CN103610717A - Preparation and purification method for bee pollen and acanthopanax senticosus compound extract through supercritical CO2 extraction and organic solvent extraction - Google Patents
Preparation and purification method for bee pollen and acanthopanax senticosus compound extract through supercritical CO2 extraction and organic solvent extraction Download PDFInfo
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Abstract
The invention relates to a preparation and purification method for bee pollen and acanthopanax senticosus compound extract through supercritical CO2 extraction and organic solvent extraction, and aims to solve the problems of complex process and high cost of the traditional method for preparing bee pollen and acanthopanax senticosus compound extract. The method provided by the invention comprises the steps of firstly, supercritically extracting broken bee pollen and rootstocks of acanthopanax senticosus to obtain a product 1 and extracted residues; secondly, carrying out reflux extraction on the residues by using ethanol water to obtain a product 2, wherein the residues are extracted in the first step; thirdly, enabling the product 2 to pass through a macroporous resin column, and collecting ethanol eluent; fourthly, carrying out reduced pressure distillation on the ethanol eluent to recover ethanol, then, merging the product 1, and drying. The preparation and purification method is applied to the preparation field of drugs or health care products.
Description
Technical field
The present invention relates to a kind of employing supercritical CO
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
Background technology
Rich in proteins, fat, carbohydrate, vitamin and mineral in bee pollen.The description of using as far back as the existing many relevant pollens of Liang Qian Duo Nianqian， China.At < < Sheng Nong's herbal classic > >, just there is the record of Pollen Typhae (Pollen Typhae) and pine yellow (Pollen Pini), " cure mainly trusted subordinate, pathogen, diuresis, the congestion that disappears, take the physical strength profiting of making light of one's life by commiting suicide for a long time, prolong life "; Chinese Zhang Zhongjing is shown in < < gold plaque outline > >, once records application Pollen Typhae activating blood circulation to dissipate blood stasis; < < Tang materia medica > > records " Song Huangzhu avoid evil spirits poison, main profit cardiopulmonary, the hemostasis of dispeling the wind ": the Tang Dynasty Sun Si invites functions such as just having set forth Herba Menthae " pollen master avoid evil spirits poison, remove fatigue " in < < a thousand pieces of gold of writing, dietetic therapy > >; All herbal > > of Song < < records pollen can control " vim and vigour cardiac and abdominal pain, a blood fortune blood stasis ... it is vexed that blood is flutterred on top ".Nearly twenty or thirty is over year, the pollen scholar of countries in the world, physician all at the Study of Pollens that deepens continuously to the pharmacological action of health and curative effect.Pollen sums up and mainly contains the following aspects with research: cardiovascular system; Improve body's immunity; Slow down aging; Radioprotective; Suppress tumor; Digestive system; Prostatitis; Diabetes; Endocrine regulation; Treatment infertility etc.Radix Et Caulis Acanthopanacis Senticosi Acanthopanaxsenticosus (Rupr.etMaxim.) Harms is root, rhizome or the stem and leaf of studies on plants of Acanthopanax Miq. in Araliaceae Radix Et Caulis Acanthopanacis Senticosi, has another name called thorn bent stick, tiger shackles.Pungent, micro-hardship, temperature, returns spleen, kidney, heart channel.The effect that has replenishing QI to invigorate the spleen, tonifying the kidney for tranquilization, for deficiency of spleen-YANG and kidneyYANG, body void is weak, inappetence, soreness of waist and knee joint, insomnia and dreamful sleep.Modern pharmacological research proves, Radix Et Caulis Acanthopanacis Senticosi has the effect of resisting fatigue, anticancer, defying age, anti-inflammation, enhancing immunity, Cardiovarscular.
To pollen and the research of Radix Et Caulis Acanthopanacis Senticosi folk prescription, in long-term various tests, treatment is not too quick-acting and obvious with Nutrition, pollen and other Chinese herbal medicine compatibilities, and its effect is also not too obvious.After both compatibilities, act on quick-acting and remarkable.Experimental results show that pollen and the treatment of Radix Et Caulis Acanthopanacis Senticosi compatibility are quick-acting and remarkable with Nutrition, can strengthen the comprehensive absorption of mice to pollens nutrition composition, contribute to nucleic acid metabolism and the protein metabolism of body, to mice adrenal gland and sexual accessory gland etc., also have obvious promotion growth effect.
