CN101274884A - Process for extracting bacterial cell coenzyme Q10 - Google Patents
Process for extracting bacterial cell coenzyme Q10 Download PDFInfo
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- CN101274884A CN101274884A CNA2008101120170A CN200810112017A CN101274884A CN 101274884 A CN101274884 A CN 101274884A CN A2008101120170 A CNA2008101120170 A CN A2008101120170A CN 200810112017 A CN200810112017 A CN 200810112017A CN 101274884 A CN101274884 A CN 101274884A
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Abstract
The invention relates to a technology for extracting coenzyme Q10 in bacterial cells, which pertains to the technical field of microbiology engineering. Thalli is automatically and quantitatively put into from the dog-house of a continuous countercurrent device under the control of a weigh-instrument, a solvent is injected from a solvent inlet under the control of a flowmeter and the leaching solution and the thalli form reverse continuous countercurrent leaching process under the push of a shovel-like thruster; the concentration gradient is large, relative movement exists between the solvent and the thalli and the thalli moves from the left end to the right end of an extraction container continuously under the function of the shovel-like thruster while the solvent moves from the right end to the left end of the container under the action of pressure; a diffusion boundary layer is thin and fast to be updated and the coenzyme Q10 is extracted after 2 to 10 hours of reaction of the thalli which enters from the left end of the device after the contact of the solvent and the thalli; the thalli enters a rake type dryer from the right end of an extraction device by press treatment and residual organic solvent in the thalli is treated with drying treatment in the rake type dryer; the yield of the coenzyme Q10 reaches more than 90 percent.
Description
Technical field
The invention belongs to the microbial engineering field, particularly a kind of technology of extracting bacterial cell coenzyme Q 10.
Background technology
Coenzyme Q10 99.0 is a kind of chemical composition that extensively is present in the biological cell, has no side effect.It is the basis that the human body cell energy is made, and has the metabolic cardiotonic, definite effect.Coenzyme Q10 99.0 is mainly used in the treatment of acute and chronic hepatitis, acute severe hepatitis, cardiovascular disorder and hypertension there is extraordinary curative effect, it can also be used for the complex therapy of cancer, simultaneously in unique effects in aspect such as anti-ageing, antifatigue, fat-reducing and beauty treatments.
The method of producing the Coenzyme Q10 99.0 raw material mainly contains four kinds: biological extraction method, solanesol semi-synthesis method, chemical synthesis and microbe fermentation method, wherein microbe fermentation method is acknowledged as a kind of technical matters of tool advantage and potentiality.Microbe fermentation method prepares Coenzyme Q10 99.0 and realizes that suitability for industrialized production mainly contains three aspects and requires: the one, the bacterial classification of stable large-scale production high quality Coenzyme Q10 99.0 be arranged; The 2nd, the method for extracting Coenzyme Q10 99.0 in the cell be arranged efficiently, the 3rd, high precision is separated, process for purification.
Because the complicated component of microbial cells, when extracting the purpose product from microbial cells, in order to obtain highly purified purpose product, raw material generally at first needs to handle through extracting.Whether the correct utilization reasonable, technology of extraction process will directly influence the abundant extraction degree of raw material and the process for refining flow process of product.
Traditional technology is to be that the single-stage of extraction unit equipment leaches (backflows) technology with the multi-function extractor, and its technical process is: thalline → 1 time → extraction of extraction 2 times → ... n time → filtration of → extraction → concentrate.Single-stage (backflow) extract technology is taked disposable feeding intake.Put into a certain proportion of thalline and solvent in the extractor, extracted at a certain temperature 2-3 hour, separate for the first time and to add an amount of solvent again behind the extracting solution and extract one again to secondary.To be extracted finishing, isolating extracting solution pumps in the thickener and concentrates several times, enters next process.For extracting effective components from thalline on a large scale, there is following shortcoming in traditional method: just lose mass transfer force when (1), thalline and extracting solution reach concentration balance, need separation and Extraction liquid, add new solvent again and carry out the second time or extract length consuming time for the third time; (2), in batches extract and get over backward, extract concentration is low more, causes the concentration of the total concentration of extracting solution mixed solution far below the extracting solution first time, has strengthened the load of thickening equipment; (3), in batches extract and must carry out batch filtration and solvent reheat, cause extractor to be in invalid operational stage, extractor is wasted in many complementary operations, the volumetric efficiency of extractor is very low.
