CN107445815A - A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 - Google Patents
A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 Download PDFInfo
- Publication number
- CN107445815A CN107445815A CN201710692406.4A CN201710692406A CN107445815A CN 107445815 A CN107445815 A CN 107445815A CN 201710692406 A CN201710692406 A CN 201710692406A CN 107445815 A CN107445815 A CN 107445815A
- Authority
- CN
- China
- Prior art keywords
- solvent
- extraction
- thalline
- continuous flow
- flow upstream
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/10—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention discloses a kind of method of continuous flow upstream ultrasonic extraction Co-Q10, thalline and Extraction solvent is entered into extraction cabin, the flowing of both opposite directions from the both ends charging aperture input of continuous flow upstream ultrasonic extractor respectively, while open ultrasonic oscillator and carry out assisted extraction；Extract solution is concentrated by evaporation, and purification obtains Co-Q10, recycling design；For thalline after extracted through slag-liquid separation, extract solution merges concentration with the extract solution that upper step obtains, and wet bacteria slag dries precipitation and obtains dry bacteria residue and recycling design；Caused gas is reclaimed by solvent tail gas recovery system in process, and condensation is recycled solvent, and all recovered solvents are squeezed into solvent tank again recycles.Extracting method of the present invention realizes continuous dynamic countercurrent ultrasonic extraction in shorter extraction tube, ensures gradient ratio, improves yield, reduces solvent load, and road filtering, separation, the output of concentration, energy-saving after mitigation, reduces production cost.
Description
Technical field
The invention belongs to Co-Q10 to extract field, and in particular to a kind of method of continuous flow upstream ultrasonic extraction Co-Q10.
Background technology
Co-Q10, English name Coenzyme Q10, abbreviation CoQ10.It is a kind of biostearin being widely distributed in human body
Material, the content highest particularly in heart.It is that existing unique active cell that has concurrently breathes and anti-freedom in the market
The natural nutriment of base oxidative function.It is a kind of very strong antioxidant that it, which is used alone or is used in combination with vitamin E,.As
A kind of metabolic activation agent, it is present in the mitochondrial inner membrane of cell, and is acted on via specific cell metabolism, it is celliferous dynamic to produce
Power.It is also the vitaminic nutriment of a species simultaneously, and after eating, energy active cell, which breathes, acceleration produces has high energy
The ATP of amount, strengthen myocardium metabolic function, improve heartbeat efficiency.It can suppress the peroxidating of mitochondria, protection biology
Membrane structure integrality, there is special humidification to immune.
At present, the main production process of Co-Q10 is extracted from microorganism, and traditional extracting method is usually by coenzyme
After Q10 filtering fermentation liquors, drying obtain thalline, it is put into multi-function extractor, repeatedly stirring extraction is carried out using organic solvent,
Extraction finishes, and merges extract solution, subsequent processing is entered after concentration.Traditional extraction process exist extract yield is low, solvent load is big,
The problems such as being unable to continuous production, deslagging difficulty.Chinese patent CN101274884B discloses coenzyme in a kind of extraction bacterial cell
Q10 technique：By thalline, from the dog-house of continuous flow upstream equipment, the automatic ration under the control of weighing apparatus is put into, and solvent is by solvent
Import control amount under the control of flowmeter is injected, and under the promotion of shovel propeller, leachate and thalline form opposite continuous
Counterflow leaching process；Relative velocity motion between solvent, thalline be present, thalline constantly holds in the presence of shovel propeller from extraction
The left end of device to right-hand member move, and solvent then under the effect of the pressure constantly from the right-hand member of container to left end move, when solvent with
After thalline fully contacts, thalline that the left end of slave unit enters extracts Co-Q10 after 2-10 hours react, and thalline is from carrying
The right-hand member of taking equipment enters rake type dryer by squeezing processing, and organic solvent remaining in thalline is entered in rake type dryer
Row drying process；Co-Q10 yield is more than 90%.Continuous flow upstream technology realizes serialization, improves production efficiency, reduces molten
Agent dosage.But in order to ensure that thalline and solvent meet certain extraction time in the state of continuous uninterrupted adverse current, just can not
What is avoided need to be made long by extraction tube, cause that equipment machine volume is bigger, outward appearance is heavy, floor space is bigger and once
Property investment it is big the defects of, hinder the application and popularization of dynamic countercurrent in practice.Chinese patent CN101381747B one kind from
The method that Co-Q10 is extracted in microorganism, is to mix the fermentates of 4g hydrogenlike silicon ions ATCC 17023 with 50mL acetone, 0
Ultrasonic, supersonic frequency 0.2-0.8, power 300-500W at DEG C, ultrasonic time 3min, ultrasonic number are 3 times, then from point
Co-Q10 is obtained in chaotropic.Chinese patent application file CN105061180A discloses a kind of carrying for Co-Q10 in fermentation thalli
Method is taken, by the microorganism for having Co-Q10 production capacity with dissolving good organic solvent to Co-Q10 by grinding solid-liquid ratio 1：
4~1：After 8 mixing, 3~7min is ground, organic solvent is evaporated, obtains Co-Q10 crude extract.Crude extract is suspended from again anhydrous
In ethanol, using radiated time as 1~5s, off time 5s, general power is 90~450 2.5~12.5min of ultrasonic disruption,
4000r/min centrifuges 30min, and supernatant is Co-Q10 extract solution.Ultrasound assisted extraction technique accelerates oozing in extraction process
Thoroughly, dissolve, spread, shorten extraction time, improve extraction yield, but if using pot type ultrasonic extraction device, first, extraction rule
Mould is small, and two are unable to serialization, simultaneously because without concentration difference, once also extracts not totally, also repeatedly to extract, can neither reduce
It solvent load, can not reduce labor intensity, and also have in the same old way the problems such as deslagging existing for traditional extraction tank, except the time
It is short, without other clear superiorities.
