CN106823453B - A kind of method of subcritical fluids fractional extraction propolis - Google Patents
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- 238000000605 extraction Methods 0.000 title claims abstract description 45
- 241000241413 Propolis Species 0.000 title claims abstract description 40
- 229940069949 propolis Drugs 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000012530 fluid Substances 0.000 title claims abstract description 14
- 239000000284 extract Substances 0.000 claims abstract description 42
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 238000001556 precipitation Methods 0.000 claims abstract description 16
- 239000003292 glue Substances 0.000 claims abstract description 15
- 235000013871 bee wax Nutrition 0.000 claims abstract description 9
- 239000012166 beeswax Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000002309 gasification Methods 0.000 claims abstract description 6
- 102000008186 Collagen Human genes 0.000 claims abstract description 5
- 108010035532 Collagen Proteins 0.000 claims abstract description 5
- 229920001436 collagen Polymers 0.000 claims abstract description 5
- 238000000935 solvent evaporation Methods 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- LVGUZGTVOIAKKC-UHFFFAOYSA-N 1,1,1,2-tetrafluoroethane Chemical compound FCC(F)(F)F LVGUZGTVOIAKKC-UHFFFAOYSA-N 0.000 claims description 6
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 239000001273 butane Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- 239000001294 propane Substances 0.000 claims description 3
- 229930003944 flavone Natural products 0.000 abstract description 10
- 235000011949 flavones Nutrition 0.000 abstract description 10
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 abstract description 10
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 abstract description 9
- RTIXKCRFFJGDFG-UHFFFAOYSA-N chrysin Chemical compound C=1C(O)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=CC=C1 RTIXKCRFFJGDFG-UHFFFAOYSA-N 0.000 abstract description 6
- 150000002212 flavone derivatives Chemical class 0.000 abstract description 6
- VCCRNZQBSJXYJD-UHFFFAOYSA-N galangin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=CC=C1 VCCRNZQBSJXYJD-UHFFFAOYSA-N 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 6
- NYCXYKOXLNBYID-UHFFFAOYSA-N 5,7-Dihydroxychromone Natural products O1C=CC(=O)C=2C1=CC(O)=CC=2O NYCXYKOXLNBYID-UHFFFAOYSA-N 0.000 abstract description 3
- 235000015838 chrysin Nutrition 0.000 abstract description 3
- 229940043370 chrysin Drugs 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 3
- CIPSYTVGZURWPT-UHFFFAOYSA-N galangin Natural products OC1=C(Oc2cc(O)c(O)cc2C1=O)c3ccccc3 CIPSYTVGZURWPT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- SUYJZKRQHBQNCA-UHFFFAOYSA-N pinobanksin Natural products O1C2=CC(O)=CC(O)=C2C(=O)C(O)C1C1=CC=CC=C1 SUYJZKRQHBQNCA-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000110 cooling liquid Substances 0.000 abstract 2
- 230000006378 damage Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 241000256844 Apis mellifera Species 0.000 description 5
- 229920000715 Mucilage Polymers 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- -1 flavone compound Chemical class 0.000 description 3
- 229930003935 flavonoid Natural products 0.000 description 3
- 150000002215 flavonoids Chemical class 0.000 description 3
- 235000017173 flavonoids Nutrition 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 210000004907 gland Anatomy 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000726221 Gemma Species 0.000 description 1
- 235000013421 Kaempferia galanga Nutrition 0.000 description 1
- 244000062241 Kaempferia galanga Species 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241000168036 Populus alba Species 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 150000005218 dimethyl ethers Chemical class 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229930003949 flavanone Natural products 0.000 description 1
- 235000011981 flavanones Nutrition 0.000 description 1
- 150000002208 flavanones Chemical class 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Natural products O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 1
- 150000002216 flavonol derivatives Chemical class 0.000 description 1
- 235000011957 flavonols Nutrition 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 150000003431 steroids Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of methods of subcritical fluids fractional extraction propolis, are extracted respectively to beeswax in hair glue and propolis, comprising: the freezing of hair glue and broken；Broken hair collagen material is fitted into bolting silk bag, is put into extractor, vacuumizes, the first extractant, extraction is added；Extract liquor, which moves into, carries out solvent evaporation in evaporator, the first extractant cooling liquid of gasification is placed in solvent tank；Evaporator negative pressure is de-, takes out extract, obtains beeswax；After extractor carries out desolventizing, the second extractant, extraction is added；Second extract liquor, which moves into, carries out solvent evaporation in evaporator, the second extractant cooling liquid of gasification is placed in solvent tank；Evaporator carries out negative pressure precipitation, obtains light refined propolis extract.This method extraction temperature is low, can reduce the destruction of active constituent, and simple process extracts at low cost, recovery rate height, general flavone content height, and Galangin and Chrysin extraction completely, are free of heavy metal, no solvent residue in propolis extract.