Summary of the invention
The object of the present invention is to provide a kind of technology of extracting bacterial cell coenzyme Q 10, this technology is compared with traditional multi-function extractor, has improved the extraction efficiency of purpose product; Disposable slagging-off, and the thalline residue made drying treatment, improved solvent recovering rate, not only saved production cost, and reduced the pollution of waste residue environment; Saved the production time.Extraction efficiency height not only, the rate of recovery height of lyase, and level of automation height save time, laborsaving.
The present invention is a continuous countercurrent technology, and processing step is as follows:
With dog-house under the control of weighing apparatus the automatic ration input of thalline from continuous countercurrent equipment, solvent is injected by solvent import control amount under the control of under meter, and under the angle of rake promotion of shovel, leach liquor and thalline form opposite continuous countercurrent leaching process; Concentration gradient is big, exist speed of relative movement motion, thalline continuous left end under the angle of rake effect of shovel to move between solvent, thalline to right-hand member from extraction vessel, solvent then under the effect of pressure constantly the right-hand member from container move to left end, diffusion boundary layer is thin and upgrade fast, when solvent with after thalline fully contacts, the thalline that the left end of slave unit enters extracts Coenzyme Q10 99.0 after reacting through 2-10 hour, thalline is handled through squeezing from the right-hand member that extracts equipment and is entered rake type dryer, in rake type dryer organic solvent remaining in the thalline is carried out drying treatment; The Coenzyme Q10 99.0 yield is more than 90%; The solvent of evaporation enters next step concentration technology through pipeline; Solvent after concentrating refills in the solvent tank by pipeline and recycles; Dried thalline residue is then by discharging in the rake type dryer; The mass ratio of described solvent and thalline is 2-12, and temperature of reaction is 20-100 ℃.
Extracting solvent can be sherwood oil, ethyl acetate, normal hexane, in a kind of or their mixture.
Can do interlayer in the outside of extraction vessel, oil bath, water-bath all can, temperature range 20-100 ℃.
When solvent with after thalline fully contacts, through 2-10 hour, through filtration treatment, flow into the solvent recuperation pipeline, and then enter next step enrichment process by the right-hand member of equipment.Solvent after concentrating can refill in the solvent tank by pipeline and recycle.
The left end of thalline slave unit after abundant extraction (2-10 hour), enters rake type dryer from the right-hand member that extracts equipment through the squeezing processing.In rake type dryer organic solvent remaining in the thalline is carried out drying treatment, the solvent of evaporation enters next step concentration technology through pipeline.Dried thalline residue is then by discharging in the rake type dryer.
3, processing parameter
1), extraction time
Because concentration gradient is big, there is the speed of relative movement motion between the solvent thalline, diffusion boundary layer is thin and it is fast to upgrade, yield is up to more than 90%, thereby also accelerated leaching velocity.Biomass with 60 tons of jars calculates, and the extraction time of a jar was controlled in 2-8 hour.Because this equipment can 24 hours continuous operation, have saved the time greatly.
2, fluid coefficient (quantity of solvent and the ratio that drops into biomass)
2-12 gets final product, and continuous countercurrent fluid coefficient amount is little, reduces investment outlay, and treatment capacity was little when back operation concentrated, and improves work efficiency, and is energy-conservation, also saves solvent (organic solvent) cost.
3, extraction temperature
20-100℃。Material and solvent stir middle heating in continuous adverse current, are heated evenly, and keep the thermo-sensitivity composition not to be destroyed, and viscous substance is difficult for leaching easily filtration.
4, extract solvent
The organic solvent that polarity is less: sherwood oil, ethyl acetate, normal hexane, in a kind of or their mixture.
Thalline of the present invention is: the thalline of bacterium comprises the thalline of photosynthetic bacterium and edaphic bacillus; Type of heating can be also oil bath of water-bath; Extracting solvent can be sherwood oil, ethyl acetate, normal hexane, in a kind of or their mixture.
Advantage and effect thereof
1), concentration gradient is big, has the speed of relative movement motion between solvent, thalline, diffusion boundary layer is thin and it is fast to upgrade, yield is up to more than 90%.
