CN115813979B - Propolis compound and preparation method thereof - Google Patents
Propolis compound and preparation method thereof Download PDFInfo
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- CN115813979B CN115813979B CN202310108269.0A CN202310108269A CN115813979B CN 115813979 B CN115813979 B CN 115813979B CN 202310108269 A CN202310108269 A CN 202310108269A CN 115813979 B CN115813979 B CN 115813979B
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Abstract
The invention relates to the field of propolis products, and particularly discloses a propolis compound and a preparation method thereof. The preparation method of the propolis compound comprises the following steps: step 1), putting propolis into ethanol solution with the mass concentration of 75-85%, and soaking and extracting at 50-60 ℃ for 6-8 hours to obtain propolis ethanol solution; step 2), putting the clove, the rheum emodi and the ailanthus altissima into boiling water, condensing and refluxing, continuously boiling for 5-6 hours, cooling to 50-60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, maintaining the temperature at 50-60 ℃, and soaking and extracting for 5-6 hours; step 3), filtering, taking filtrate, heating, concentrating and drying to obtain the propolis compound; flos Caryophylli, radix Rumicis, and herba Eichhorniae are sun-cured Chinese medicinal materials. The invention has the advantage of better curative effects of reducing blood fat, blood pressure and blood sugar.
Description
Technical Field
The invention relates to the field of propolis products, in particular to a propolis compound and a preparation method thereof.
Background
Propolis is a natural medicine, and is a viscous solid jelly formed by mixing plant resin collected by worker bees with secretions such as palate glands, wax glands and the like. The main effects include deficiency, turbid fat elimination and diabetes resistance; it is used externally to detoxify, detumescence, astringe and promote granulation. Can be used for treating asthenia, senilism, hyperlipidemia, and diabetes; it can be used for treating chapped skin, burn and scald.
Although propolis is a natural medicinal material with various effects, the propolis has a general effect on reducing blood fat, blood pressure and blood sugar, and has a slow curative effect, so there is room for improvement.
Disclosure of Invention
In order to achieve better curative effects of reducing blood fat, reducing blood pressure and reducing blood sugar, the application provides a propolis compound and a preparation method thereof.
In a first aspect, the present application provides a preparation method of a propolis compound, which adopts the following technical scheme:
a preparation method of propolis compound comprises the following steps:
step 1), putting propolis into ethanol solution with the mass concentration of 75-85%, and soaking and extracting at 50-60 ℃ for 6-8 hours to obtain propolis ethanol solution;
step 2), putting the clove, the rheum emodi and the ailanthus altissima into boiling water, condensing and refluxing, continuously boiling for 5-6 hours, cooling to 50-60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, maintaining the temperature at 50-60 ℃, and soaking and extracting for 5-6 hours;
step 3), filtering, taking filtrate, heating, concentrating and drying to obtain the propolis compound;
the flos Caryophylli, radix Rumicis, and herba Eichhorniae are sun-cured Chinese medicinal materials.
By adopting the technical scheme, the bee glue compound is prepared by compounding the clove, the rheum emodi, the ailanthus altissima and the bee glue, so that the bee glue compound has remarkable curative effects on lowering blood pressure, lowering blood fat and lowering blood sugar after taking, is quick in effect, is not easy to rebound obviously after short-term use, can be lowered to a safe level after taking for 1 month, has remarkable effect, can not generate remarkable drug resistance after continuous taking, can not cause rapid rebound of blood pressure, blood fat and blood sugar after taking for 3 months, and can effectively keep physical health for a long time.
The ethanol extraction of the propolis, the water extraction of the clove, the rheum officinale and the ailanthus altissima, and the combination of the special processes for continuous extraction enable the effective substances in the medicinal materials to be better extracted, the content of the effective components to be higher, and the types of the effective components to be rich, so that the effective components are matched with each other, and the obvious curative effects of reducing blood pressure, blood fat and blood sugar are realized.
Preferably, the input mass ratio of the propolis, the clove, the rheum officinale and the ailanthus altissima is 1:0.3:0.1:0.6.
by adopting the technical scheme, the extracted active ingredients are matched according to a certain proportion by adopting a special proportion, so that the synergistic matching effect is better, and the effects of reducing blood pressure, blood fat and blood sugar are better.