Adopt supercritical CO
2abstraction technique extracts existing correlational study report to bee pollen and Radix Et Caulis Acanthopanacis Senticosi.Yet, a lot of research just adopts above-mentioned single raw material to process, its goods effective ingredient is single, need to extract twice could be by both compatibilities, complex process, cost is higher, and the raffinate after extraction oil is not further extracted, cannot fully efficiently utilize the compositions such as polysaccharide abundant in raffinate, protein, carbohydrate, these useful components cannot be brought into play to larger effect again.
Summary of the invention
The object of the invention is, in order to solve existing method complex process and the high problem of cost of preparing bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, provides a kind of employing supercritical CO
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
A kind of employing supercritical CO of the present invention
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, carry out according to the following steps:
One, 1～2 part, Radix Et Caulis Acanthopanacis Senticosi rhizome getting 2～4 parts of broker wall bee pollens and drying and crushing by mass fraction, then adds in extraction kettle, then by liquid CO
2send into high-pressure pump, then by the CO after pressurization
2adding in extraction kettle, is 30～60 ℃ in temperature, under extracting pressure 25～40MPa condition, extracts 5～6 hours, and entrainer is that quality percentage composition is 60% ethanol, then carries out separation, obtains product 1 and stripped residue;
Two, to adding quality percentage composition in the stripped residue of step 1, be 60%～80% soak with ethanol 0.5h, then under the condition of 60～90 ℃ of temperature after reflux, extract, 1～2h, filter, collect to obtain filtrate 1, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 10～12 times of stripped residue quality; Then to adding quality percentage composition in filtrate 1, be 60%～80% ethanol, at 60～90 ℃ of temperature, after reflux, extract, 1～2h, filter, collect to obtain filtrate 2, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 8～10 times of filtrate 1 quality; Merging filtrate 1 and filtrate 2, reconcentration, is cooled to room temperature, obtains product 2;
Three, product 2 is crossed to macroporous resin column, loading flow velocity is 0.5 column volume per hour, with deionized water, with the flow velocity of 2～3 times of column volumes per hour, carry out eluting again, elution amount is 5 times of column volumes, discard water lotion, then the alcoholic solution that is 55%～85% by volumetric concentration is with the flow velocity eluting resin column of 2～2.5 column volumes per hour, and the elution amount of alcoholic solution is 5 times of column volumes, collects ethanol elution;
Four, ethanol elution is carried out after ethanol is reclaimed in distilling under reduced pressure merging product 1, dry, obtain bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, complete employing supercritical CO
2preparation and the purification of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
The present invention can be out by the extracts active ingredients of bee pollen and Radix Et Caulis Acanthopanacis Senticosi simultaneously, step is simple, saved cost, the present invention simultaneously adopts the method for supercritical extraction, ethanol water reflux, extract,, purification by macroporous resin, can fully obtain effective ingredient in bee pollen and Radix Et Caulis Acanthopanacis Senticosi, its product is rich in the compositions such as fatty acid, manyprickle acanthopanax general flavone, pollen total flavones, polysaccharide, and general flavone content can reach 55.2%, and yield can reach 3.88%.Resulting product active constituent content is high, impurity is few, comprehensive nutrition, can be used for the preparation of medicine or health promoting product.