2), the fully-closed system, solvent recovering rate height, 95-99%.Not only saved solvent cost, and helped safety in production, greatly reduced the pollution of organic solvent simultaneously environment.
3), fluid coefficient (promptly adding quantity of solvent and the ratio that drops into the medicinal material amount) is little, 2-12 get final product, saves solvent (organic solvent), treatment capacity was little when back operation was concentrated, the raising work efficiency is energy-conservation, reduces cost.
4), extraction temperature is low, 20-100 ℃.Material and solvent stir middle heating in continuous adverse current, are heated evenly, and improve the dissolution efficiency of purpose product.
4), totally closed operation, finish automatically, easy to operate, indirect heating, all and material contact site are stainless steel, adopt demountable structure, but both on-line cleaning also can thoroughly be cleaned clean health, GMP compatible with the internal components shedder is outer.
5), the complete machine height is low, reduces investment outlay, and is convenient to operation.The relative multi-function extractor of the whole height of this unit is also much lower.This is because the tall and big tank body of multi-function extractor is high the setting to be put, and occupies tall and big factory building and production space, and this unit all takes into account support equipment, and clear height is below 3-5 rice, and this is very favourable to saving construction investment and operation.
6), automated operation, only need make an inspection tour getting final product.
Description of drawings
Fig. 1 is for realizing the continuous countercurrent equipment synoptic diagram of technology of the present invention, wherein, dog-house (with poidometer) 1, advance solvent mouth (with under meter) 2, slag-drip opening (with press apparatus) 3, solvent tank 4, shovel thruster 5, liquid outlet (with filtering net) 6, rake type dryer (with slag notch) 7, solvent recuperation pipeline 8.
Embodiment:
The present invention carries out in a cover closed system, and the operational scheme that enters in the system is:
Dry thalline is from dog-house (1) automatic ration input, and solvent is then injected by solvent inlet (2) control amount, and under the promotion of thruster (5), leach liquor and thalline form opposite continuous countercurrent leaching process.Effusive from liquid outlet (6) is the extracting solution that effective constituent is fully leached, from slag-drip opening (3) discharge is the bacterium slag that contains effective constituent hardly, then it is clean with solvent treatment to enter rake type dryer (7), enter concentrating unit by solvent recuperation pipeline (8) at last, by solvent collection pipeline (8) solvent is returned back in the container for storing liquid (4) again after the solvent recuperation, solvent but also free from environmental pollution had not only been saved in recycling.Complete assembly belongs to closed system, is applicable to volatile organic solvent fully, clean health, and reinforced and deslagging is all finished automatically, and is easy to operate.
Lifting specific examples is below again illustrated the inventive method.
Example 1
Processing parameter:
(1) thalline: photosynthetic bacterium or edaphic bacillus thalline, 80Kg.
(2) solvent: food normal hexane.
(3) fluid coefficient: 1: 3 (solid-to-liquid ratio)
(4) temperature: normal temperature.
(5) extraction time: 4 hours.
Extracting method: (1) Continuous Countercurrent Extraction scheme; (2) Multifunction tank extraction scheme
Extraction efficiency: (1) Continuous Countercurrent Extraction scheme: 90%; (2) Multifunction tank extraction scheme: 72%.
Attached:
Calculation Method as a result:
Standard method: get 1g thalline (or extract after dried bacterium slag), add the 100mL dehydrated alcohol, supersound extraction 1 hour is measured the content of its CoQ10.
Result: represent by the percentage that extracts
The CoQ10 content of (the CoQ10 content in the CoQ10 content-bacterium slag of thalline) * 100/ thalline
Example 2
Processing parameter:
(1) thalline: photosynthetic bacterium or edaphic bacillus thalline, 80Kg.
(2) solvent: food normal hexane.
(3) solid-to-liquid ratio: 1: 6.
(4) temperature: 40 ℃.
(5) extraction time: 4 hours.
Extracting method: (1) Continuous Countercurrent Extraction scheme; (2) Multifunction tank extraction scheme
Extraction efficiency: (1) Continuous Countercurrent Extraction scheme: 95%; (2) Multifunction tank extraction scheme: 80%.