Description
Technical field
The invention belongs to technical field of natural product extraction, the side of specifically a kind of subcritical fluids fractional extraction propolis
Method.
Background technique
In recent years, propolis is a hot spot of bee product research and development, and broad-spectrum biological activity obtains in modern medicine
It is widely applied.
Propolis is that the resin that honeybee acquires from plant gemma or trunk is mixed into made of the secretion of palatine gland, wax gland thereon
Jelly plays the role of sterilizing corrosion-resistant for smearing, repairing, reinforce honeycomb.10000 be only capable of within honeybee 1 year adopting to 10 ~
The propolis of 12g or so is known as " purple gold ".Propolis has special aromatic odor, in yellowish-brown to dark brown, can enter
Medicine.Propolis ingredient is complicated, including flavones, acid, alcohol, phenol, aldehyde, ester, ethers and alkene, terpene, steroid and a variety of ammonia
Base acid, fatty acid, enzyme, vitamin, various trace elements etc., wherein main ingredient flavone compound accounts for about 10 ~ 35%.This
A little chromocor compounds include flavonoids, flavonols and Flavanones etc., wherein Chrysin category flavone compound, galangal
Element belongs to flavonoid drugs.According to the literature, flavone compound has various physiology and pharmacological action, can help people
Body prevents and treats a variety of diseases, and strengthen immunity makes the various function normalizations of body, enhancingization.
The traditional extraction process of propolis mainly has: water extraction, alcoholic extraction method, propylene glycol extraction method, macroporous resin adsorption
Method, supercritical carbon dioxide extraction method etc. contain a large amount of inert ingredient beeswax in extracted propolis, and in various degree
There are complex technical process, operating cost height, active constituents to extract incomplete, extract color is deep, content of beary metal is exceeded etc.
Problem.
Subcritical fluid extraction technology is a kind of liposoluble substance Efficient extraction method, is obtained in terms of vegetable fat extraction
It is widely applied, in recent years subcritical fluid extraction technology is expanding application field.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of subcritical fluids fractional extraction propolis, this method works
Skill is simple, extraction temperature is low, extraction is at low cost, and beeswax and propolis extract respectively, propolis recovery rate height, flavonoid content
High, Galangin and Chrysin extraction are complete, are free of heavy metal, no solvent residue.
For achieving the above object, the invention adopts the following technical scheme:
A kind of method of subcritical fluids fractional extraction propolis, comprising the following steps:
1) hair glue is pre-processed；
2) pretreated hair collagen material is fitted into bolting silk bag, tying, is put into the extraction of solvent pairs subcritical abstraction device
It takes in tank, vacuumizes, the first extractant of metering is added, extracted 3 times in 20 ~ 25 DEG C, 0.3 ~ 0.5MPa, extract 30 ~ 60 every time
Minute；
3) the first extract liquor, which moves into, carries out solvent evaporation in evaporator, the solvent of gasification is cold through compressor compresses, condenser
But it is placed in solvent tank, in case being recycled；
4) evaporator opened evaporator in -0.09MPa negative pressure precipitation 10 ~ 60 minutes after emptying, took out extract, obtained
Beeswax；
5) extractor through precipitation, vacuumize after, the second extractant of metering is added, in 30 ~ 55 DEG C, 0.6 ~ 0.9MPa extract
It 3 ~ 4 times, extracts 40 ~ 70 minutes every time；Second extract liquor moves into evaporator, and solvent obtains light color after evaporation, negative pressure precipitation
The solvent of refined propolis extract gasification compressed, cool down and be placed in solvent tank, in case being recycled.
General flavone content is measured (GB/T 24283-using common rutin standard curve method in propolis extract
2009)；
Further, described that pretreated process is carried out to hair glue are as follows: hair collagen material is placed in refrigerator-freezer and is freezed in -20 DEG C
48 hours, it is crushed to 0.1 ~ 2 millimeter of particle.