Preferably, in the step 3), after filtering, the filtrate is reserved, the filter residue is taken and burned to obtain plant ash, the plant ash is put into the filtrate, and after being stirred uniformly, the filtrate is filtered again to obtain secondary filtrate, and the secondary filtrate is heated, concentrated and dried to obtain the propolis compound.
Through adopting above-mentioned technical scheme, through burning the filter residue, form plant ash, through the input of plant ash, can effectively adsorb the acidic material in the propolis, reduce acidity for compound curative effect is better, and need not to throw into alkaline component, reduces the destruction to nutrient substance, and, in addition, the water-soluble substance in the plant ash can dissolve in the extract, makes the nutrient component of the extract of preparation higher, more is favorable to human health.
Preferably, in the step 3), the secondary filtrate is ultrafiltered by an ultrafiltration membrane and then concentrated by heating.
By adopting the technical scheme, harmful substances can be removed better through ultrafiltration, so that the extract is healthier and safer, and the efficacy of the extract is better.
Preferably, in the step 2), the clove, the rheum emodi and the ailanthus are frozen to-18 to-22 ℃ and then put into boiling water.
Through adopting above-mentioned technical scheme, through throwing into boiling water after freezing clove, rhaponticum carthamoides, the cell wall of messenger's frozen clove, rhaponticum carthamoides, the water hyacinth crassipes becomes fragile, under expend with heat and contract with cold, destroys the structure of cell wall and cell membrane better for the extraction effect is better, extracts the nutrient substance better, makes the nutrient substance of extract richer, and the curative effect is better.
Preferably, in the step 3), heating to 80-85 ℃ and recovering ethanol for 30-40 min, and then heating and concentrating to extract.
By adopting the technical scheme, the ethanol waste is reduced, the cost is reduced and the economic value is higher by recycling the ethanol.
Preferably, in the step 1), the mass of the ethanol solution with the mass concentration of 75-85% is 5-6 times of the mass of the added propolis, and in the step 2), the mass of the boiling water is 8-10 times of the total mass of the added clove, the rheum emodi and the ailanthus altissima.
By adopting the technical scheme, the extraction effect is better by adopting sufficient water and ethanol solution for extraction, and the nutrient substances are better released into the solvent based on concentration difference, so that the curative effect of the extract is better.
In a second aspect, the present application provides a propolis complex, which adopts the following technical scheme: a propolis composition is prepared by the above preparation method.
By adopting the technical scheme, the propolis compound has the advantages of better efficacy of reducing blood pressure, blood fat and blood sugar, quick and lasting effect and difficult rebound.
In summary, the present application has the following beneficial effects:
1. the invention prepares the propolis compound by compounding the clove, the rheum emodi, the ailanthus and the propolis, so that the propolis compound has remarkable curative effects on reducing blood pressure, blood fat and blood sugar after taking, especially has quicker effect, is not easy to generate obvious rebound after being used, can be reduced to a safe level after taking for 1 month, has remarkable effect, can not generate obvious drug resistance after being continuously taken for 3 months, can not cause rapid rebound of blood pressure, blood fat and blood sugar after being stopped for a short time (about 5-7 days), and can effectively keep the health for a long time.
2. The invention preferably extracts the propolis by alcohol, extracts the clove, the rheum officinale and the ailanthus altissima, and then combines the special processes of continuous extraction, so that the active substances in the medicinal materials are better extracted, the content of the active ingredients is higher, the types of the active ingredients are rich, and the active ingredients are matched with each other, thereby realizing the remarkable curative effects of reducing blood pressure, blood fat and blood sugar.
3. The invention preferably burns the filter residue to form plant ash, and can effectively adsorb acidic substances in the propolis, reduce acidity, avoid adding alkaline components and reduce damage to nutrient substances through the investment of the plant ash, and water-soluble substances in the plant ash can be dissolved in the extracting solution, so that the nutrient components of the prepared extract are higher and are more beneficial to human health.
