CN102429140B - Supercritical CO2 fluid extraction method of propolis - Google Patents
Supercritical CO2 fluid extraction method of propolis Download PDFInfo
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- CN102429140B CN102429140B CN2011103309920A CN201110330992A CN102429140B CN 102429140 B CN102429140 B CN 102429140B CN 2011103309920 A CN2011103309920 A CN 2011103309920A CN 201110330992 A CN201110330992 A CN 201110330992A CN 102429140 B CN102429140 B CN 102429140B
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- 241000241413 Propolis Species 0.000 title claims abstract description 95
- 229940069949 propolis Drugs 0.000 title claims abstract description 95
- 238000000605 extraction Methods 0.000 title claims abstract description 70
- 239000012530 fluid Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 37
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 244000299461 Theobroma cacao Species 0.000 claims abstract description 13
- 235000009470 Theobroma cacao Nutrition 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000010298 pulverizing process Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 20
- 238000009792 diffusion process Methods 0.000 claims description 15
- 238000000746 purification Methods 0.000 claims description 15
- 238000005243 fluidization Methods 0.000 claims description 10
- 238000012546 transfer Methods 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 125000004122 cyclic group Chemical group 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 230000035699 permeability Effects 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 230000002906 microbiologic effect Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
- 230000000050 nutritive effect Effects 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- 229910052700 potassium Inorganic materials 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract 2
- AUNGANRZJHBGPY-UHFFFAOYSA-N D-Lyxoflavin Natural products OCC(O)C(O)C(O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-UHFFFAOYSA-N 0.000 abstract 1
- AUNGANRZJHBGPY-SCRDCRAPSA-N Riboflavin Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-SCRDCRAPSA-N 0.000 abstract 1
- 229930003471 Vitamin B2 Natural products 0.000 abstract 1
- 239000004480 active ingredient Substances 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000005453 pelletization Methods 0.000 abstract 1
- 229960002477 riboflavin Drugs 0.000 abstract 1
- 239000011716 vitamin B2 Substances 0.000 abstract 1
- 235000019164 vitamin B2 Nutrition 0.000 abstract 1
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- 230000000694 effects Effects 0.000 description 5
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- 235000013305 food Nutrition 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 206010012601 diabetes mellitus Diseases 0.000 description 3
- 241000256844 Apis mellifera Species 0.000 description 2
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- 238000009534 blood test Methods 0.000 description 1
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- 231100000957 no side effect Toxicity 0.000 description 1
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- Jellies, Jams, And Syrups (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention discloses a supercritical CO2 fluid extraction method of propolis. The method comprises the following steps of: dewaxing, quick-freezing and grinding propolis, pelletizing, putting pelletized propolis in a reaction kettle, starting supercritical CO2 extraction equipment for pressurizing and heating CO2 so that propolis is extracted with CO2 in a supercritical liquid state in an extraction tank; adding cocoa powder in extracted and purified propolis in different proportions in different seasons, wherein the purified propolis is blocky and then ground into power by a grinder; evenly stirring so that propolis keeps powdery. Cocoa powder which contains vitamin B2 and elements such as potassium, magnesium, calcium and ferrum is added for improving the nutritive value of propolis. The method is a green low-temperature pure physical separation method, and no entraining agent is used in the extraction process. Compared with the conventional ethanol method, the method disclosed by the invention has the advantages that no solvent residue is caused, thermally sensitive components and active ingredients of propolis are remained completely, the average propolis extraction yield is 30%, and the extraction time is shorten to be within 4 hours.
Description
Technical field
The present invention relates to a kind of supercritical CO
2the method of fluid extraction propolis.
Background technology
Propolis is the maximum a kind of living resources of active component in the edible natural drug of the mankind and food.As the health care resource of ideals of human being, the applicating history of existing more than 3,000 year.Propolis has collected the elite of animal and plant, is rich in more than 300 kind of active skull cap components, is the edible desirable health care resources of the mankind.Propolis mainly contains eight large effects: (1) resisting pathogenic microbes effect; (2) calm, anesthetic effect; (3) promote the tissue repair effect; (4) on the impact of impaired cardiovascular system; (5) protect the liver, liver protection effect; (6) antitumor action; (7) anti-oxidant, effect of scavenging radical; (8) other action of nervous system.