Further, 200 ~ 400 mesh of bolting silk bag model.
Further, the propolis content of the hair glue is 20 ~ 70%.
Further, first extractant and the second extractant are the liquid such as butane, propane, tetrafluoroethane, dimethyl ether
Change one of compressed gas.
Further, the first extractant volume and quality of material ratio are 3 ~ 10 ︰ 1(mL/g)；Second extractant volume
It is 2 ~ 10 ︰ 1(mL/g with quality of material ratio).
The method of subcritical fluids fractional extraction propolis of the invention has the advantages that and existing propolis extractive technique phase
Than that can be extracted for the hair glue of different propolis contents；Propolis extract has special fragrance, and of light color, recovery rate can
Reaching 99% or more, general flavone content is greater than 25% in extract, higher than traditional method for extracting propolis, and Galangin and white poplar
Completely, heavy metal is not detected in propolis extract, no solvent residue, and present invention process is simple, and extraction temperature is low, bee for element extraction
Active constituent conservation degree is good in glue, and extractant is recycled, and operating cost is low, reduces the extraction cost of propolis accordingly, mentions
The high quality of propolis extract.
Detailed description of the invention
Fig. 1 is the device figure that the method for subcritical fluids fractional extraction propolis of the invention uses.
Specific embodiment
With reference to the accompanying drawing, the method to a kind of subcritical fluids fractional extraction propolis proposed by the present invention and its work side
Method is described in detail.
Example one
Weigh a mao glue 1000g(content 40.7%), it is freezed under the conditions of being placed in -20 DEG C and is crushed within 48 hours 0.1 ~ 2 millimeter thick
Particle；Smashed hair mucilage binding is entered in the bolting silk bag of 300 mesh, tying is put into the extraction kettle of subcritical abstraction device, is taken out true
5200 mL liquefied butane gas are added in sky, extract 3 times in 23 DEG C, every time extraction 40 minutes；Extract liquor is moved into evaporator 2 and is carried out
Evaporation is recycled through compressor compresses, cooling be placed in solvent tank 4；By 2 precipitation of evaporator under -0.09MPa negative pressure
40 minutes, extract is taken out, beeswax 186g is obtained.2 precipitation of extractor vacuumizes, and 6100 mL liquefaction tetrafluoroethane is added, in 30
DEG C extraction 3 times, every time extraction 50 minutes；Extract liquor moves into evaporator 2, evaporation, negative pressure precipitation, obtains light refined propolis extraction
Object 218g is taken, general flavone content 26.8% is measured；Extractant tetrafluoroethane compressed, is cooled down and is placed on circulation in solvent tank 5 and makes
With.Calculate propolis extract total amount be 404g, total recovery rate 99.3%.
Example two
Weigh a mao glue 1000g(content 23.4%), it is freezed under the conditions of being placed in -20 DEG C and is crushed within 48 hours 0.1 ~ 2 millimeter thick
Particle；Smashed hair mucilage binding is entered in the bolting silk bag of 300 mesh, tying is put into the extraction kettle of subcritical abstraction device, is taken out true
3100 mL liquid propane gas are added in sky, extract 3 times in 20 DEG C, every time extraction 30 minutes；Extract liquor is moved into evaporator 2 and is carried out
Evaporation is recycled through compressor compresses, cooling be placed in solvent tank 4；By 2 precipitation of evaporator under -0.09MPa negative pressure
20 minutes, extract is taken out, beeswax 107g is obtained.2 precipitation of extractor vacuumizes, and 2100 mL liquefaction tetrafluoroethane is added, in 30
DEG C extraction 3 times, every time extraction 40 minutes；Extract liquor moves into evaporator 2, evaporation, negative pressure precipitation, obtains light refined propolis extraction
Object 125g is taken, general flavone content 25.8% is measured；Extractant tetrafluoroethane compressed, is cooled down and is placed on circulation in solvent tank 5 and makes
With.Calculate propolis extract total amount be 232g, total recovery rate 99.1%.