Detailed Description
The present application is described in further detail below with reference to examples.
Example 1
A propolis composition is prepared from propolis, flos Caryophylli, radix Rumicis, and herba Eichhorniae by extracting.
Wherein the propolis is propolis crude gel purchased from Rui Jian Royal Beehive Co., ltd.
Wherein flos Caryophylli is sun-cured Chinese medicinal material, and is commercially available.
Wherein the Rumex madaio is sun-cured Chinese medicinal material, and is commercially available.
Wherein the herba Eichhorniae is sun-cured Chinese medicinal material, and is commercially available.
The preparation method of the propolis compound comprises the following steps:
step 1), weighing 1kg of propolis, putting into 5kg of ethanol solution with the mass concentration of 75%, continuously stirring at the rotating speed of 60r/min, and soaking and extracting at the temperature of 60 ℃ for 6 hours to obtain the propolis ethanol solution.
Step 2), weighing 0.3kg of clove, 0.1kg of rheum emodi and 0.6kg of ailanthus altissima swingle, putting into 8kg of boiling water, continuously stirring at the rotating speed of 60r/min, continuously stirring, condensing and refluxing, continuously boiling for 5h, cooling to 60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, continuously stirring at the rotating speed of 60r/min, maintaining the temperature of 60 ℃, and soaking and extracting for 5h.
Step 3), filtering with 200-mesh filter cloth, heating the filtrate to 85 ℃, recovering ethanol for 30min, heating and concentrating to extract, spraying powder and drying to obtain the propolis compound.
Example 2
A propolis composition is prepared from propolis, flos Caryophylli, radix Rumicis, and herba Eichhorniae by extracting.
Wherein the propolis is propolis crude gel purchased from Rui Jian Royal Beehive Co., ltd.
Wherein flos Caryophylli is sun-cured Chinese medicinal material, and is commercially available.
Wherein the Rumex madaio is sun-cured Chinese medicinal material, and is commercially available.
Wherein the herba Eichhorniae is sun-cured Chinese medicinal material, and is commercially available.
The preparation method of the propolis compound comprises the following steps:
step 1), weighing 1kg of propolis, putting into 6kg of ethanol solution with the mass concentration of 85%, continuously stirring at the rotating speed of 60r/min, and soaking and extracting at 50 ℃ for 8 hours to obtain the propolis ethanol solution.
Step 2), weighing 0.3kg of clove, 0.1kg of rheum emodi and 0.6kg of ailanthus altissima swingle, putting into 10kg of boiling water, continuously stirring at the rotating speed of 60r/min, continuously boiling for 6h by condensing and refluxing, cooling to 50 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, continuously stirring at the rotating speed of 60r/min, maintaining the temperature of 50 ℃, and soaking and extracting for 6h.
Step 3), filtering with 200-mesh filter cloth, heating the filtrate to 80 ℃, recovering ethanol for 40min, heating and concentrating to extract, spraying powder and drying to obtain the propolis compound.
Example 3
A propolis composition is prepared from propolis, flos Caryophylli, radix Rumicis, and herba Eichhorniae by extracting.
Wherein the propolis is propolis crude gel purchased from Rui Jian Royal Beehive Co., ltd.
Wherein flos Caryophylli is sun-cured Chinese medicinal material, and is commercially available.
Wherein the Rumex madaio is sun-cured Chinese medicinal material, and is commercially available.
Wherein the herba Eichhorniae is sun-cured Chinese medicinal material, and is commercially available.
The preparation method of the propolis compound comprises the following steps:
step 1), weighing 1kg of propolis, putting into 5kg of ethanol solution with the mass concentration of 75%, continuously stirring at the rotating speed of 60r/min, and soaking and extracting at the temperature of 60 ℃ for 6 hours to obtain the propolis ethanol solution.
Step 2), weighing 0.3kg of clove, 0.1kg of rheum emodi and 0.6kg of ailanthus altissima swingle, putting into 8kg of boiling water, continuously stirring at the rotating speed of 60r/min, continuously stirring, condensing and refluxing, continuously boiling for 5h, cooling to 60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, continuously stirring at the rotating speed of 60r/min, maintaining the temperature of 60 ℃, and soaking and extracting for 5h.
