CN106823453A - A kind of method of subcritical fluids fractional extraction propolis - Google Patents
A kind of method of subcritical fluids fractional extraction propolis Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 51
- 241000241413 Propolis Species 0.000 title claims abstract description 44
- 229940069949 propolis Drugs 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000012530 fluid Substances 0.000 title claims abstract description 17
- 239000000284 extract Substances 0.000 claims abstract description 37
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 238000001556 precipitation Methods 0.000 claims abstract description 15
- 239000003292 glue Substances 0.000 claims abstract description 14
- 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
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000000935 solvent evaporation Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 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
- 230000006835 compression Effects 0.000 claims description 5
- 238000007906 compression Methods 0.000 claims description 5
- LVGUZGTVOIAKKC-UHFFFAOYSA-N 1,1,1,2-tetrafluoroethane Chemical compound FCC(F)(F)F LVGUZGTVOIAKKC-UHFFFAOYSA-N 0.000 claims description 4
- 241000256844 Apis mellifera Species 0.000 claims description 4
- 239000001273 butane Substances 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
- 238000004064 recycling Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 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
- 238000007710 freezing Methods 0.000 abstract description 5
- 230000008014 freezing Effects 0.000 abstract description 5
- 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
- 229920000715 Mucilage Polymers 0.000 description 3
- 239000002253 acid Substances 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
- 230000008859 change Effects 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
- 241000256837 Apidae Species 0.000 description 1
- 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
- 230000009471 action Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 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
- 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
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 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
- 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
- 239000008187 granular material Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000002932 luster 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
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 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 method of subcritical fluids fractional extraction propolis, beeswax in hair glue and propolis are extracted respectively, including：The freezing of hair glue and broken；Broken hair collagen material is fitted into bolting silk bag, is put into extractor, vacuumized, add the first extractant, extraction；Extract carries out solvent evaporation in moving into evaporator, is placed in solvent tank after the first extractant cooling liquid of gasification；Evaporator negative pressure takes off, and takes out extract, obtains beeswax；After extractor carries out desolventizing, the second extractant, extraction are added；Second extract carries out solvent evaporation in moving into evaporator, is placed in solvent tank after the second extractant cooling liquid of gasification；Evaporator carries out negative pressure precipitation, obtains light refined propolis extract.The method extraction temperature is low, can reduce the destruction of active constituent, and process is simple extracts low cost, and recovery rate is high, and general flavone content is high, and Galangin and Chrysin extraction are complete, and heavy metal, no solvent residue are free of in propolis extract.
Description
Technical field
The invention belongs to technical field of natural product extraction, specifically a kind of side of subcritical fluids fractional extraction propolis
Method.
Background technology
In recent years, propolis is a focus of bee product research and development, and its broad-spectrum biological activity is obtained in modern medicine
Extensive use.
Propolis is the secretion that the resin that honeybee gathers from plant gemma or trunk is mixed into palatine gland, wax gland thereon
Jelly, for smearing, repairing, reinforce honeycomb, plays the effect of sterilizing corrosion-resistant.10000 honeybees are only capable of adopting to 10 for 1 year ~
The propolis of 12g or so, is described 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 various ammonia
Base acid, aliphatic acid, enzyme, vitamin, various trace elements etc., wherein Main Ingredients and Appearance flavone compound accounts for 10 ~ 35%.This
Including flavonoids, flavonols and Flavanones etc., wherein Chrysin belongs to flavone compound to a little chromocor compounds, galangal
Element category flavonoid drugs.According to the literature, flavone compound has many physiology and pharmacological action, can help people
Body prevents and treats various diseases, and strengthen immunity makes body various functions normalization, enhancingization.
The traditional extraction process of propolis mainly has：Water extraction, alcoholic extraction method, propane diols extraction method, macroporous resin adsorption
Method, supercritical carbon dioxide extraction method etc., contain substantial amounts of inert ingredient beeswax in the propolis for being extracted, and different degrees of
There is complex technical process, running cost are high, active constituent extraction is incomplete, extract color and luster 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
Extensive use, in recent years subcritical fluid extraction technology expand application field.
The content 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, the method work
Skill is simple, extraction temperature is low, extraction low cost, and beeswax and propolis are extracted respectively, and propolis recovery rate is high, flavonoid content
High, Galangin and Chrysin are extracted completely, without heavy metal, no solvent residue.