Example three
Weigh a mao glue 500g(content 68.8%), it is freezed under the conditions of being placed in -20 DEG C and is crushed within 48 hours 0.1 ~ 2 millimeter thick
Particle；Smashed hair mucilage binding is entered in the bolting silk bag of 300 mesh, tying is put into the extraction kettle of solvent pairs subcritical abstraction device
In, it vacuumizes, 5000 mL liquefied butane gas is added, extracted 3 times in 25 DEG C, every time extraction 60 minutes；Extract liquor moves into evaporator
It is evaporated in 2, is recycled through compressor compresses, cooling be placed in solvent tank 4；It will evaporation under -0.09MPa negative pressure
2 precipitation of tank 60 minutes takes out extract, obtains beeswax 157g.2 precipitation of extractor vacuumizes, and 4000 mL liquefied dimethyl ethers are added,
It is extracted 4 times in 55 DEG C, every time extraction 70 minutes；Extract liquor moves into evaporator 2, and evaporation, negative pressure precipitation obtain light purification bee
Glue extract 184g, measures general flavone content 26.3%；Extractant dimethyl ether compressed, is cooled down to be placed in solvent tank 5 and is recycled
It uses.Calculate propolis extract total amount be 341g, total recovery rate 99.1%.
Based on description of the preferred embodiment of the present invention, it should be apparent that the sheet being defined by the appended claims
Invention is not limited only to the specific detail that is illustrated in specification above, without departing from present inventive concept or range to this hair
Bright many obviously change equally possible reaches the purpose of the present invention.
Claims (3)
1. a kind of method of subcritical fluids fractional extraction propolis, which comprises the following steps:
Hair glue is pre-processed；
Pretreated hair collagen material is fitted into bolting silk bag, tying is put into the extractor of solvent pairs subcritical abstraction device,
It vacuumizes, the first extractant of metering is added, extract 3 times in 20~25 DEG C, 0.3~0.5MPa, extract 30~60 minutes every time；
First extract liquor moves into and carries out solvent evaporation in evaporator, and the solvent of gasification is through compressor compresses, the cooling postposition of condenser
In solvent tank, in case being recycled；
Evaporator opened evaporator in -0.09MPa negative pressure precipitation 10~60 minutes after emptying, take out extract, obtained beeswax；
Extractor through precipitation, vacuumize after, the second extractant of metering is added, in 30~55 DEG C, 0.6~0.9MPa extraction 3~4
It is secondary, it extracts 40~70 minutes every time；Second extract liquor moves into evaporator, and solvent obtains light color after evaporation, negative pressure precipitation
Refined propolis extract；The solvent of gasification compressed, is cooled down and is placed in solvent tank, in case being recycled；
It is described that pretreated process is carried out to hair glue are as follows: hair collagen material is placed in refrigerator-freezer and is freezed 48 hours in -20 DEG C, is crushed to
0.1-2 millimeters of particle；
First extractant and the second extractant are butane, propane, tetrafluoroethane, one in dimethyl ether liquefied compressed gas
Kind；
The first extractant volume and quality of material ratio are 3-10 ︰ 1mL/g；Second extractant volume and quality of material ratio are 2-
10 ︰ 1mL/g.
2. the method for subcritical fluids fractional extraction propolis according to claim 1, which is characterized in that the bolting silk pouch-type
Number be 200-400 mesh.
3. the method for subcritical fluids fractional extraction propolis according to claim 1, which is characterized in that the bee of the hair glue
Glue content is 20-70%.
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| CN111808673A (en) * | 2020-07-09 | 2020-10-23 | 江苏海宏制药有限公司 | Subcritical fluid extraction process of sea cucumber oil |
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| CN1389218A (en) * | 2002-07-12 | 2003-01-08 | 江苏大学 | Method for supercritical extraction and microwave-assisted extraction separation of effective components of propolis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1389218A (en) * | 2002-07-12 | 2003-01-08 | 江苏大学 | Method for supercritical extraction and microwave-assisted extraction separation of effective components of propolis |
Non-Patent Citations (1)
| Title |
|---|
| 蜂胶的亚临界流体萃取技术研究;史嘉辰等;《首届中国亚临界生物萃取技术发展论坛论文集》;20161231;第2页 |
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Application publication date: 20170613 Assignee: JIANGSU FENG-AO BIOLOGICAL TECHNOLOGY CO.,LTD. Assignor: JIANGSU HONGQI BIOTECHNOLOGY Co.,Ltd. Contract record no.: X2024980018021 Denomination of invention: A method of subcritical fluid stepwise extraction of propolis Granted publication date: 20190430 License type: Common License Record date: 20241011 |