Step 3), filtering with 200-mesh filter cloth, standing filtrate, taking filter residues to dry in an oven at 150 ℃, then burning the filter residues to obtain plant ash, putting the plant ash into the filtrate at a rotating speed of 60r/min, stirring for 10min, filtering with 200-mesh filter cloth to obtain secondary filtrate, heating the secondary filtrate to 85 ℃, recovering ethanol for 30min, heating and concentrating to extract, spraying powder and drying to obtain the propolis compound.
Example 4
A propolis composition is prepared from propolis, flos Caryophylli, radix Rumicis, and herba Eichhorniae by extracting.
Wherein the propolis is propolis crude gel purchased from Rui Jian Royal Beehive Co., ltd.
Wherein flos Caryophylli is sun-cured Chinese medicinal material, and is commercially available.
Wherein the Rumex madaio is sun-cured Chinese medicinal material, and is commercially available.
Wherein the herba Eichhorniae is sun-cured Chinese medicinal material, and is commercially available.
The preparation method of the propolis compound comprises the following steps:
step 1), weighing 1kg of propolis, putting into 5kg of ethanol solution with the mass concentration of 75%, continuously stirring at the rotating speed of 60r/min, and soaking and extracting at the temperature of 60 ℃ for 6 hours to obtain the propolis ethanol solution.
Step 2), weighing 0.3kg of clove, 0.1kg of rheum emodi and 0.6kg of ailanthus altissima swingle, putting into 8kg of boiling water, continuously stirring at the rotating speed of 60r/min, continuously stirring, condensing and refluxing, continuously boiling for 5h, cooling to 60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, continuously stirring at the rotating speed of 60r/min, maintaining the temperature of 60 ℃, and soaking and extracting for 5h.
Step 3), filtering with 200-mesh filter cloth, standing filtrate, taking filter residues to dry in an oven at 150 ℃, burning the filter residues to obtain plant ash, putting the plant ash into the filtrate at a rotating speed of 60r/min, stirring for 10min, filtering with 200-mesh filter cloth to obtain secondary filtrate, ultrafiltering the secondary filtrate with an ultrafiltration membrane with a molecular weight cut-off of 500D and an operating pressure of 3bar, collecting the filtrate to obtain tertiary filtrate, heating the tertiary filtrate to 85 ℃, recovering ethanol for 30min, heating and concentrating to extract, spraying powder and drying to obtain the propolis compound.
Example 5
A propolis composition is prepared from propolis, flos Caryophylli, radix Rumicis, and herba Eichhorniae by extracting.
Wherein the propolis is propolis crude gel purchased from Rui Jian Royal Beehive Co., ltd.
Wherein flos Caryophylli is sun-cured Chinese medicinal material, and is commercially available.
Wherein the Rumex madaio is sun-cured Chinese medicinal material, and is commercially available.
Wherein the herba Eichhorniae is sun-cured Chinese medicinal material, and is commercially available.
The preparation method of the propolis compound comprises the following steps:
step 1), weighing 1kg of propolis, putting into 5kg of ethanol solution with the mass concentration of 75%, continuously stirring at the rotating speed of 60r/min, and soaking and extracting at the temperature of 60 ℃ for 6 hours to obtain the propolis ethanol solution.
Step 2), weighing 0.1kg of clove, 0.1kg of rheum emodi and 0.1kg of ailanthus altissima swingle, putting into 2.4kg of boiling water, continuously stirring at a rotating speed of 60r/min, condensing and refluxing, continuously boiling for 5h, cooling to 60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, continuously stirring at a rotating speed of 60r/min, maintaining at a temperature of 60 ℃, and soaking and extracting for 5h.
Step 3), filtering with 200-mesh filter cloth, heating the filtrate to 85 ℃, recovering ethanol for 30min, heating and concentrating to extract, spraying powder and drying to obtain the propolis compound.
Example 6
A propolis composition is prepared from propolis, flos Caryophylli, radix Rumicis, and herba Eichhorniae by extracting.