The specific embodiment
The specific embodiment one: a kind of employing supercritical CO of present embodiment
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, carry out according to the following steps:
One, 1～2 part, Radix Et Caulis Acanthopanacis Senticosi rhizome getting 2～4 parts of broker wall bee pollens and drying and crushing by mass fraction, then adds in extraction kettle, then by liquid CO
2send into high-pressure pump, then by the CO after pressurization
2adding in extraction kettle, is 30～60 ℃ in temperature, under extracting pressure 25～40MPa condition, extracts 5～6 hours, and entrainer is that quality percentage composition is 60% ethanol, then carries out separation, obtains product 1 and stripped residue;
Two, to adding quality percentage composition in the stripped residue of step 1, be 60%～80% soak with ethanol 0.5h, then under the condition of 60～90 ℃ of temperature after reflux, extract, 1～2h, filter, collect to obtain filtrate 1, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 10～12 times of stripped residue quality; Then to adding quality percentage composition in filtrate 1, be 60%～80% ethanol, at 60～90 ℃ of temperature, after reflux, extract, 1～2h, filter, collect to obtain filtrate 2, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 8～10 times of filtrate 1 quality; Merging filtrate 1 and filtrate 2, reconcentration, is cooled to room temperature, obtains product 2;
Three, product 2 is crossed to macroporous resin column, loading flow velocity is 0.5 column volume per hour, with deionized water, with the flow velocity of 2～3 times of column volumes per hour, carry out eluting again, elution amount is 5 times of column volumes, discard water lotion, then the alcoholic solution that is 55%～85% by volumetric concentration is with the flow velocity eluting resin column of 2～2.5 column volumes per hour, and the elution amount of alcoholic solution is 5 times of column volumes, collects ethanol elution;
Four, ethanol elution is carried out after ethanol is reclaimed in distilling under reduced pressure merging product 1, dry, obtain bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, complete employing supercritical CO
2preparation and the purification of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
Present embodiment can be out by the extracts active ingredients of bee pollen and Radix Et Caulis Acanthopanacis Senticosi simultaneously, step is simple, saved cost, present embodiment adopts the method for supercritical extraction, ethanol water reflux, extract,, purification by macroporous resin simultaneously, can fully obtain effective ingredient in bee pollen and Radix Et Caulis Acanthopanacis Senticosi, its product is rich in the compositions such as fatty acid, manyprickle acanthopanax general flavone, pollen total flavones, polysaccharide, and general flavone content can reach 55.2%, and yield can reach 3.88%.Resulting product active constituent content is high, impurity is few, comprehensive nutrition, can be used for the preparation of medicine or health promoting product.
The specific embodiment two: that present embodiment is different from the specific embodiment one is the liquid CO described in step 1
2for food stage purity is more than 99% liquid CO
2.Other steps and parameter are identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from the specific embodiment one or two is that the separated condition described in step 1 is 35～45 ℃ of separated 1 temperature, pressure 12～16MPa, 15～35 ℃ of separated 2 temperature, pressure 8～10MPa.Other steps and parameter are identical with the specific embodiment one or two.
The specific embodiment four: that present embodiment is different from one of specific embodiment one to three is the CO after the pressurization described in step 1
2pressure be 20～30MPa, flow is 15～20kg/Hr.Other steps and parameter are identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to four is that the broker wall bee pollen described in step 1 is that sporoderm-broken rate is not less than 90% through physics or biological method broken wall treatment; Radix Et Caulis Acanthopanacis Senticosi rhizome, through pulverizing dried, is crossed 20～60 mesh sieves.Other steps and parameter are identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five is that concentrated described in step 2 is the clear paste that while wanting 80 ℃ of simmer down tos, relative density is 1.02～1.08.Other steps and parameter are identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different from one of specific embodiment one to six is to be dried described in step 4 as drying under reduced pressure or lyophilization.Other steps and parameter are identical with one of specific embodiment one to six.