For achieving the above object, the present invention uses following technical scheme：
A kind of method of subcritical fluids fractional extraction propolis, comprises 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 extractor of solvent pairs subcritical abstraction device
In, vacuumize, the first extractant of metering is added, extracted 3 times in 20 ~ 25 DEG C, 0.3 ~ 0.5MPa, extract 30 ~ 60 minutes every time；
3）First extract carries out solvent evaporation in moving into evaporator, after the solvent of gasification is cooled down through compressor compression, condenser
It is placed in solvent tank, in case recycling；
4）Evaporator opened evaporator in -0.09MPa negative pressure precipitation 10 ~ 60 minutes after emptying, take out extract, obtained beeswax；
5）Extractor through precipitation, vacuumize after, add metering the second extractant, in 30 ~ 55 DEG C, 0.6 ~ 0.9MPa extraction 3 ~ 4
It is secondary, extract 40 ~ 70 minutes every time；Second extract is moved into evaporator, after solvent is through evaporation, negative pressure precipitation, obtains light color
Refined propolis extract gasification solvent it is compressed, cooling after be placed in solvent tank, in case recycle.
General flavone content is measured using common rutin standard curve method in propolis extract（GB/T 24283—
2009）；
Further, it is described to be to the process that hair glue is pre-processed：Hair collagen material is placed in refrigerator-freezer small in -20 DEG C of freezings 48
When, it is crushed to 0.1 ~ 2 millimeter of particle.
Further, the bolting silk bag mesh of model 200 ~ 400.
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, HFC-134a, dimethyl ether
Change the one kind in 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 with quality of material ratio（mL/g）.
The method of subcritical fluids fractional extraction propolis of the invention has the following advantages that：With existing propolis extractive technique phase
Than the hair glue that can be directed to different propolis contents is extracted；Propolis extract has special fragrance, and of light color, recovery rate can
More than 99% is reached, general flavone content is more than 25% in extract, higher than traditional method for extracting propolis, and Galangin and white poplar
Element extraction is complete, and heavy metal is not detected in propolis extract, no solvent residue, and present invention process is simple, and extraction temperature is low, honeybee
Active constituent conservation degree is good in glue, and extractant is recycled, and operating cost is low, and the extraction cost of propolis is reduced accordingly, carries
The quality of propolis extract high.
Brief description of the drawings
Fig. 1 is the installation drawing that uses of method of subcritical fluids fractional extraction propolis of the invention.
Specific embodiment
Below in conjunction with the accompanying drawings, 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 placed in thick that freezing under the conditions of -20 DEG C is crushed to 0.1 ~ 2 millimeter for 48 hours
Grain；Hair mucilage binding after crushing is entered in the bolting silk bag of 300 mesh, tying is put into the extraction kettle of subcritical abstraction device, take out true
Sky, adds 5200 mL liquefied butane gas, is extracted 3 times in 23 DEG C, every time extraction 40 minutes；Extract is carried out in moving into evaporator 2
Evaporation, is placed in solvent tank 4 after compressor compression, cooling and recycles；In under -0.09MPa negative pressure by the precipitation of evaporator 2
40 minutes, extract is taken out, obtain beeswax 186g.The precipitation of extractor 2, vacuumize, 6100 mL liquefaction HFC-134as are added, in 30
DEG C extraction 3 times, every time extraction 50 minutes；Extract is moved into evaporator 2, evaporation, negative pressure precipitation, obtains light refined propolis extraction
Thing 218g is taken, general flavone content 26.8% is measured；Extractant HFC-134a is compressed, be placed in circulation in solvent tank 5 after cooling makes
With.It is 404g, total recovery rate 99.3% to calculate propolis and extract total amount.
Example two
Weigh a mao glue 1000g（Content 23.4%）, it is placed in thick that freezing under the conditions of -20 DEG C is crushed to 0.1 ~ 2 millimeter for 48 hours
Grain；Hair mucilage binding after crushing is entered in the bolting silk bag of 300 mesh, tying is put into the extraction kettle of subcritical abstraction device, take out true
Sky, adds 3100 mL liquid propane gas, is extracted 3 times in 20 DEG C, every time extraction 30 minutes；Extract is carried out in moving into evaporator 2
Evaporation, is placed in solvent tank 4 after compressor compression, cooling and recycles；In under -0.09MPa negative pressure by the precipitation of evaporator 2
20 minutes, extract is taken out, obtain beeswax 107g.The precipitation of extractor 2, vacuumize, 2100 mL liquefaction HFC-134as are added, in 30
DEG C extraction 3 times, every time extraction 40 minutes；Extract is moved into evaporator 2, evaporation, negative pressure precipitation, obtains light refined propolis extraction
Thing 125g is taken, general flavone content 25.8% is measured；Extractant HFC-134a is compressed, be placed in circulation in solvent tank 5 after cooling makes
With.It is 232g, total recovery rate 99.1% to calculate propolis and extract total amount.