The content of the invention
Continuous dynamic countercurrent ultrasonic extraction is realized in shorter extraction tube object of the present invention is to provide a kind of, is protected
Gradient ratio is demonstrate,proved, yield is improved, reduces solvent load, road filtering, separation, the output of concentration, energy-saving after mitigation, reduces life
Cost is produced, suitable for the method for the continuous flow upstream ultrasonic extraction Co-Q10 of industrialized production.
In order to realize the object of the invention, the invention provides a kind of method of continuous flow upstream ultrasonic extraction Co-Q10, extraction
Step is as follows：
Thalline Co-Q10 extracts：Thalline is entered into extraction cabin from the dog-house input of continuous flow upstream ultrasonic extractor one end,
Extraction solvent is put into from the solvent charging aperture of the other end simultaneously, thalline slowly pushes away in the presence of propeller to slag notch direction
Enter, and Extraction solvent flows to the opposite direction that thalline moves, thalline and Extraction solvent input open ultrasonic wave while extracting cabin
Oscillator carries out assisted extraction；
Extract solution concentrates：Extract solution is discharged from continuous flow upstream ultrasonic extractor liquid outlet, the extract solution enters dynamic and followed
It is concentrated by evaporation in ring low-temperature evaporation inspissator, obtained extract solution concentrate is medicinal extract, and the medicinal extract is purified to obtain coenzyme
Q10, recycling design squeeze into solvent tank recycling again；
Bacterium solution separation bacteria residue is dried：Thalline after the discharge extraction of continuous flow upstream ultrasonic extractor slag-drip opening, then through slag liquid
The isolated extract solution of separator and wet bacteria slag, extract solution merge concentration, wet bacteria slag with the extract solution of extract solution concentration step
Enter back into bacteria residue drying machine precipitation is dried and obtain dry bacteria residue and recovered solvent；The recovered solvent is squeezed into again
Solvent tank recycles；
Solvent tail gas recovery condensation：Caused gas is reclaimed by solvent tail gas recovery system in process, then is condensed
Recovery obtains solvent, and it is squeezed into solvent tank recycling again；The solvent tail gas recovery system by collecting pipe with
Continuous flow upstream ultrasonic extractor, dynamic circulation low-temperature evaporation inspissator, dregs and liquor separation device are connected with each part of bacteria residue drying machine.
Further, in thalline Co-Q10 extraction step, the Extraction solvent is low polar solvent and highly polar solvent
The volume ratio that mixed liquor, wherein low polar solvent account for mixed liquor is more than 80%.
Further, the low polar solvent is the solvent of solvent polarity index≤0.2；Preferably, the low polarity
Solvent is the one or more in pentane, n-hexane, normal heptane, petroleum ether；
Optional, the highly polar solvent is the solvent of solvent polarity index >=4.0；Preferably, the highly polar solvent
For the one or more in ethyl acetate, acetone, butanone, ethanol.
Further, in thalline Co-Q10 extraction step, the thalline is in the extraction cabin of continuous flow upstream ultrasonic extractor
Residence time is 20~120min；It is preferred that 30~60min.
Further, the continuous flow upstream ultrasonic extractor is duct type continuous flow upstream ultrasonic extractor, the duct type
Continuous flow upstream ultrasonic extractor includes 4~10 section extraction tubes, wherein it is soak extraction pipe to have 1 to 4 section, has 3 to 9 sections to be carried for ultrasound
Take pipe.During normal continuous flow upstream ultrasonic extraction, soak extraction pipe just only serves the effect of immersion, and ultrasonic extraction pipe is
Play the effect of ultrasound；When closing ultrasonic extraction function, ultrasonic extraction pipe can also be as soak extraction pipe.
Further, in thalline Co-Q10 extraction step, the mass/volume ratio of the thalline and Extraction solvent is 1kg/
3L~1kg/8L；It is preferred that 1kg/4L~1kg/6L.
Further, the temperature of the extraction of the thalline Co-Q10 extraction step is 15~50 DEG C, preferably 25~35 DEG C；
Optional, it is 20~60kHz that the unlatching ultrasonic oscillator, which carries out frequency ultrasonic in assisted extraction step,.
Further, in extract solution concentration step, described dynamic circulation low-temperature evaporation inspissator is dropped using vacuum decompression
Low evaporating temperature, vacuum≤- 0.06MPa, evaporating temperature are 25~60 DEG C.
Further, in bacterium solution separation bacteria residue drying steps, the dregs and liquor separation device is single screw extrusion machine, twin-screw
One kind in extruder, horizontal screw centrifuge, continuous band vacuum filter；Optional, the bacteria residue drying machine is tray drying
One kind in machine, rake type drier, hollow blade dryer.
Further, in solvent tail gas recovery condensing steps, the solvent tail gas recovery system is paraffin tail gas recycle system
System.
Extracting temperature of the present invention can cause to extract too many impurity when being more than 50 DEG C, the extract yield when temperature is less than 15 DEG C
It is low.
The beneficial effects of the invention are as follows：
1st, solvent and thalline are continuously added at slave unit both ends respectively using continuous flow upstream ultrasonic extraction process, both adverse currents
Contact, while using accelerating medium particle movement, cavitation effect and the ultrasonic vibration homogenization of ultrasonic extraction, further strengthen
Leaching effect, concentration gradient remain at higher level, and so as to form larger mass transfer force, extract solution comes out i.e. reachable
To higher concentration, extraction time is shortened, improves the yield of product.
2nd, whole extraction process has high extraction efficiency, effective component extraction rate height compared with traditional extraction technique, goes out liquid
Coefficient (Extraction solvent of input and the ratio of thalline) is small, extraction rate is fast, the features such as significantly saving.