Especially at society, owing to being subject to environmental pollution, social competition and the bad cause influences such as eating habit, diseases of cardiovascular and cerebrovascular systems, diabetes have become the main killer who threatens human health.And propolis has good preventive and therapeutic action to these diseases, and have no side effect.
The scientific research personnel of honeybee research institute of the Chinese Academy of Agricultural Sciences and the long-term treatment observation discovery of relevant medical institutions, utilizing propolis treatment diabetes total effective rate is 94.7%, and can prevent generation and the development of diabetic syndrome.It is 88% left and right that the expert Ni Keluofu of the former Soviet Union treats hypertension, high fat of blood test total effective rate with propolis.1991, Ministry of Health of the People's Republic of China's Food Hygiene Surveillance check was carried out safety examination according to " toxicological evaluation of food safety procedure " to Beijing Propolis, has no the toxicity reflection.In June, 2002, the Ministry of Agriculture classified propolis as pollution-free food, and standard code is NY5136-2002.
But, due to the restriction that is subject to propolis output and extractive technique, the technical development of China's bee glue product is always slower.
At present, China's propolis product suitability for industrialized production is mainly to adopt the organic solvent lixiviate, the method extract the propolis composition be polar component, there is dissolvent residual in extraction product, lead tolerance is high, needs further processing to eat.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defect of prior art, and a kind of supercritical CO is provided
2the method of fluid extraction propolis, it is the separation method of a kind of green, low temperature, pure physics, do not use any agent of carrying in extraction process, with traditional Ethanol Method, compare, without any dissolvent residual, the intact preservation of thermal sensitivity composition and active component, propolis extracts average yield and reaches 30%, and extraction time shortened in 4 hours.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of supercritical CO
2the method of fluid extraction propolis, described method for propolis is dewaxed, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2extraction equipment, by CO
2pressurize, heat, it is extracted propolis in extractor with the supercritical liq state, add cocoa power after the propolis purification by liquid extraction.
Described method is for making propolis particle and CO
2fluidization, make propolis particle and CO
2between fluid, carry out mass transfer, conduct heat and make solid particle to be suspended in critical fluids, the diffusion process of fortification substance, make CO
2the bottom-up biofilm carrier that flows through of fluid, biofilm carrier is a kind of microbiologic population of very thin bonding, play a part to divide and cut apart cell, with the cell biomembrane that works be self-assembling formation along with the generation of propolis, make carrier layer be flow regime, thereby strengthen the same CO of biomembrane within the unit interval
2fluid contact area, abundant mass transfer, by particle and CO
2fluidisation diffusion between fluid, the cyclic process of dissolving, separating, make CO
2fluid is uniformly distributed in extraction kettle, improves CO
2fluid permeability and diffusion rate, thus CO strengthened
2carrying capacity, the propolis purification by liquid extraction adds the cocoa power of propolis gross mass 20%-30% afterwards.
Extracting pressure is that 20-36Mpa gets, and extraction temperature is 25-40 ℃; Extraction time is 3-4 hour; CO
2flow velocity 3-5Kg/Kgh, extraction procedure is the one-level extraction, the second-order separation; One-level knockout drum pressure is 4-9Mpa, and temperature is 25-40 ℃; The second-order separation tank is 2-6Mpa, and temperature is 15-25 ℃.
Stir pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20%-30% while pulverizing, propolis is block after purifying, and through pulverizer, pulverizes as powdery.
The CO that one-level is separated
2gas, after purification utensil, recycles.
Supercritical CO of the present invention
2the method of fluid extraction propolis, it is a kind of green, low temperature, the separation method of pure physics, do not use any agent of carrying in extraction process, with traditional Ethanol Method, compare, without any dissolvent residual, the intact preservation of thermal sensitivity composition and active component, propolis extracts average yield and reaches 30%, extraction time shortened in 4 hours, propolis is block after purifying, with in stainless steel pulverizing machine, stirring pulverizing, it is powdery, now in the propolis of purification by liquid extraction, add the cocoa power of 20%-30%, can make propolis not lump, easily caking is heated summer, so what add is many, make propolis keep powdery, cocoa power is containing Cobastab
2reach the elements such as potassium, magnesium, calcium, iron, improved the nutritive value of propolis.