By following verification experimental verification beneficial effect of the present invention:
Test 1, a kind of employing supercritical CO
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, carry out according to the following steps:
One, 1 part, Radix Et Caulis Acanthopanacis Senticosi rhizome getting 2 parts of broker wall bee pollens and drying and crushing by mass fraction, then adds in extraction kettle, then by liquid CO
2send into high-pressure pump, then by the CO after pressurization
2adding in extraction kettle, is 50 ℃ in temperature, extracts 6 hours under extracting pressure 40MPa condition, and entrainer is that quality percentage composition is 60% ethanol, then carries out separation, obtains product 1 and stripped residue;
Two, to adding quality percentage composition in the stripped residue of step 1, be 60%～80% soak with ethanol 0.5h, then under the condition of 60～90 ℃ of temperature after reflux, extract, 2h, filter, collect to obtain filtrate 1, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 12 times of stripped residue quality; Then to adding quality percentage composition in filtrate 1, be 60%～80% ethanol, at 60～90 ℃ of temperature, after reflux, extract, 1～2h, filter, collect to obtain filtrate 2, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 10 times of filtrate 1 quality; Merging filtrate 1 and filtrate 2, reconcentration, is cooled to room temperature, obtains product 2;
Three, product 2 is crossed to macroporous resin column, loading flow velocity is 0.5 column volume per hour, with deionized water, with the flow velocity of 2～3 times of column volumes per hour, carry out eluting again, elution amount is 5 times of column volumes, discard water lotion, then the alcoholic solution that is 55%～85% by volumetric concentration is with the flow velocity eluting resin column of 2～2.5 column volumes per hour, and the elution amount of alcoholic solution is 5 times of column volumes, collects ethanol elution;
Four, ethanol elution is carried out after ethanol is reclaimed in distilling under reduced pressure merging product 1, drying under reduced pressure, obtains bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, completes employing supercritical CO
2preparation and the purification of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
Separated condition described in this test procedure one is 40 ℃ of separated 1 temperature, pressure 16MPa, 30 ℃ of separated 2 temperature, pressure 10MPa; CO after pressurization
2pressure be 20～30MPa, flow is 15～20kg/Hr.Concentrated described in step 2 is the clear paste that while wanting 80 ℃ of simmer down tos, relative density is 1.02～1.08.
Bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract to this test preparation are 54.8% with its general flavone content of spectrophotometry, yield 3.67%.
Test 2, a kind of employing supercritical CO
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, carry out according to the following steps:
One, 1 part, Radix Et Caulis Acanthopanacis Senticosi rhizome getting 2 parts of broker wall bee pollens and drying and crushing by mass fraction, then adds in extraction kettle, then by liquid CO
2send into high-pressure pump, then by the CO after pressurization
2adding in extraction kettle, is 45 ℃ in temperature, extracts 6 hours under extracting pressure 35MPa condition, and entrainer is that quality percentage composition is 60% ethanol, then carries out separation, obtains product 1 and stripped residue;
Two, to adding quality percentage composition in the stripped residue of step 1, be 60%～80% soak with ethanol 0.5h, then under the condition of 60～90 ℃ of temperature after reflux, extract, 2h, filter, collect to obtain filtrate 1, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 12 times of stripped residue quality; Then to adding quality percentage composition in filtrate 1, be 60%～80% ethanol, at 60～90 ℃ of temperature, after reflux, extract, 1～2h, filter, collect to obtain filtrate 2, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 10 times of filtrate 1 quality; Merging filtrate 1 and filtrate 2, reconcentration, is cooled to room temperature, obtains product 2;
Three, product 2 is crossed to macroporous resin column, loading flow velocity is 0.5 column volume per hour, with deionized water, with the flow velocity of 2～3 times of column volumes per hour, carry out eluting again, elution amount is 5 times of column volumes, discard water lotion, then the alcoholic solution that is 55%～85% by volumetric concentration is with the flow velocity eluting resin column of 2～2.5 column volumes per hour, and the elution amount of alcoholic solution is 5 times of column volumes, collects ethanol elution;
Four, ethanol elution is carried out after ethanol is reclaimed in distilling under reduced pressure merging product 1, lyophilization, obtains bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, completes employing supercritical CO
2preparation and the purification of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
Separated condition described in this test procedure one is 35 ℃ of separated 1 temperature, pressure 15MPa, 25 ℃ of separated 2 temperature, pressure 10MPa; CO after pressurization
2pressure be 20～30MPa, flow is 15～20kg/Hr.Concentrated described in step 2 is the clear paste that while wanting 80 ℃ of simmer down tos, relative density is 1.02～1.08.
Bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract to this test preparation are 51.4% with its general flavone content of spectrophotometry, yield 3.83%.