3rd, low polar solvent extract yield is relatively low, highly polar solvent extraction high income, but the extraction of highly polar solvent extraction
Liquid poor quality, impurity are more, content is low, are unfavorable for subsequent treatment.Extraction solvent of the present invention is from low polar solvent and highly polar molten
The mixed liquor of agent, under appropriate proportioning, it can be ensured that improve extract yield in the case of extract solution quality, overcome independent use
Low polar solvent extract yield is relatively low, individually uses the highly polar solvent extraction then inferior shortcoming of extract solution.
4th, the present invention uses continuous flow upstream ultrasonic extraction process whole process serialization sealing operation, and solvent tail gas is condensed
Recovery, Extraction solvent recycling, solvent-oil ratio is small, with the multi-functional extraction process of tradition compare have efficiently, save,
It is safe and environment-friendly to wait clear superiority.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is intended to be used to explain the present invention, and can not
It is interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, according to described by document in the art
Technology or condition or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, are to lead to
Cross the conventional products of acquisition purchased in market.
The specification of continuous flow upstream ultrasonic extractor is as follows used in embodiment：
Producer：Jining pair and ultrasonic device Co., Ltd.
Pattern：Single-stage duct type continuous flow upstream ultrasonic extractor.
Extract bore：400mm.
Extraction tube joint number：Totally 6 section, wherein：Ultrasonic extraction pipe 4 saves, and soak extraction pipe 2 saves.
Extraction tube overall length：About 15m.
Extraction tube volume：Total measurement (volume) about 1800L.
Ultrasonic power：32kw
Co-Q10 fermentation thalli used is as follows in embodiment：
The fermentation thalli of hydrogenlike silicon ion：Hydrogenlike silicon ion (CGMCC No.4497, CN 102154182B) is with grape
In culture medium based on sugar, yeast extract and monosodium glutamate, culture obtains zymotic fluid, and filtering fermentation liquor is removed into filtrate, filtered
Cake, obtain thalline after filter cake drying, Co-Q10 content 26.8mg/g in thalline.
The fermentation thalli of radioactivity rhizobium：Radioactivity rhizobium (ATCC4452, commercially available) are taken out with glucose, yeast
In culture medium based on extract and monosodium glutamate, culture obtains zymotic fluid, and filtering fermentation liquor is removed into filtrate, obtains filter cake, and filter cake dries
Obtain thalline after dry, Co-Q10 content 25.1mg/g in thalline.
Extract yield calculation formula：
Extract yield=(Co-Q10 content in medicinal extract weight × medicinal extract)/(Co-Q10 content in thalline weight × thalline)
× 100%
The Co-Q10 detection method of content of embodiment 1
Co-Q10 detection method of content in thalline, extract solution concentrate (medicinal extract)：
Co-Q10 in sample, through the anti-phase post separation of high performance liquid chromatography, its peak area is directly proportional to the content of Co-Q10.
Chromatographic condition
Chromatographic column：Hypersil ODS 4.6mm × 150mm, 5 μm, stainless steel column；
Detection wavelength：275nm；
Mobile phase：Absolute ethyl alcohol/absolute methanol=50/50；
Column temperature：35℃
Flow velocity：1mL/min；
Sample size：20μL.
Determination method：Precision weighs 0.05g reference substances (being accurate to 0.00002g), is placed in 50mL volumetric flasks, adds 30mL
Absolute ethyl alcohol, ultrasound make to be completely dissolved, and scale is settled to absolute ethyl alcohol after cooling；Precision draws 10.00mL, is placed in 50mL appearances
In measuring bottle, scale is settled to absolute ethyl alcohol, is shaken up, filtered with 0.45 μm of disposable organic system filtering head, discard primary filtrate, received
Collect subsequent filtrate, analyzed for high performance liquid chromatograph.
Separately materials (fermentation thalli takes 1g, and medicinal extract takes 0.05g, is accurate to 0.0002g), be placed in 100mL brown volumetric flasks
In, scale is settled to absolute ethyl alcohol, puts ultrasonic 2h in ultrasonic cleaner, ultrasound finishes taking-up, naturally cools to room temperature, shakes
It is even, filtered with 0.45 μm of syringe filter, discard primary filtrate, collect subsequent filtrate, analyzed for high performance liquid chromatograph.Mark is taken respectively
The quasi- μ L of solution and sample solution 20, analyzed for high performance liquid chromatograph.
As a result calculate：
In terms of W1, numerical value is represented Co-Q10 content with mg/g, is calculated as follows：
In formula：
The numerical value of m --- sample mass, unit are gram (g)；
Pi--- sample solution peak area value；
Vi--- the numerical value of sample solution sampling volume, unit are microlitre (μ L)；
V --- sample dilutes the numerical value of volume, and unit is milliliter (mL)；
ρi--- the numerical value of the mass concentration of standard liquid, unit are every milliliter of milligram (mg/mL)；
Vst --- the numerical value of standard liquid sampling volume, unit are microlitre (μ L)；
Pst --- the average value of standard liquid peak area.
The Co-Q10 of embodiment 2 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and the solvent charging aperture of Extraction solvent (n-hexane) from the other end is (close to slag tap
The side of mouth) put into by flowmeter with 800L/h charging rate, thalline is in the presence of spiral propeller to slag notch side
To being slowly advanced, and solvent flows to the opposite direction that thalline moves, and thalline fully contacts with solvent in this countercurrent movement, from
And the Co-Q10 in thalline is extracted.During Continuous Countercurrent Extraction, while open ultrasonic oscillator and carry out auxiliary and carry
Take, supersonic frequency 20KHZ, control 25 DEG C of Extracting temperature.Extract solution is discharged from continuous flow upstream ultrasonic extractor liquid outlet, is entered
It is concentrated by evaporation into dynamic circulation low-temperature evaporation inspissator, 25 DEG C, vacuum -0.09MPa of thickening temperature, obtains Co-Q10 leaching
Cream 58.2kg, Co-Q10 content 433mg/g in the medicinal extract of survey, extract yield 94.03%, medicinal extract enter into next production technology
Row purification obtains Co-Q10, and recycling design squeezes into solvent tank recycling again；Thalline after extracted surpasses from continuous flow upstream
Sound extractor slag-drip opening is discharged, and precipitation, which is dried, into tray drier after single screw extrusion machine separates obtains dry bacterium
Slag and reclaim obtain solvent, the solvent for reclaiming to obtain squeeze into again solvent tank recycling.
