Bios Line S.p.a. | High-efficiency procedure for preparing standarized hydroalcoholic propolis extract |
| CN100500164C (en) * | 2005-03-10 | 2009-06-17 | 浙江省中医药研究院 | Process for preparing bee glue water solution and use |
| CN102349605A (en) * | 2011-10-19 | 2012-02-15 | 北京农科亿健蜂产品研究院 | Propolis extraction method and propolis capsule |
| CN102404998A (en) * | 2009-05-14 | 2012-04-04 | 生物蜂胶技术株式会社 | Method for extracting propolis using far-infrared rays from earthenware |
| CN104719706A (en) * | 2015-04-07 | 2015-06-24 | 北京农科亿健蜂产品研究院 | Propolis purification method |
| CN105534850A (en) * | 2015-12-30 | 2016-05-04 | 苏州威尔德工贸有限公司 | Propolis-containing skin moisturizing product for infants and preparation method thereof |
| CN106805177A (en) * | 2017-01-06 | 2017-06-09 | 重庆师范大学 | A kind of extracting method of propolis |
| CN109197683A (en) * | 2018-11-29 | 2019-01-15 | 桑植县湘西密码生物科技有限公司 | Mobile honey harvests platform |
-
2003
- 2003-09-30 CN CNA031350917A patent/CN1528130A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100500164C (en) * | 2005-03-10 | 2009-06-17 | 浙江省中医药研究院 | Process for preparing bee glue water solution and use |
| EP2070543A1 (en) * | 2007-12-12 | 2009-06-17 | Bios Line S.p.a. | High-efficiency procedure for preparing standarized hydroalcoholic propolis extract |
| CN102404998A (en) * | 2009-05-14 | 2012-04-04 | 生物蜂胶技术株式会社 | Method for extracting propolis using far-infrared rays from earthenware |
| CN102349605A (en) * | 2011-10-19 | 2012-02-15 | 北京农科亿健蜂产品研究院 | Propolis extraction method and propolis capsule |
| CN104719706A (en) * | 2015-04-07 | 2015-06-24 | 北京农科亿健蜂产品研究院 | Propolis purification method |
| CN105534850A (en) * | 2015-12-30 | 2016-05-04 | 苏州威尔德工贸有限公司 | Propolis-containing skin moisturizing product for infants and preparation method thereof |
| CN105534850B (en) * | 2015-12-30 | 2019-01-11 | 苏州威尔德工贸有限公司 | A kind of moisturising product of propolis-containing for baby and preparation method thereof |
| CN106805177A (en) * | 2017-01-06 | 2017-06-09 | 重庆师范大学 | A kind of extracting method of propolis |
| CN106805177B (en) * | 2017-01-06 | 2020-04-07 | 重庆师范大学 | Propolis extraction method |
| CN109197683A (en) * | 2018-11-29 | 2019-01-15 | 桑植县湘西密码生物科技有限公司 | Mobile honey harvests platform |
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