Wherein the propolis is propolis crude gel purchased from Rui Jian Royal Beehive Co., ltd.
Wherein flos Caryophylli is sun-cured Chinese medicinal material, and is commercially available.
Wherein the Rumex madaio is sun-cured Chinese medicinal material, and is commercially available.
Wherein the herba Eichhorniae is sun-cured Chinese medicinal material, and is commercially available.
The preparation method of the propolis compound comprises the following steps:
step 1), weighing 1kg of propolis, putting into 5kg of ethanol solution with the mass concentration of 75%, continuously stirring at the rotating speed of 60r/min, and soaking and extracting at the temperature of 60 ℃ for 6 hours to obtain the propolis ethanol solution.
Step 2), weighing 0.5kg of clove, 0.5kg of rheum emodi and 0.5kg of ailanthus altissima swingle, putting into 12kg of boiling water, continuously stirring at the rotating speed of 60r/min, continuously boiling for 5h by condensing and refluxing, cooling to 60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, continuously stirring at the rotating speed of 60r/min, maintaining the temperature of 60 ℃, and soaking and extracting for 5h.
Step 3), filtering with 200-mesh filter cloth, heating the filtrate to 85 ℃, recovering ethanol for 30min, heating and concentrating to extract, spraying powder and drying to obtain the propolis compound.
Comparative example 1
The propolis complex differs from example 1 only in that:
the equivalent of cinnamon is used for replacing clove.
Comparative example 2
The propolis complex differs from example 1 only in that:
the Hibiscus flower is used to replace Rumex madaio.
Comparative example 3
The propolis complex differs from example 1 only in that:
the Eichhornia crassipes is replaced by the same amount of radix Scutellariae.
Comparative example 4
The propolis complex differs from example 1 only in that:
the equivalent of cinnamon is used for replacing clove.
The Hibiscus flower is used to replace Rumex madaio.
The Eichhornia crassipes is replaced by the same amount of radix Scutellariae.
Experiment 1
The propolis compound of each example, i.e., the comparative example, was dissolved in deionized water to prepare an oral liquid.
Each bottle of oral liquid has a constant volume of 10ml, and each bottle of oral liquid contains 100mg of propolis compound.
A number of patients with three highs were summoned and the initial serum triglycerides, initial serum low density lipoprotein cholesterol, initial fasting blood glucose, and initial systolic blood pressure of the patients were measured.
Then, after breakfast and supper, one bottle of oral liquid is taken respectively, and after taking for 1 month and 3 months, serum triglyceride, serum low density lipoprotein cholesterol, fasting blood glucose and systolic blood pressure of the patient are measured again and are respectively recorded as 1 month serum triglyceride, 1 month serum low density lipoprotein cholesterol, 1 month fasting blood glucose, 1 month systolic blood pressure, 3 month serum triglyceride, 3 month serum low density lipoprotein cholesterol, 3 month fasting blood glucose and 3 month systolic blood pressure.
After taking for 3 months, stopping taking for 7 days, and measuring the serum triglyceride for stopping taking 7d, the serum low density lipoprotein cholesterol for stopping taking 7d, the fasting blood glucose for stopping taking 7d and the systolic pressure for stopping taking 7d again.
And then taken again for 3 months, i.e. after taking the total of 6 months, serum triglyceride for 6 months, serum low density lipoprotein cholesterol for 6 months, fasting blood glucose for 6 months, and systolic blood pressure for 6 months were measured again.
All patients had initial serum triglycerides in the range of 2.5-2.9 mmol/L. (to be reduced to 0.56-1.71)
The initial serum low density lipoprotein cholesterol of all patients was within 4.3-4.6 mmol/L. (to be reduced to 2.07-3.37)
All patients had an initial fasting blood glucose within 7.6-8.2 (to 3.9-6.1) (mmol/L).
All patients had an initial systolic blood pressure within 160-175 mmHg. (to be reduced to 90-119)
Every 10 patients were in a group, and the test data were averaged.
The specific test data for experiment 1 are detailed in tables 1-4.