The Co-Q10 of embodiment 3 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (n-hexane of 5% ethyl acetate -95%) is from the molten of the other end
Matchmaker's charging aperture (close to the side of slag notch) is put into by flowmeter with 1000L/h charging rate, and thalline is in spiral propeller
In the presence of be slowly advanced to slag notch direction, and the opposite direction that solvent is moved to thalline flows, and thalline is with solvent this inverse
Fully contacted in stream motion, so as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open super
Acoustic wave transducer carries out assisted extraction, supersonic frequency 20KHZ, controls 35 DEG C of Extracting temperature.Extract solution carries from continuous flow upstream ultrasound
Take machine liquid outlet to discharge, enter in dynamic circulation low-temperature evaporation inspissator and be concentrated by evaporation, 35 DEG C of thickening temperature, vacuum-
0.085MPa, obtains Co-Q10 medicinal extract 60.8kg, Co-Q10 content 432mg/g in the medicinal extract of survey, extract yield 98.01%,
Medicinal extract is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；Through carrying
Thalline after taking is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, is entered after single screw extrusion machine separates into tray drier
The dry precipitation of row obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank circulation again to be made
With.
The Co-Q10 of embodiment 4 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (n-hexane of 10% acetone -90%) enters from the solvent of the other end
Material mouth (close to the side of slag notch) is put into by flowmeter with 1200L/h charging rate, work of the thalline in spiral propeller
It is slowly advanced with lower to slag notch direction, and solvent flows to the opposite direction that thalline moves, thalline is transported with solvent in this adverse current
Fully contacted in dynamic, so as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open ultrasonic wave
Oscillator carries out assisted extraction, supersonic frequency 20KHZ, controls 30 DEG C of Extracting temperature.Extract solution is from continuous flow upstream ultrasonic extractor
Liquid outlet is discharged, and is entered in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, 45 DEG C of thickening temperature, and vacuum-
0.075MPa, obtains Co-Q10 medicinal extract 61.0kg, Co-Q10 content 430mg/g in the medicinal extract of survey, extract yield 97.87%,
Medicinal extract is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；Through carrying
Thalline after taking is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, is entered after single screw extrusion machine separates into tray drier
The dry precipitation of row obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank circulation again to be made
With.
The Co-Q10 of embodiment 5 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (n-hexane of 15% ethanol -85%) enters from the solvent of the other end
Material mouth (close to the side of slag notch) is put into by flowmeter with 800L/h charging rate, effect of the thalline in spiral propeller
It is lower to be slowly advanced to slag notch direction, and solvent flows to the opposite direction that thalline moves, thalline is with solvent in this countercurrent movement
In fully contact, so that the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open ultrasonic wave and shake
Son carries out assisted extraction, supersonic frequency 40KHZ, controls 45 DEG C of Extracting temperature.Extract solution goes out from continuous flow upstream ultrasonic extractor
Liquid mouth is discharged, and is entered in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, 50 DEG C, vacuum -0.07MPa of thickening temperature,
Obtain Co-Q10 medicinal extract 61.1kg, Co-Q10 content 431mg/g in the medicinal extract of survey, extract yield 98.26%, under medicinal extract enters
One production technology is purified to obtain Co-Q10, and recycling design squeezes into solvent tank recycling again；Thalline after extracted
Discharged from continuous flow upstream ultrasonic extractor slag-drip opening, precipitation is dried into tray drier after single screw extrusion machine separates
Obtain dry bacteria residue and recovery obtains solvent, the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
The Co-Q10 of embodiment 6 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (ethyl acetate) is from the solvent charging aperture of the other end (close to going out
The side of cinder notch) put into by flowmeter with 1200L/h charging rate, thalline is in the presence of spiral propeller to slag notch
Direction is slowly advanced, and solvent flows to the opposite direction that thalline moves, and thalline fully contacts with solvent in this countercurrent movement,
So as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open ultrasonic oscillator and carry out auxiliary and carry
Take, supersonic frequency 40KHZ, control 25 DEG C of Extracting temperature.Extract solution is discharged from continuous flow upstream ultrasonic extractor liquid outlet, is entered
It is concentrated by evaporation into dynamic circulation low-temperature evaporation inspissator, 35 DEG C, vacuum -0.07MPa of thickening temperature, obtains Co-Q10 leaching
Cream 69.4kg, Co-Q10 content 385mg/g in the medicinal extract of survey, extract yield 99.70%, medicinal extract enter into next production technology
Row purification obtains Co-Q10, and recycling design squeezes into solvent tank recycling again；Thalline after extracted surpasses from continuous flow upstream
Sound extractor slag-drip opening is discharged, and precipitation, which is dried, into tray drier after single screw extrusion machine separates obtains dry bacterium
Slag and reclaim obtain solvent, the solvent for reclaiming to obtain squeeze into again solvent tank recycling.