Test 3, a kind of employing supercritical CO
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, carry out according to the following steps:
One, 1 part, Radix Et Caulis Acanthopanacis Senticosi rhizome getting 2 parts of broker wall bee pollens and drying and crushing by mass fraction, then adds in extraction kettle, then by liquid CO
2send into high-pressure pump, then by the CO after pressurization
2adding in extraction kettle, is 60 ℃ in temperature, extracts 6 hours under extracting pressure 40MPa condition, and entrainer is that quality percentage composition is 60% ethanol, then carries out separation, obtains product 1 and stripped residue;
Two, to adding quality percentage composition in the stripped residue of step 1, be 60%～80% soak with ethanol 0.5h, then under the condition of 60～90 ℃ of temperature after reflux, extract, 2h, filter, collect to obtain filtrate 1, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 12 times of stripped residue quality; Then to adding quality percentage composition in filtrate 1, be 60%～80% ethanol, at 60～90 ℃ of temperature, after reflux, extract, 1～2h, filter, collect to obtain filtrate 2, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 10 times of filtrate 1 quality; Merging filtrate 1 and filtrate 2, reconcentration, is cooled to room temperature, obtains product 2;
Three, product 2 is crossed to macroporous resin column, loading flow velocity is 0.5 column volume per hour, with deionized water, with the flow velocity of 2～3 times of column volumes per hour, carry out eluting again, elution amount is 5 times of column volumes, discard water lotion, then the alcoholic solution that is 55%～85% by volumetric concentration is with the flow velocity eluting resin column of 2～2.5 column volumes per hour, and the elution amount of alcoholic solution is 5 times of column volumes, collects ethanol elution;
Four, ethanol elution is carried out after ethanol is reclaimed in distilling under reduced pressure merging product 1, lyophilization, obtains bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, completes employing supercritical CO
2preparation and the purification of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
Separated condition described in this test procedure one is 40 ℃ of separated 1 temperature, pressure 12MPa, 35 ℃ of separated 2 temperature, pressure 8MPa; CO after pressurization
2pressure be 20～30MPa, flow is 15～20kg/Hr.Concentrated described in step 2 is the clear paste that while wanting 80 ℃ of simmer down tos, relative density is 1.02～1.08.
Bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract to this test preparation are 55.2% with its general flavone content of spectrophotometry, yield 3.88%.
Test 4, a kind of employing supercritical CO
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, carry out according to the following steps:
One, 1 part, Radix Et Caulis Acanthopanacis Senticosi rhizome getting 2 parts of broker wall bee pollens and drying and crushing by mass fraction, then adds in extraction kettle, then by liquid CO
2send into high-pressure pump, then by the CO after pressurization
2adding in extraction kettle, is 40 ℃ in temperature, extracts 6 hours under extracting pressure 45MPa condition, and entrainer is that quality percentage composition is 60% ethanol, then carries out separation, obtains product 1 and stripped residue;
Two, to adding quality percentage composition in the stripped residue of step 1, be 60%～80% soak with ethanol 0.5h, then under the condition of 60～90 ℃ of temperature after reflux, extract, 2h, filter, collect to obtain filtrate 1, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 12 times of stripped residue quality; Then to adding quality percentage composition in filtrate 1, be 60%～80% ethanol, at 60～90 ℃ of temperature, after reflux, extract, 1～2h, filter, collect to obtain filtrate 2, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 10 times of filtrate 1 quality; Merging filtrate 1 and filtrate 2, reconcentration, is cooled to room temperature, obtains product 2;
Three, product 2 is crossed to macroporous resin column, loading flow velocity is 0.5 column volume per hour, with deionized water, with the flow velocity of 2～3 times of column volumes per hour, carry out eluting again, elution amount is 5 times of column volumes, discard water lotion, then the alcoholic solution that is 55%～85% by volumetric concentration is with the flow velocity eluting resin column of 2～2.5 column volumes per hour, and the elution amount of alcoholic solution is 5 times of column volumes, collects ethanol elution;
Four, ethanol elution is carried out after ethanol is reclaimed in distilling under reduced pressure merging product 1, drying under reduced pressure, obtains bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, completes employing supercritical CO
2preparation and the purification of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
Separated condition described in this test procedure one is 35 ℃ of separated 1 temperature, pressure 14MPa, 25 ℃ of separated 2 temperature, pressure 9MPa; CO after pressurization
2pressure be 20～30MPa, flow is 15～20kg/Hr.Concentrated described in step 2 is the clear paste that while wanting 80 ℃ of simmer down tos, relative density is 1.02～1.08.
Bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract to this test preparation are 50.2% with its general flavone content of spectrophotometry, yield 3.14%.
Broker wall bee pollen in test 1～4 is that sporoderm-broken rate is not less than 90% through physics or biological method broken wall treatment; Radix Et Caulis Acanthopanacis Senticosi rhizome, through pulverizing dried, is crossed 20～60 mesh sieves; Liquid CO
2for food stage purity is more than 99% liquid CO
2.
Claims (7)
1. one kind adopts supercritical CO
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, is characterized in that adopting supercritical CO
2preparation and the purification process thereof of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract carry out according to the following steps:
One, 1～2 part, Radix Et Caulis Acanthopanacis Senticosi rhizome getting 2～4 parts of broker wall bee pollens and drying and crushing by mass fraction, then adds in extraction kettle, then by liquid CO
2send into high-pressure pump, then by the CO after pressurization
2adding in extraction kettle, is 30～60 ℃ in temperature, under extracting pressure 25～40MPa condition, extracts 5～6 hours, and entrainer is that quality percentage composition is 60% ethanol, then carries out separation, obtains product 1 and stripped residue;
Two, to adding quality percentage composition in the stripped residue of step 1, be 60%～80% soak with ethanol 0.5h, then under the condition of 60～90 ℃ of temperature after reflux, extract, 1～2h, filter, collect to obtain filtrate 1, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 10～12 times of stripped residue quality; Then to adding quality percentage composition in filtrate 1, be 60%～80% ethanol, at 60～90 ℃ of temperature, after reflux, extract, 1～2h, filter, collect to obtain filtrate 2, the addition of the ethanol that wherein quality percentage composition is 60%～80% is 8～10 times of filtrate 1 quality; Merging filtrate 1 and filtrate 2, reconcentration, is cooled to room temperature, obtains product 2;
Three, product 2 is crossed to macroporous resin column, loading flow velocity is 0.5 column volume per hour, with deionized water, with the flow velocity of 2～3 times of column volumes per hour, carry out eluting again, elution amount is 5 times of column volumes, discard water lotion, then the alcoholic solution that is 55%～85% by volumetric concentration is with the flow velocity eluting resin column of 2～2.5 column volumes per hour, and the elution amount of alcoholic solution is 5 times of column volumes, collects ethanol elution;
Four, ethanol elution is carried out after ethanol is reclaimed in distilling under reduced pressure merging product 1, dry, obtain bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, complete employing supercritical CO
2preparation and the purification of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract.
2. a kind of employing supercritical CO according to claim 1
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, is characterized in that the liquid CO described in step 1
2for food stage purity is more than 99% liquid CO
2.
3. a kind of employing supercritical CO according to claim 1
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, the separated condition described in step 1 that it is characterized in that is 35～45 ℃ of separated 1 temperature, pressure 12～16MPa, 15～35 ℃ of separated 2 temperature, pressure 8～10MPa.
4. a kind of employing supercritical CO according to claim 1
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, is characterized in that the CO after the pressurization described in step 1
2pressure be 20～30MPa, flow is 15～20kg/Hr.
5. a kind of employing supercritical CO according to claim 1
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, is characterized in that the broker wall bee pollen described in step 1 is that sporoderm-broken rate is not less than 90% through physics or biological method broken wall treatment; Radix Et Caulis Acanthopanacis Senticosi rhizome, through pulverizing dried, is crossed 20～60 mesh sieves.
6. a kind of employing supercritical CO according to claim 1
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, is characterized in that concentrated described in step 2 is the clear paste that while wanting 80 ℃ of simmer down tos, relative density is 1.02～1.08.
7. a kind of employing supercritical CO according to claim 1
2preparation and the purification process of extraction, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract, is characterized in that being dried as drying under reduced pressure or lyophilization described in step 4.