TABLE 1
Serum triglyceride values
TABLE 2
Serum low density lipoprotein cholesterol value
TABLE 3 Table 3
Fasting blood glucose level
TABLE 4 Table 4
Systolic blood pressure value
According to the comparison of the data of the embodiment 1 and the data of the comparative examples 1 to 4 in the tables 1 to 4, when the propolis, the clove, the rheum officinale and the ailanthus altissima are adopted for compound extraction, the propolis compound has better effects of reducing blood fat, reducing blood sugar and reducing blood pressure, can reach normal values after taking the medicine for three months, stops taking the medicine for 7d, has insignificant rebound of blood fat, blood sugar and blood pressure and still is in safe values, has no significant drug resistance after continuously taking the medicine, does not continuously reduce blood fat, blood sugar and blood pressure, can continuously maintain physical health, has significantly reduced curative effect, cannot be synergistically acted with the propolis when the cinnamon, the hibiscus flower and the baical skullcap root are adopted to independently replace or completely replace the clove, the rheum officinale and the ailanthus altissima, has general effects of treating hyperlipidemia, hyperglycemia and hypertension, and has significant rebound after stopping taking the medicine.
According to the comparison of the data of the embodiment 1 and the embodiment 3 to 4 in the tables 1 to 4, the acid substances in the propolis can be adsorbed by burning the filter residues to form plant ash and mixing the plant ash with the filtrate, so that the curative effect is better, more harmful substances can be filtered by adding ultrafiltration, and the curative effect is further improved.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (7)
1. A preparation method of a propolis compound for reducing three highs is characterized by comprising the following steps: the method comprises the following steps:
step 1), putting propolis into ethanol solution with the mass concentration of 75-85%, and soaking and extracting at 50-60 ℃ for 6-8 hours to obtain propolis ethanol solution;
step 2), putting the clove, the rheum emodi and the ailanthus altissima into boiling water, condensing and refluxing, continuously boiling for 5-6 hours, cooling to 50-60 ℃, adding the propolis ethanol solution prepared in the step 1), mixing, maintaining the temperature at 50-60 ℃, and soaking and extracting for 5-6 hours;
step 3), filtering, taking filtrate, heating, concentrating and drying to obtain the propolis compound for reducing hypertension, hyperlipidemia and hyperglycemia;
the clove, the rheum emodi and the ailanthus are all sun-cured traditional Chinese medicinal materials;
the input mass ratio of the propolis, the clove, the rheum officinale and the ailanthus altissima is 1:0.3:0.1:0.6.
2. the method for preparing the three-high propolis complex in accordance with claim 1, which is characterized in that: in the step 3), the filtrate is reserved after filtration, the filter residue is taken and burnt to obtain plant ash, the plant ash is put into the filtrate and is stirred uniformly, the filtrate is filtered again to obtain secondary filtrate, and the secondary filtrate is heated, concentrated and dried to obtain the propolis compound.
3. The method for preparing the three-high propolis composite in accordance with claim 2, which is characterized in that: in the step 3), the secondary filtrate is ultrafiltered by an ultrafiltration membrane and then heated and concentrated.
4. The method for preparing the three-high propolis complex in accordance with claim 1, which is characterized in that: in the step 2), the clove, the rheum emodi and the ailanthus are frozen to-18 to-22 ℃ and then put into boiling water.
5. The method for preparing the three-high propolis complex in accordance with claim 1, which is characterized in that: in the step 3), when heating and concentrating, the mixture is heated to 80-85 ℃ firstly, ethanol is recovered for 30-40 min, and then the mixture is heated and concentrated to extract.
6. The method for preparing the three-high propolis complex in accordance with claim 1, which is characterized in that: in the step 1), the mass of the ethanol solution with the mass concentration of 75-85% is 5-6 times of the mass of the added propolis, and in the step 2), the mass of the boiling water is 8-10 times of the total mass of the added clove, the rhaponticum carthamoides and the ailanthus altissima.
7. A propolis compound for reducing three highs is characterized in that: the method for preparing the three-high-lowering propolis compound according to any one of claims 1 to 6.
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