The Co-Q10 of embodiment 7 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (petroleum ether of 20% acetone -80%) enters from the solvent of the other end
Material mouth (close to the side of slag notch) is put into by flowmeter with 600L/h charging rate, effect of the thalline in spiral propeller
It is lower to be slowly advanced to slag notch direction, and solvent flows to the opposite direction that thalline moves, thalline is with solvent in this countercurrent movement
In fully contact, so that the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open ultrasonic wave and shake
Son carries out assisted extraction, supersonic frequency 60KHZ, controls 50 DEG C of Extracting temperature.Extract solution goes out from continuous flow upstream ultrasonic extractor
Liquid mouth is discharged, and is entered in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, 60 DEG C, vacuum -0.06MPa of thickening temperature,
Obtain Co-Q10 medicinal extract 61.4kg, Co-Q10 content 428mg/g in the medicinal extract of survey, extract yield 98.06%, under medicinal extract enters
One production technology is purified to obtain Co-Q10, and recycling design squeezes into solvent tank recycling again；Thalline after extracted
Discharged from continuous flow upstream ultrasonic extractor slag-drip opening, precipitation is dried into tray drier after single screw extrusion machine separates
Obtain dry bacteria residue and recovery obtains solvent, the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
The Co-Q10 of embodiment 8 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (normal heptane of 10% ethyl acetate -90%) is from the molten of the other end
Matchmaker's charging aperture (close to the side of slag notch) is put into by flowmeter with 1600L/h charging rate, and thalline is in spiral propeller
In the presence of be slowly advanced to slag notch direction, and the opposite direction that solvent is moved to thalline flows, and thalline is with solvent this inverse
Fully contacted in stream motion, so as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open super
Acoustic wave transducer carries out assisted extraction, supersonic frequency 60KHZ, controls 15 DEG C of Extracting temperature.Extract solution carries from continuous flow upstream ultrasound
Take machine liquid outlet to discharge, enter in dynamic circulation low-temperature evaporation inspissator and be concentrated by evaporation, 55 DEG C of thickening temperature, vacuum-
0.065MPa, obtains Co-Q10 medicinal extract 60.6kg, Co-Q10 content 433mg/g in the medicinal extract of survey, extract yield 97.91%,
Medicinal extract is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；Through carrying
Thalline after taking is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, is entered after single screw extrusion machine separates into tray drier
The dry precipitation of row obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank circulation again to be made
With.
The Co-Q10 of embodiment 9 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, solvent charging aperture (close slag notch of the Extraction solvent (acetone) from the other end
Side) put into by flowmeter with 1200L/h charging rate, thalline is in the presence of spiral propeller to slag notch direction
It is slowly advanced, and solvent flows to the opposite direction that thalline moves, thalline fully contacts with solvent in this countercurrent movement, so as to
Co-Q10 in thalline is extracted.During Continuous Countercurrent Extraction, while open ultrasonic oscillator and carry out assisted extraction,
Supersonic frequency is 40KHZ, controls 25 DEG C of Extracting temperature.Extract solution is discharged from continuous flow upstream ultrasonic extractor liquid outlet, is entered
It is concentrated by evaporation in dynamic circulation low-temperature evaporation inspissator, 35 DEG C of thickening temperature, vacuum -0.07MPa, obtains Co-Q10 medicinal extract
70.5kg, Co-Q10 content 377mg/g in the medicinal extract of survey, extract yield 99.17%, medicinal extract are carried out into next production technology
Purification obtains Co-Q10, and recycling design squeezes into solvent tank recycling again；Thalline after extracted is ultrasonic from continuous flow upstream
Extractor slag-drip opening is discharged, and precipitation, which is dried, into tray drier after single screw extrusion machine separates obtains dry bacteria residue
And reclaim and obtain solvent, the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
The Co-Q10 of embodiment 10 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (n-hexane of 10% ethyl acetate -90%) is from the molten of the other end
Matchmaker's charging aperture (close to the side of slag notch) is put into by flowmeter with 800L/h charging rate, and thalline is in spiral propeller
It is slowly advanced under effect to slag notch direction, and solvent flows to the opposite direction that thalline moves, thalline is with solvent in this adverse current
Fully contacted in motion, so as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open ultrasound
Ripple oscillator carries out assisted extraction, supersonic frequency 20KHZ, controls 25 DEG C of Extracting temperature.Extract solution is from continuous flow upstream ultrasonic extraction
Machine liquid outlet is discharged, and is entered in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, 25 DEG C of thickening temperature, and vacuum-
0.09MPa, obtains Co-Q10 medicinal extract 61.0kg, Co-Q10 content 430mg/g in the medicinal extract of survey, extract yield 97.87%, leaching
Cream is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；It is extracted
Thalline afterwards is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, and tray drier is entered after single screw extrusion machine separates and is carried out
Dry precipitation obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
The Co-Q10 of embodiment 11 extracts
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (n-hexane of 10% ethyl acetate -90%) is from the molten of the other end
Matchmaker's charging aperture (close to the side of slag notch) is put into by flowmeter with 1200L/h charging rate, and thalline is in spiral propeller
In the presence of be slowly advanced to slag notch direction, and the opposite direction that solvent is moved to thalline flows, and thalline is with solvent this inverse
Fully contacted in stream motion, so as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open super
Acoustic wave transducer carries out assisted extraction, supersonic frequency 40KHZ, controls 25 DEG C of Extracting temperature.Extract solution carries from continuous flow upstream ultrasound
Take machine liquid outlet to discharge, enter in dynamic circulation low-temperature evaporation inspissator and be concentrated by evaporation, 35 DEG C of thickening temperature, vacuum-