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| CN201310674040.XA CN103610717B (en) | 2013-12-11 | 2013-12-11 | A kind of preparation and purification process adopting SCF-CO 2, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract |
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|---|---|---|---|
| CN201310674040.XA CN103610717B (en) | 2013-12-11 | 2013-12-11 | A kind of preparation and purification process adopting SCF-CO 2, organic solvent extraction bee pollen and Radix Et Caulis Acanthopanacis Senticosi compound extract |
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| CN103610717B CN103610717B (en) | 2016-03-09 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108719904A (en) * | 2018-04-11 | 2018-11-02 | 湖南农业大学 | A kind of Bee Pollen and its processing method |
| CN109874960A (en) * | 2019-03-27 | 2019-06-14 | 山西农业大学 | A kind of preparation process of Bee Pollen pollen crystalline substance |
| CN110959830A (en) * | 2019-12-18 | 2020-04-07 | 宁波杰顺生物科技有限公司 | Bee product and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631217A (en) * | 2004-11-29 | 2005-06-29 | 沈道金 | Concentrated solution of acanthopanax root, royal jelly, pollen and honey and method for making it |
| CN101103805A (en) * | 2007-08-09 | 2008-01-16 | 山东师范大学 | Industrial producing method for extracting fatty compound from melissa pollen |
| CN101555433A (en) * | 2008-04-08 | 2009-10-14 | 中国科学院西北高原生物研究所 | Process for extracting canola plant bee pollen grease by supercritical CO* |
| CN102366621A (en) * | 2011-09-30 | 2012-03-07 | 多多药业有限公司 | Plant estrogenic effect of acanthopanax biochemical traditional Chinese medicine compound extract and its application |
| CN103040941A (en) * | 2012-12-18 | 2013-04-17 | 浙江工业大学 | Supercritical extraction pollen extractive as well as preparation and application thereof |
-
2013
- 2013-12-11 CN CN201310674040.XA patent/CN103610717B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631217A (en) * | 2004-11-29 | 2005-06-29 | 沈道金 | Concentrated solution of acanthopanax root, royal jelly, pollen and honey and method for making it |
| CN101103805A (en) * | 2007-08-09 | 2008-01-16 | 山东师范大学 | Industrial producing method for extracting fatty compound from melissa pollen |
| CN101555433A (en) * | 2008-04-08 | 2009-10-14 | 中国科学院西北高原生物研究所 | Process for extracting canola plant bee pollen grease by supercritical CO* |
| CN102366621A (en) * | 2011-09-30 | 2012-03-07 | 多多药业有限公司 | Plant estrogenic effect of acanthopanax biochemical traditional Chinese medicine compound extract and its application |
| CN103040941A (en) * | 2012-12-18 | 2013-04-17 | 浙江工业大学 | Supercritical extraction pollen extractive as well as preparation and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李幸阳等: "复方花粉制剂药效学试验报告", 《中国蜂业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108719904A (en) * | 2018-04-11 | 2018-11-02 | 湖南农业大学 | A kind of Bee Pollen and its processing method |
| CN109874960A (en) * | 2019-03-27 | 2019-06-14 | 山西农业大学 | A kind of preparation process of Bee Pollen pollen crystalline substance |
| CN109874960B (en) * | 2019-03-27 | 2022-01-11 | 山西农业大学 | Preparation process of bee pollen crystal |
| CN110959830A (en) * | 2019-12-18 | 2020-04-07 | 宁波杰顺生物科技有限公司 | Bee product and preparation method thereof |
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| CN103610717B (en) | 2016-03-09 |
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Effective date of registration: 20211210 Address after: 150000 room a307-169, building 20, innovation and entrepreneurship Plaza, science and technology innovation city, high tech Industrial Development Zone, Harbin, Heilongjiang Province (178 Xiuyue Street) Patentee after: Harbin Pharmaceutical Group traditional Chinese Medicine Co.,Ltd. Address before: 150078 No. 243 Airport Road, Daoli District, Heilongjiang, Harbin Patentee before: The Second Chinese Medicine Factory, Harbin Pharmaceutical Group Co.,Ltd. |
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