CN103520213A - Preparation method for propolis flavoid extract and application of propolis flavoid extract - Google Patents
Preparation method for propolis flavoid extract and application of propolis flavoid extract Download PDFInfo
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- CN103520213A CN103520213A CN201310483526.5A CN201310483526A CN103520213A CN 103520213 A CN103520213 A CN 103520213A CN 201310483526 A CN201310483526 A CN 201310483526A CN 103520213 A CN103520213 A CN 103520213A
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Abstract
The invention discloses a preparation method for a propolis flavoid extract and application of the propolis flavoid extract. The preparation method comprises the following steps of a. freezing propolis under an environment of (-35)-(-5) DEG C for 6-10 hours, and performing superfine grinding, wherein the particle size of propolis particles subjected to the superfine grinding is 20-80 micrometers; b. adding an ethanol solution with the concentration of 68-75 percent into the smashed propolis particles, and immersing the propolis particles for 8-12 hours, wherein the volume adding amount of the ethanol solution is 20-40 times of the weight of the propolis particles; c. performing ultrahigh-pressure extraction on a mixed solution in the step b to obtain an extracting solution, wherein the extraction pressure is 400-600MPa, and the extraction time is 6-12min; and d. concentrating and drying the extracting solution in the step c to obtain a finished propolis flavoid extract. The preparation method for the propolis flavoid extract, which is disclosed by the invention, is high in extraction efficiency and low in production cost; the flavoid extract is high in purity; the propolis flavoid extract can be used for curing osteoporosis.
Description
Technical field
The present invention relates to compound extractive technique field, be specifically related to a kind of preparation method and its usage of propolis flavone extract.
Background technology
Propolis resin similar substance and the endocrine complex compound of Apis that to be Apis gather from the raw branch of collagen plant axillalry bud, have the effects such as antibiotic, antiviral, enhancing immunity, has higher using value.In propolis, contain the multiple compounds such as flavonoid, phenolic acids, wherein, flavone compound is the main active substances in propolis, plays a part main in the various pharmacological actions of propolis.Propolis flavone compounds can help human body control various diseases, makes the various function normalization of body, enhancingization, can be applicable in the disease treatment of hyperlipidemia, coronary heart diseases and angina pectoris.Therefore, propolis flavone compounds is extracted and had great importance.
In prior art, the extracting method of propolis flavone mainly contains alcohol steep method, microwave extraction method, supercritical CO
2extraction etc.Wherein, microwave extraction method extraction time is short, and extraction ratio is high compared with alcohol steep method, but can produce a large amount of Cera Flavas, has reduced the purity of propolis flavone extract; Supercritical CO
2extraction no solvent residue, impurity is few, but because flavone compound is at supercritical fluid CO
2in dissolubility low, in extraction process, need to add entrainer to increase dissolubility, the flavone extract that the extraction that is obtains is mixed with entrainer, affects the purity of flavone extract, and supercritical CO
2extraction process cost is high, in commercial Application, is not generally promoted; Alcohol steep method is simple to operate, and the production cycle is long, and extraction efficiency is not high.
Summary of the invention
The object of the invention is to overcome above shortcoming, provide a kind of extraction efficiency high, production cost is low, and the preparation method and its usage of the high propolis flavone extract of flavone extract purity.
Technical scheme of the present invention is:
A preparation method for propolis flavone extract, comprises the steps:
A, propolis is carried out to micronizing processing after freezing 6-10h under-35 ℃～-5 ℃ environment, the propolis grain graininess after described micronizing is processed is 20-80 μ m;
B, to adding concentration in the propolis granule after pulverizing, be the alcoholic solution of 68-75%, soak 8-12h; The volume addition of described alcoholic solution is 20-40 times of propolis particle weight;
C, the mixed solution in step b is carried out to hyperpressure extraction, obtain extracting solution, wherein, extraction pressure is 400-600Mpa, and extraction time is 6-12min;
D, by the extracting solution in step c concentrate, dry, obtain propolis flavone extract finished product.
Further, in described step b, the concentration of alcoholic solution is 70-72%.
Further, described soaking temperature is 65-70 ℃.
Further, in described step c, the extraction pressure of hyperpressure extraction technique is 400-500Mpa.
Further, the weight of described propolis flavone extract is the 52-56% of described propolis gross weight.
The purposes of a kind of propolis flavone extract in treatment osteoporosis agents.
The preparation method of propolis flavone extract provided by the invention, tool has the following advantages:
1, the preparation method of propolis flavone extract provided by the invention, extraction efficiency is high, and production cost is low.The preparation method of propolis flavone extract provided by the invention, comprise that freezing, micronizing processing, alcohol solution dipping, hyperpressure extraction are processed, the technique such as concentrated, carry out after micronizing processing, the grain graininess of propolis is 20-80 μ m, there is good dissolubility, dispersibility, reactivity, after alcohol solution dipping, can improve the extracted amount of propolis flavone compounds; Propolis mixed liquor after immersion carries out hyperpressure extraction processing again, under the condition of supertension, alcoholic solution can be penetrated in the cell of propolis flavone compounds within the extremely short time, and propolis flavone compounds is dissolved in rapidly in alcoholic solution, and extraction efficiency is high.After testing, the weight of propolis flavone extract is the 52-56% of propolis gross weight.