The present invention can reject impurity effectively, the propolis product no solvent residue of extraction; Extract and save propolis Semi-polarity composition and nonpolarity element from damage to greatest extent; The propolis material composition of extraction is comparatively stable and complete.
Thereby advantage of the present invention has: a. adopts CO
2with the propolis granule fluid; B. technique is simple, and extraction time is short, and production cost is low; C. effectively reject impurity; D. no solvent residue; E. extract and save propolis Semi-polarity composition and nonpolarity element from damage to greatest extent; F. adopt the extraction of different operating pressure state multi-stage separation tank; G. the propolis material composition of extraction is comparatively stable and complete, and the propolis yield is high.
The specific embodiment
Embodiment 1
The invention provides a kind of supercritical CO
2the method of fluid extraction propolis, by propolis dewaxed, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2extraction equipment, by CO
2pressurize, heat, it is extracted propolis in extractor with the supercritical liq state.
Make propolis particle and CO
2fluidization, make propolis particle and CO
2between fluid, carry out mass transfer, conduct heat and make solid particle to be suspended in critical fluids, the diffusion process of fortification substance, make CO
2the bottom-up biofilm carrier that flows through of fluid, CO
2flow velocity 5Kg/Kgh, biofilm carrier is a kind of microbiologic population of very thin bonding, play a part to divide and cut apart cell, and the cell biomembrane that works is self-assembling formation along with the generation of propolis, make carrier layer be flow regime, thereby strengthen the same CO of biomembrane within the unit interval
2fluid contact area, abundant mass transfer, by particle and CO
2fluidisation diffusion between fluid, the cyclic process of dissolving, separating, make CO
2fluid is uniformly distributed in extraction kettle, improves CO
2fluid permeability and diffusion rate, thus CO strengthened
2carrying capacity.
Extracting pressure is that 20Mpa gets, and extraction temperature is 40 ℃; Extraction time is 3 hours; Extraction procedure is the one-level extraction, the second-order separation; One-level knockout drum pressure is 9Mpa, and temperature is 25 ℃; The second-order separation tank is 6Mpa, and temperature is 15 ℃.
Stir pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 30% while pulverizing summer, propolis is block after purifying, and through pulverizer, pulverizes as powdery.
The CO that one-level is separated
2gas, after purification utensil, recycles.
Embodiment 2
The invention provides a kind of supercritical CO
2the method of fluid extraction propolis, by propolis dewaxed, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2extraction equipment, by CO
2pressurize, heat, it is extracted propolis in extractor with the supercritical liq state.
Make propolis particle and CO
2fluidization, make propolis particle and CO
2between fluid, carry out mass transfer, conduct heat and make solid particle to be suspended in critical fluids, the diffusion process of fortification substance, make CO
2the bottom-up biofilm carrier that flows through of fluid, CO
2flow velocity 5Kg/Kgh, biofilm carrier is a kind of microbiologic population of very thin bonding, play a part to divide and cut apart cell, and the cell biomembrane that works is self-assembling formation along with the generation of propolis, make carrier layer be flow regime, thereby strengthen the same CO of biomembrane within the unit interval
2fluid contact area, abundant mass transfer, by particle and CO
2fluidisation diffusion between fluid, the cyclic process of dissolving, separating, make CO
2fluid is uniformly distributed in extraction kettle, improves CO
2fluid permeability and diffusion rate, thus CO strengthened
2carrying capacity.
Extracting pressure is that 36Mpa gets, and extraction temperature is 25 ℃; Extraction time is 4 hours; Extraction procedure is the one-level extraction, the second-order separation; One-level knockout drum pressure is 4Mpa, and temperature is 40 ℃; The second-order separation tank is 2Mpa, and temperature is 25 ℃.
Stir pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20% while pulverizing winter, propolis is block after purifying, and through pulverizer, pulverizes as powdery.
The CO that one-level is separated
2gas, after purification utensil, recycles.