0.07MPa, obtains Co-Q10 medicinal extract 61.3kg, Co-Q10 content 428mg/g in the medicinal extract of survey, extract yield 97.90%, leaching
Cream is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；It is extracted
Thalline afterwards is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, and tray drier is entered after single screw extrusion machine separates and is carried out
Dry precipitation obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
The Co-Q10 of embodiment 12 extracts
The fermentation thalli 1000kg of radioactivity rhizobium is taken, passes through spiral shell from the dog-house of continuous flow upstream ultrasonic extractor one end
Revolve drawing-in device to put into 200kg/h charging rate, Extraction solvent (n-hexane of 10% acetone -90%) is from the solvent of the other end
Charging aperture (close to the side of slag notch) is put into by flowmeter with 800L/h charging rate, work of the thalline in spiral propeller
It is slowly advanced with lower to slag notch direction, and solvent flows to the opposite direction that thalline moves, thalline is transported with solvent in this adverse current
Fully contacted in dynamic, so as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open ultrasonic wave
Oscillator carries out assisted extraction, supersonic frequency 20KHZ, controls 25 DEG C of Extracting temperature.Extract solution is from continuous flow upstream ultrasonic extractor
Liquid outlet is discharged, and is entered in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, 35 DEG C of thickening temperature, and vacuum-
0.07MPa, obtains Co-Q10 medicinal extract 56.1kg, Co-Q10 content 436mg/g in the medicinal extract of survey, extract yield 97.45%, leaching
Cream is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；It is extracted
Thalline afterwards is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, and tray drier is entered after single screw extrusion machine separates and is carried out
Dry precipitation obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
The Co-Q10 of embodiment 13 extracts
The fermentation thalli 1000kg of root radioactivity rhizobium is taken, is passed through from the dog-house of continuous flow upstream ultrasonic extractor one end
Spiral feeder apparatus is put into 200kg/h charging rate, and Extraction solvent (n-hexane of 10% acetone -90%) is from the molten of the other end
Matchmaker's charging aperture (close to the side of slag notch) is put into by flowmeter with 1200L/h charging rate, and thalline is in spiral propeller
In the presence of be slowly advanced to slag notch direction, and the opposite direction that solvent is moved to thalline flows, and thalline is with solvent this inverse
Fully contacted in stream motion, so as to which the Co-Q10 in thalline be extracted.During Continuous Countercurrent Extraction, while open super
Acoustic wave transducer carries out assisted extraction, supersonic frequency 40KHZ, controls 35 DEG C of Extracting temperature.Extract solution carries from continuous flow upstream ultrasound
Take machine liquid outlet to discharge, enter in dynamic circulation low-temperature evaporation inspissator and be concentrated by evaporation, 35 DEG C of thickening temperature, vacuum-
0.07MPa, obtains Co-Q10 medicinal extract 57.4kg, Co-Q10 content 428mg/g in the medicinal extract of survey, extract yield 97.88%, leaching
Cream is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；It is extracted
Thalline afterwards is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, and tray drier is entered after single screw extrusion machine separates and is carried out
Dry precipitation obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
Comparative example 1 (Continuous Countercurrent Extraction, but be not turned on ultrasonic wave added)
The fermentation thalli 1000kg of hydrogenlike silicon ion is taken, passes through spiral from the dog-house of continuous flow upstream ultrasonic extractor one end
Drawing-in device is put into 200kg/h charging rate, and Extraction solvent (n-hexane of 10% acetone -90%) enters from the solvent of the other end
Material mouth (close to the side of slag notch) is put into by flowmeter with 800L/h charging rate, effect of the thalline in spiral propeller
It is lower to be slowly advanced to slag notch direction, and solvent flows to the opposite direction that thalline moves, thalline is with solvent in this countercurrent movement
In fully contact, so that the Co-Q10 in thalline be extracted, control 25 DEG C of Extracting temperature.Extract solution is from countercurrent extraction machine
Liquid outlet is discharged, and is entered in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, 35 DEG C of thickening temperature, and vacuum-
0.07MPa, obtains Co-Q10 medicinal extract 52.9kg, Co-Q10 content 436mg/g in the medicinal extract of survey, extract yield 86.06%, leaching
Cream is purified to obtain Co-Q10 into next production technology, and recycling design squeezes into solvent tank recycling again；It is extracted
Thalline afterwards is discharged from continuous flow upstream ultrasonic extractor slag-drip opening, and tray drier is entered after single screw extrusion machine separates and is carried out
Dry precipitation obtains dry bacteria residue and recovery obtains solvent, and the solvent for reclaiming to obtain squeezes into solvent tank recycling again.
Comparative example 2 (uses multi-function extractor ultrasonic extraction 1 time)
Take the fermentation thalli 100kg of hydrogenlike silicon ion, put into multi-function extractor, add 400L Extraction solvents (10% the third
The n-hexane of ketone -90%), control 25 DEG C of Extracting temperature, ultrasonic agitation extraction 30min, supersonic frequency 20KHZ.Mistake after extraction terminates
Filter obtains extract solution, enters in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, 35 DEG C of thickening temperature, and vacuum-
0.07MPa, obtains Co-Q10 medicinal extract 4.45kg, Co-Q10 content 432mg/g in the medicinal extract of survey, extract yield 71.73%.
Comparative example 3 (uses multi-function extractor ultrasonic extraction 3 times)
The fermentation thalli 100kg of the fermentation thalli of hydrogenlike silicon ion is taken, puts into multi-function extractor, it is molten to add 400L extractions
Agent (n-hexane of 10% acetone -90%), control 25 DEG C of Extracting temperature, ultrasonic agitation extraction 30min, supersonic frequency 20kHZ.Extraction
Extract solution is filtrated to get after end, thalline adds Extraction solvent (n-hexane of 10% acetone -90%) and repeats extraction 2 times, merges 3
Secondary extract solution is entered in dynamic circulation low-temperature evaporation inspissator and is concentrated by evaporation, and 35 DEG C of thickening temperature, vacuum -0.07MPa, is obtained
To Co-Q10 medicinal extract 6.15kg, Co-Q10 content 425mg/g in the medicinal extract of survey, extract yield 97.53%.