Example three
Weigh a mao glue 500g（Content 68.8%）, it is placed in the coarse granule that freezing under the conditions of -20 DEG C is crushed to 0.1 ~ 2 millimeter for 48 hours；
Hair mucilage binding after crushing is entered in the bolting silk bag of 300 mesh, tying is put into the extraction kettle of solvent pairs subcritical abstraction device, is taken out
Vacuum, adds 5000 mL liquefied butane gas, is extracted 3 times in 25 DEG C, every time extraction 60 minutes；Extract enters in moving into evaporator 2
Row evaporation, is placed in solvent tank 4 after compressor compression, cooling and recycles；In evaporator 2 is taken off under -0.09MPa negative pressure
Molten 60 minutes, extract is taken out, obtain beeswax 157g.The precipitation of extractor 2, vacuumize, 4000 mL liquefied dimethyl ethers are added, in 55
DEG C extraction 4 times, every time extraction 70 minutes；Extract is moved into evaporator 2, evaporation, negative pressure precipitation, obtains light refined propolis extraction
Thing 184g is taken, general flavone content 26.3% is measured；Extractant dimethyl ether is compressed, be placed in circulation in solvent tank 5 after cooling makes
With.It is 341g, total recovery rate 99.1% to calculate propolis and extract total amount.
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 scope to this hair
Bright many obviously change equally possible reaches the purpose of the present invention.
Claims (6)
1. a kind of method of subcritical fluids fractional extraction propolis, it is characterised in that comprise 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,
Vacuumize, add the first extractant of metering, extracted 3 times in 20 ~ 25 DEG C, 0.3 ~ 0.5MPa, extract 30 ~ 60 minutes every time；
First extract carries out solvent evaporation in moving into evaporator, and the solvent of gasification is rearmounted through compressor compression, condenser cooling
In solvent tank, in case recycling；
Evaporator opened evaporator in -0.09MPa negative pressure precipitation 10 ~ 60 minutes after emptying, take out extract, obtained beeswax；
Extractor through precipitation, vacuumize after, add metering the second extractant, in 30 ~ 55 DEG C, 0.6 ~ 0.9MPa extract 3 ~ 4 times,
Extract 40 ~ 70 minutes every time；Second extract is moved into evaporator, after solvent is through evaporation, negative pressure precipitation, obtains the refined of light color
Propolis extract；The solvent of gasification is compressed, be placed in solvent tank after cooling, in case recycling.
2. the method for subcritical fluids fractional extraction propolis according to claim 1, it is characterised in that described to enter to hair glue
Row pretreatment process be：Hair collagen material is placed in refrigerator-freezer and is freezed 48 hours in -20 DEG C, be crushed to 0.1 ~ 2 millimeter of particle.
3. the method for subcritical fluids fractional extraction propolis according to claim 1, it is characterised in that the bolting silk pouch-type
Number be 200 ~ 400 mesh.
4. the method for subcritical fluids fractional extraction propolis according to claim 1, it is characterised in that the honeybee of the hair glue
Glue content is 20 ~ 70%.
5. the method for subcritical fluids fractional extraction propolis according to claim 1, it is characterised in that first extraction
Agent and the second extractant are the one kind in the liquefied compressed gas such as butane, propane, HFC-134a, dimethyl ether.
6. the method for subcritical fluids fractional extraction propolis according to claim 1, it is characterised in that first extraction
Agent volume is 3 ~ 10 ︰ 1 with quality of material ratio（mL/g）；Second extractant volume is 2 ~ 10 ︰ 1 with quality of material ratio（mL/g）.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537177A (en) * | 2017-08-10 | 2018-01-05 | 镇江市高等专科学校 | A kind of method of subcritical fluids fractional extraction propolis |
| CN108531288A (en) * | 2018-06-06 | 2018-09-14 | 安阳工学院 | The technique of subcritical stage extraction Chinese prickly ash flavor components |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537177A (en) * | 2017-08-10 | 2018-01-05 | 镇江市高等专科学校 | A kind of method of subcritical fluids fractional extraction propolis |
| CN108531288A (en) * | 2018-06-06 | 2018-09-14 | 安阳工学院 | The technique of subcritical stage extraction Chinese prickly ash flavor components |
| CN108531288B (en) * | 2018-06-06 | 2022-04-12 | 安阳工学院 | Process for subcritical segmented extraction of pepper flavor components |
| 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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| CN106823453B (en) | 2019-04-30 |
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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 |