Embodiment 3
The invention provides a kind of supercritical CO
2the method of fluid extraction propolis, by propolis dewaxed, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2extraction equipment, by CO
2pressurize, heat, it is extracted propolis in extractor with the supercritical liq state.
Make propolis particle and CO
2fluidization, make propolis particle and CO
2between fluid, carry out mass transfer, conduct heat and make solid particle to be suspended in critical fluids, the diffusion process of fortification substance, make CO
2the bottom-up biofilm carrier that flows through of fluid, CO
2flow velocity 3-5Kg/Kgh, make carrier layer be flow regime, thereby strengthen the same CO of biomembrane within the unit interval
2fluid contact area, abundant mass transfer, by particle and CO
2fluidisation diffusion between fluid, the cyclic process of dissolving, separating, make CO
2fluid is uniformly distributed in extraction kettle, improves CO
2fluid permeability and diffusion rate, thus CO strengthened
2carrying capacity.
Extracting pressure is that 30Mpa gets, and extraction temperature is 35 ℃; Extraction time is 3.5 hours; Extraction procedure is the one-level extraction, the second-order separation; One-level knockout drum pressure is 6Mpa, and temperature is 35 ℃; The second-order separation tank is 4Mpa, and temperature is 20 ℃.
Stir pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20% while pulverizing winter, propolis is block after purifying, and through pulverizer, pulverizes as powdery.
The CO that one-level is separated
2gas, after purification utensil, recycles.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of being amplified out thus or change are still among protection scope of the present invention.
Claims (5)
1. a supercritical CO
2the method of fluid extraction propolis is characterized in that: described method for propolis is dewaxed, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2extraction equipment, by CO
2pressurize, heat, it is extracted propolis in extractor with the supercritical liq state, add the cocoa power of propolis gross mass 20%-30% after the propolis purification by liquid extraction.
2. supercritical CO as claimed in claim 1
2the method of fluid extraction propolis is characterized in that: described method is for making propolis particle and CO
2fluidization, make propolis particle and CO
2between fluid, carry out mass transfer, conduct heat and make solid particle to be suspended in critical fluids, the diffusion process of fortification substance, make CO
2the bottom-up biofilm carrier that flows through of fluid, biofilm carrier is a kind of microbiologic population of very thin bonding, play a part to divide and cut apart cell, with the cell biomembrane that works be self-assembling formation along with the generation of propolis, make carrier layer be flow regime, thereby strengthen the same CO of biomembrane within the unit interval
2fluid contact area, abundant mass transfer, by particle and CO
2fluidisation diffusion between fluid, the cyclic process of dissolving, separating, make CO
2fluid is uniformly distributed in extraction kettle, improves CO
2fluid permeability and diffusion rate, thus CO strengthened
2carrying capacity, the propolis purification by liquid extraction adds the cocoa power of propolis gross mass 20%-30% afterwards.
3. supercritical CO as claimed in claim 2
2the method of fluid extraction propolis is characterized in that: extracting pressure is 20-36Mpa, and extraction temperature is 25-40 ℃; Extraction time is 3-4 hour; CO
2flow velocity 3-5Kg/Kg
.h, extraction procedure is the one-level extraction, the second-order separation; One-level knockout drum pressure is 4-9Mpa, and temperature is 25-40 ℃; The second-order separation tank is 2-6Mpa, and temperature is 15-25 ℃.
4. supercritical CO as claimed in claim 3
2the method of fluid extraction propolis is characterized in that: stir pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20%-30% while pulverizing, propolis is block after purifying, and through pulverizer, pulverizes as powdery.
5. supercritical CO as claimed in claim 4
2the method of fluid extraction propolis is characterized in that: the CO that one-level is separated
2gas, after purification utensil, recycles.
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| CN2011103309920A CN102429140B (en) | 2011-10-27 | 2011-10-27 | Supercritical CO2 fluid extraction method of propolis |
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| CN103549249A (en) * | 2013-10-11 | 2014-02-05 | 吕明 | Purification technology for propolis |
| CN104770629B (en) * | 2015-03-24 | 2018-02-09 | 南昌同心紫巢生物工程有限公司 | A kind of supercritical CO of high flavones content propolis2Extracting process |
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