The preparation method of propolis flavone extract provided by the invention, processes micronizing, soak and extract and the combination of hyperpressure extraction technique, and the extraction process of propolis flavone compounds is optimized, and has improved the extraction efficiency of propolis flavone compounds; And time shorten, the hyperpressure extraction process time of soaking extraction process are short, whole extraction process is simplified, and production cost is low.
2, the preparation method of propolis flavone extract provided by the invention, the flavone extract purity obtaining is high.The preparation method of propolis flavone extract provided by the invention, comprises hyperpressure extraction technique, and the flavone extractive clarity that obtains is high, good stability, impurity content are few, thereby makes the flavone extract purity that obtains high, function admirable.Because the impurity content of flavone extractive is few, can simplify purifying process afterwards, thereby further simplify the extraction process of propolis flavone compounds.
The specific embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for propolis flavone extract, comprises the steps:
A, propolis is carried out to micronizing processing after freezing 6h under-35 ℃ of environment, the propolis grain graininess after micronizing is processed is 80 μ m;
B, to adding concentration in the propolis granule after pulverizing, be 68% alcoholic solution, soak 8h; The volume addition of alcoholic solution is 20 times of propolis particle weight; According to 1 gram of propolis, add the ratio of 20ml alcoholic solution to process;
C, the mixed solution in step b is carried out to hyperpressure extraction, obtain extracting solution, wherein, extraction pressure is 400Mpa, and extraction time is 6min;
D, by the extracting solution in step c concentrate, dry, obtain propolis flavone extract finished product; In concentrated, drying process, can remove the ethanol containing in extracting solution.
According to above-mentioned process, the weight of the propolis flavone extract preparing is 52% of propolis gross weight, and extraction efficiency is high.
Embodiment 2
A preparation method for propolis flavone extract, comprises the steps:
A, propolis is carried out to micronizing processing after freezing 8h under-20 ℃ of environment, the propolis grain graininess after micronizing is processed is 50 μ m;
B, to adding concentration in the propolis granule after pulverizing, be 70% alcoholic solution, under 65 ℃ of conditions, soak 10h; The volume addition of alcoholic solution is 30 times of propolis particle weight; According to 1 gram of propolis, add the ratio of 30ml alcoholic solution to process;
C, the mixed solution in step b is carried out to hyperpressure extraction, obtain extracting solution, wherein, extraction pressure is 500Mpa, and extraction time is 10min; Hyperpressure extraction technique is carried out at normal temperatures;
D, by the extracting solution in step c concentrate, dry, obtain propolis flavone extract finished product.
According to above-mentioned process, the weight of the propolis flavone extract preparing is 56% of propolis gross weight, and extraction efficiency is high.
Embodiment 3
A preparation method for propolis flavone extract, comprises the steps:
A, propolis is carried out to micronizing processing after freezing 10h under-5 ℃ of environment, the propolis grain graininess after micronizing is processed is 80 μ m;
B, to adding concentration in the propolis granule after pulverizing, be 72% alcoholic solution, under 70 ℃ of conditions, soak 9h; The volume addition of alcoholic solution is 40 times of propolis particle weight; According to 1 gram of propolis, add the ratio of 40ml alcoholic solution to process;
C, the mixed solution in step b is carried out to hyperpressure extraction, obtain extracting solution, wherein, extraction pressure is 600Mpa, and extraction time is 12min; Hyperpressure extraction technique is carried out at normal temperatures;
D, by the extracting solution in step c concentrate, dry, obtain propolis flavone extract finished product.
According to above-mentioned process, the weight of the propolis flavone extract preparing is 55% of propolis gross weight, and extraction efficiency is high.
Embodiment 4
A preparation method for propolis flavone extract, comprises the steps:
A, propolis is carried out to micronizing processing after freezing 7h under-10 ℃ of environment, the propolis grain graininess after micronizing is processed is 60 μ m;
B, to adding concentration in the propolis granule after pulverizing, be 75% alcoholic solution, under 68 ℃ of conditions, soak 11h; The volume addition of alcoholic solution is 25 times of propolis particle weight; According to 1 gram of propolis, add the ratio of 25ml alcoholic solution to process;
C, the mixed solution in step b is carried out to hyperpressure extraction, obtain extracting solution, wherein, extraction pressure is 560Mpa, and extraction time is 8min; Hyperpressure extraction technique is carried out at normal temperatures;
D, by the extracting solution in step c concentrate, dry, obtain propolis flavone extract finished product.
According to above-mentioned process, the weight of the propolis flavone extract preparing is 54% of propolis gross weight, and extraction efficiency is high.
The impact of the propolis flavone extract preparing according to technical scheme of the present invention on ovariectomized female rats bone metabolism:
1, materials and methods
Select 21 of healthy rats, female, at 6 monthly ages, body weight 18-22g, is divided into each seven of blank group, model control group and propolis flavone extract groups at random.