Claims (6)
1, a kind of technology of extracting bacterial cell coenzyme Q 10, it is characterized in that, with dog-house under the control of weighing apparatus the automatic ration input of thalline from continuous countercurrent equipment, solvent is injected by solvent import control amount under the control of under meter, under the angle of rake promotion of shovel, leach liquor and thalline form opposite continuous countercurrent leaching process; Concentration gradient is big, exist speed of relative movement motion, thalline continuous left end under the angle of rake effect of shovel to move between solvent, thalline to right-hand member from extraction vessel, solvent then under the effect of pressure constantly the right-hand member from container move to left end, diffusion boundary layer is thin and upgrade fast, when solvent with after thalline fully contacts, the thalline that the left end of slave unit enters extracts Coenzyme Q10 99.0 after reacting through 2-10 hour, thalline is handled through squeezing from the right-hand member that extracts equipment and is entered rake type dryer, in rake type dryer organic solvent remaining in the thalline is carried out drying treatment; The Coenzyme Q10 99.0 yield is more than 90%; The solvent of evaporation enters next step concentration technology through pipeline; Solvent after concentrating refills in the solvent tank by pipeline and recycles; Dried thalline residue is then by discharging in the rake type dryer; The mass ratio of described solvent and thalline is 2-12, and temperature of reaction is 20-100 ℃.
According to the described technology of claim 1, it is characterized in that 2, described Coenzyme Q10 99.0 is present in the cell of bacterium.
According to the described technology of claim 1, it is characterized in that 3, described solvent is a kind of in sherwood oil, ethyl acetate, the normal hexane or their mixture.
According to the described technology of claim 1, it is characterized in that 4, described thalline is: the thalline of bacterium, the thalline of bacterium comprises the thalline of photosynthetic bacterium and edaphic bacillus.
5, according to the described technology of claim 1, it is characterized in that the input amount 10-10000kg of thalline.
According to the described technology of claim 1, it is characterized in that 6, the type of heating of realization response temperature is to do interlayer in the outside of extraction vessel, takes oil bath or heating in water bath.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810112017 CN101274884B (en) | 2008-05-20 | 2008-05-20 | Process for extracting bacterial cell coenzyme Q10 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810112017 CN101274884B (en) | 2008-05-20 | 2008-05-20 | Process for extracting bacterial cell coenzyme Q10 |
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| CN101274884A true CN101274884A (en) | 2008-10-01 |
| CN101274884B CN101274884B (en) | 2011-05-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200810112017 Expired - Fee Related CN101274884B (en) | 2008-05-20 | 2008-05-20 | Process for extracting bacterial cell coenzyme Q10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445815A (en) * | 2017-08-14 | 2017-12-08 | 内蒙古金达威药业有限公司 | A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2307616Y (en) * | 1997-05-04 | 1999-02-17 | 赵履祥 | Screw-type continuous counterflow extraction device |
| CN1267175C (en) * | 2004-03-17 | 2006-08-02 | 苏为科 | Equipment of continuous counter current extracting Chinese traditional medicine |
| US20070025976A1 (en) * | 2005-08-01 | 2007-02-01 | Cargill, Inc. | Process for the purification of coenzyme Q10 |
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- 2008-05-20 CN CN 200810112017 patent/CN101274884B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445815A (en) * | 2017-08-14 | 2017-12-08 | 内蒙古金达威药业有限公司 | A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 |
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| Publication number | Publication date |
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| CN101274884B (en) | 2011-05-04 |
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Address after: 100081 Zhongguancun South Street, Haidian District, Haidian District, Beijing Co-patentee after: China Academy of Space Technology Patentee after: Shenzhou Tianchen Technology Industry Co., Ltd. Address before: 100081 Zhongguancun South Street, Haidian District, Haidian District, Beijing Co-patentee before: China Academy of Space Technology Patentee before: Tianchen Shenzhou Industrial Co., Ltd. |
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Address after: 100081 Zhongguancun South Street, Haidian District, Haidian District, Beijing Co-patentee after: China Academy of Space Technology Patentee after: Biotechnology Group Co.,Ltd of space flight divine boat Address before: 100081 Zhongguancun South Street, Haidian District, Haidian District, Beijing Co-patentee before: China Academy of Space Technology Patentee before: Shenzhou Tianchen Technology Industry Co., Ltd. |
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Granted publication date: 20110504 Termination date: 20210520 |