1 different extracting modes of table and its extraction result table
It can be obtained by table 1：
Embodiment 2-11 uses the technical scheme of continuous flow upstream ultrasonic extraction, and it is continuously inverse that extract yield is better than comparative example 1-2
Extraction method or Multifunction tank ultrasonic extraction are flowed, although comparative example 3 is reachable using the technical scheme of Multifunction tank ultrasonic extraction 3 times
To 97.53% extract yield, but it need to be extracted 3 times, and solvent-oil ratio is big, with duration, and the labor intensity of intermittently operated is big；
Embodiment 2 uses the technical scheme of low polarity single solvent system continuous flow upstream ultrasonic extraction, with the shape of embodiment 10
In contrast with, the extract yield of embodiment 10 is substantially better than embodiment 2, illustrates to be favorably improved coenzyme using mixed solvent system
Q10 extract yield；
Embodiment 6 and 9 uses the technical scheme of highly polar single solvent system continuous flow upstream ultrasonic extraction, with embodiment 11
It is contrasted, the content of Co-Q10 illustrates using mixing apparently higher than embodiment 6 and embodiment 9 in the gained medicinal extract of embodiment 11
Dicyandiamide solution is favorably improved the extract solution quality of Co-Q10.
In summary, technical solution of the present invention has high extraction efficiency, effective component extraction rate height, goes out the small (throwing of liquid coefficient
The Extraction solvent and the ratio of thalline entered) the advantages of.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art is not departing from the principle and objective of the present invention
In the case of above-described embodiment can be changed within the scope of the invention, change, replace and modification.
Claims (10)
- A kind of 1. method of continuous flow upstream ultrasonic extraction Co-Q10, it is characterised in that extraction step is as follows：Thalline Co-Q10 extracts：Thalline is entered into extraction cabin from the dog-house input of continuous flow upstream ultrasonic extractor one end, simultaneously Extraction solvent is put into from the solvent charging aperture of the other end, thalline is slowly advanced in the presence of propeller to slag notch direction, And Extraction solvent flows to the opposite direction that thalline moves, thalline and Extraction solvent input open ultrasonic oscillator while extracting cabin Carry out assisted extraction；Extract solution concentrates：Extract solution is discharged from continuous flow upstream ultrasonic extractor liquid outlet, it is low that the extract solution enters dynamic circulation It is concentrated by evaporation in warm evaporation concentrator, obtained extract solution concentrate is medicinal extract, and the medicinal extract is purified to obtain Co-Q10, Recycling design squeezes into solvent tank recycling again；Bacterium solution separation bacteria residue is dried：Thalline after the discharge extraction of continuous flow upstream ultrasonic extractor slag-drip opening, then through slag-liquid separation The isolated extract solution of device and wet bacteria slag, extract solution merge concentration with the extract solution of extract solution concentration step, and wet bacteria slag enters again Enter bacteria residue drying machine precipitation be dried to obtain dry bacteria residue and recovered solvent；The recovered solvent squeezes into solvent again Storage tank recycles；Solvent tail gas recovery condensation：Caused gas is reclaimed by solvent tail gas recovery system in process, then condenses recovery Solvent is obtained, it is squeezed into solvent tank recycling again；The solvent tail gas recovery system is by collecting pipe and continuously Reverse-flow ultrasonic extracting machine, dynamic circulation low-temperature evaporation inspissator, dregs and liquor separation device are connected with each part of bacteria residue drying machine.
- 2. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that thalline Co-Q10 carries Take in step, the Extraction solvent is the mixed liquor of low polar solvent and highly polar solvent, and wherein low polar solvent accounts for mixed liquor Volume ratio be more than 80%.
- 3. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 2, it is characterised in that the low polarity is molten Agent is the solvent of solvent polarity index≤0.2；Preferably, the low polar solvent is pentane, n-hexane, normal heptane, petroleum ether In one or more；Optional, the highly polar solvent is the solvent of solvent polarity index >=4.0；Preferably, the highly polar solvent is second One or more in acetoacetic ester, acetone, butanone, ethanol.
- 4. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that thalline Co-Q10 carries Take in step, thalline residence time in the extraction cabin of continuous flow upstream ultrasonic extractor is 20~120min；It is preferred that 30 ~60min.
- 5. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that the continuous flow upstream Ultrasonic extractor is duct type continuous flow upstream ultrasonic extractor, and the duct type continuous flow upstream ultrasonic extractor includes 4~10 sections Extraction tube, wherein it is soak extraction pipe to have 1 to 4 section, it is ultrasonic extraction pipe to have 3 to 9 sections.
- 6. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that thalline Co-Q10 carries Take in step, the mass/volume ratio of the thalline and Extraction solvent is 1kg/3L~1kg/8L；It is preferred that 1kg/4L~1kg/6L.
- 7. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that the thalline coenzyme The temperature of the extraction of Q10 extraction steps is 15~50 DEG C；It is preferred that 25~35 DEG C；Optional, it is 20~60kHz that the unlatching ultrasonic oscillator, which carries out frequency ultrasonic in assisted extraction step,.
- 8. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that extract solution concentration step In rapid, described dynamic circulation low-temperature evaporation inspissator reduces evaporating temperature using vacuum decompression, vacuum≤- 0.06MPa, steams It is 25~60 DEG C to send out temperature.
- 9. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that bacterium solution separates bacteria residue In drying steps, the dregs and liquor separation device is that single screw extrusion machine, double screw extruder, horizontal screw centrifuge, continuous band are true One kind in empty filter；Optional, the bacteria residue drying machine is tray drier, rake type drier, hollow blade dryer In one kind.