2, the foundation of model
After each group is all anaesthetized with the anesthetis of equivalent, the position of bowing is fixing, aseptic disinfecting.Blank group is at spinal column both sides otch, and each excises a fritter fat (approximate with ovarian size); Model control group and propolis flavone extract matched group excise respectively bilateral ovaries, after performing the operation three days, enter experiment.
Blank group, model control group gavage are to distilled water 8mlKg
-1d
-1; Propolis flavone extract group gavage is to propolis flavone extract 80mgKg
-1d
-1; Each group all gives normal feedstuff, freely drinks water.Experimental period 10 weeks, experiment finishes the previous day and collects and respectively organize Rat 24 h urine with metabolic cage; When experiment finishes, gather centrifugal blood and collect serum.
3, assay method
With serum alkaline phosphatase determination box, survey serum levels of ALP, atomic absorption spectrophotometer is surveyed urine calcium, and hydroxyproline testing cassete is surveyed urine HOP.
4, serum levels of ALP, urine calcium, urine HOP measurement result
Model control group is compared with blank group, and serum levels of ALP increases (P < 0.01) urine calcium, urine HOP increases (P < 0.05); Propolis flavone extract group is compared with model control group, and serum levels of ALP, urine calcium reduce (P < 0.05), and urine HOP reduces (P < 0.01); Propolis flavone extract group and blank group indices are all without significant difference (P > 0.05).Specific experiment data see the following form:
Serum levels of ALP participates in the adjusting of bone metabolism, and content increases, and bone metabolism parameter increases, and between bone formation parameter and ALP measured value, has dependency.Urine calcium is the result of the multiple effect comprehensive functions such as intestinal calcium absorption, bone calcium dissolve, renal tubules calcium heavily absorbs.24h total amount can reflect the situation of bone resorption in bone metabolism substantially, and HOP is the main component for human collagen, can be used to evaluate the situation of bone resorption in body.Propolis flavone extract group is compared serum levels of ALP and is reduced with model control group, the adjusting that is conducive to bone metabolism is described, reduces bone loss; Urine calcium reduces, and prompting calcium is lost and reduced, and to becoming bone metabolism, is favourable, promotes the formation of bone; Urine HOP reduces, and shows that bone resorption reduces, and improves bone and transforms.Propolis flavone extract group is compared with blank group, and above index is all without significant difference.
In this experiment, take ovariectomized female rats as object of study, is that estrogen long-term lacking there will be the symptoms such as osteoporosis because ovary produces estrogen.The effect known by above-mentioned experiment, propolis flavone extract has the osteoporosis of preventing to occur and develop, and can improve bone metabolism, the discharge of minimizing calcium, promoting bone growing, inhibition bone resorption.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing, be equal to replacement etc., within all should being included in protection scope of the present invention in protection scope of the present invention.
Claims (6)
1. a preparation method for propolis flavone extract, is characterized in that, described preparation method comprises the steps:
A, propolis is carried out to micronizing processing after freezing 6-10h under-35 ℃～-5 ℃ environment, the propolis grain graininess after described micronizing is processed is 20-80 μ m;
B, to adding concentration in the propolis granule after pulverizing, be the alcoholic solution of 68-75%, soak 8-12h; The volume addition of described alcoholic solution is 20-40 times of propolis particle weight;
C, the mixed solution in step b is carried out to hyperpressure extraction, obtain extracting solution, wherein, extraction pressure is 400-600Mpa, and extraction time is 6-12min;
D, by the extracting solution in step c concentrate, dry, obtain propolis flavone extract finished product.
2. the preparation method of propolis flavone extract according to claim 1, is characterized in that, in described step b, the concentration of alcoholic solution is 70-72%.
3. the preparation method of propolis flavone extract according to claim 2, is characterized in that, described soaking temperature is 65-70 ℃.
4. the preparation method of propolis flavone extract according to claim 1, is characterized in that, in described step c, the extraction pressure of hyperpressure extraction technique is 400-500Mpa.
5. according to the preparation method of the propolis flavone extract described in any one in claim 1 to 4, it is characterized in that, the weight of described propolis flavone extract is the 52-56% of described propolis gross weight.
Propolis flavone extract claimed in claim 1 in treatment the purposes in osteoporosis agents.
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| CN110946998A (en) * | 2019-12-13 | 2020-04-03 | 河南牧业经济学院 | Propolis extract containing ferulic acid compound and extraction method and application thereof |
| KR20200145047A (en) * | 2019-06-20 | 2020-12-30 | 한남대학교 산학협력단 | A pharmaceutical composition for preventing or treating osteoporosis comprising propolis extract as an active ingredient |
| CN114224920A (en) * | 2022-01-24 | 2022-03-25 | 吉林蜂道馆健康产业有限公司 | Bee therapy product with sterilizing and inflammation diminishing functions and preparation method thereof |
| CN114392278A (en) * | 2022-01-23 | 2022-04-26 | 吉林蜂道馆健康产业有限公司 | Mutation-resistant and radiation-resistant bee therapy product and preparation method thereof |
| CN114558035A (en) * | 2022-04-29 | 2022-05-31 | 中国农业科学院蜜蜂研究所 | Propolis flavone extract and preparation method and application thereof |
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Application publication date: 20140122 |