- 10. the method for continuous flow upstream ultrasonic extraction Co-Q10 according to claim 1, it is characterised in that solvent tail gas reclaims In condensing steps, the solvent tail gas recovery system is paraffin exhaust gas recovery system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710692406.4A CN107445815A (en) | 2017-08-14 | 2017-08-14 | A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710692406.4A CN107445815A (en) | 2017-08-14 | 2017-08-14 | A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107445815A true CN107445815A (en) | 2017-12-08 |
Family
ID=60491113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710692406.4A Pending CN107445815A (en) | 2017-08-14 | 2017-08-14 | A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107445815A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400458A (en) * | 2018-11-30 | 2019-03-01 | 内蒙古金达威药业有限公司 | A method of the separation and Extraction Co-Q10 from microbial fermentation solution |
| CN112755589A (en) * | 2021-02-23 | 2021-05-07 | 山东泰和水处理科技股份有限公司 | Extraction method and device of refined coenzyme Q10 |
| CN113069492A (en) * | 2021-05-07 | 2021-07-06 | 广州市润研基因科技有限公司 | Production technology for ultrasonic-assisted continuous countercurrent extraction of sapindus saponin |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274884A (en) * | 2008-05-20 | 2008-10-01 | 天辰神舟实业有限公司 | Process for extracting bacterial cell coenzyme Q10 |
| CN101381747A (en) * | 2008-10-28 | 2009-03-11 | 中国人民解放军军事医学科学院野战输血研究所 | Method for extracting coenzyme Q10 from microorganism |
| CN102058999A (en) * | 2010-12-08 | 2011-05-18 | 黑龙江省计算中心 | Multistage combinational continuous countercurrent ultrasonic extraction device |
| CN103520949A (en) * | 2013-10-15 | 2014-01-22 | 四川省砚山中药饮片有限公司 | Complete equipment for continuous counter-current ultrasonic extraction |
| CN104591993A (en) * | 2014-12-30 | 2015-05-06 | 内蒙古金达威药业有限公司 | Method for extracting coenzyme Q10 from fermentation mycelia |
| CN105061180A (en) * | 2015-08-31 | 2015-11-18 | 苏州科技学院 | Method for extracting coenzyme Q10 in fermentation biomass |
-
2017
- 2017-08-14 CN CN201710692406.4A patent/CN107445815A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274884A (en) * | 2008-05-20 | 2008-10-01 | 天辰神舟实业有限公司 | Process for extracting bacterial cell coenzyme Q10 |
| CN101381747A (en) * | 2008-10-28 | 2009-03-11 | 中国人民解放军军事医学科学院野战输血研究所 | Method for extracting coenzyme Q10 from microorganism |
| CN102058999A (en) * | 2010-12-08 | 2011-05-18 | 黑龙江省计算中心 | Multistage combinational continuous countercurrent ultrasonic extraction device |
| CN103520949A (en) * | 2013-10-15 | 2014-01-22 | 四川省砚山中药饮片有限公司 | Complete equipment for continuous counter-current ultrasonic extraction |
| CN104591993A (en) * | 2014-12-30 | 2015-05-06 | 内蒙古金达威药业有限公司 | Method for extracting coenzyme Q10 from fermentation mycelia |
| CN105061180A (en) * | 2015-08-31 | 2015-11-18 | 苏州科技学院 | Method for extracting coenzyme Q10 in fermentation biomass |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400458A (en) * | 2018-11-30 | 2019-03-01 | 内蒙古金达威药业有限公司 | A method of the separation and Extraction Co-Q10 from microbial fermentation solution |
| CN109400458B (en) * | 2018-11-30 | 2021-11-23 | 内蒙古金达威药业有限公司 | Method for separating and extracting coenzyme Q10 from microbial fermentation broth |
| CN112755589A (en) * | 2021-02-23 | 2021-05-07 | 山东泰和水处理科技股份有限公司 | Extraction method and device of refined coenzyme Q10 |
| CN113069492A (en) * | 2021-05-07 | 2021-07-06 | 广州市润研基因科技有限公司 | Production technology for ultrasonic-assisted continuous countercurrent extraction of sapindus saponin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107445815A (en) | A kind of method of continuous flow upstream ultrasonic extraction Co-Q10 | |
| CN103520949B (en) | Complete equipment for continuous counter-current ultrasonic extraction | |
| CN101899122B (en) | Aqueous two-phase system extraction method for ganodenic acid and ganoderma lucidum polysaccharide | |
| CN102719396B (en) | Rapid extraction method of human body fat stem cells and special human fat tissue digestant for same | |
| CN106146278B (en) | A kind of technique for extracting separation Co-Q10 from bacteria residue | |
| CN103432193A (en) | Microwave-assisted aqueous two-phase extraction and separation method of kudzu root total flavones | |
| CN104592323B (en) | A kind of method of phloridzin in aqueous two-phase extraction pomace | |
| CN102093748B (en) | Method for preparing radish red pigment homopolymer and radish proanthocyanidin from red-core radishes | |
| CN101337960A (en) | Process for extracting matrine form Chinese traditional medicine extract | |
| CN102746355B (en) | Method for extracting and separating cordycepin | |
| CN104490941B (en) | It is a kind of to improve immunity, antitumor, improvement renal function, the golden cicada flower extract for promoting sleep | |
| CN107033159B (en) | A kind of technique that eurycomanone is extracted from Tongkat Ali | |
| CN108017530A (en) | A kind of method that Co-Q10 is continuously separated from bacteria residue | |
| CN101328201A (en) | Method for extracting betulin from birch bark | |
| CN105477433B (en) | A method of extracting bamboo-leaves flavones from the leaf of bamboo | |
| CN101712731B (en) | Preparation and application of emodin molecular imprinted polymer | |
| CN103641716A (en) | Method for extracting refined chicoric acid | |
| CN107556284A (en) | The method that OPC is extracted from litchi rind | |
| CN104706717B (en) | The method for extraction and purification of herba sophorae alopecuroide total alkali | |
| CN102964407B (en) | Method for extracting astilbin from rhizoma smilacis glabrae and astilbin prepared thereby | |
| CN107827738A (en) | A kind of method that carnosic acid is separated from Rosmarinus officinalis extract | |
| CN107721965A (en) | The extraction process of litchi rind OPC | |
| CN102304177B (en) | Method for extracting and purifying lycoris radiata lectin from lycoris radiata bulbs and lycoris radiata lectin produced by method | |
| CN105748580A (en) | Low-temperature extraction device and method of active ingredients of natural products | |
| CN2910365Y (en) | Single-stage foam separating tower |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171208 |
|
| RJ01 | Rejection of invention patent application after publication |