CN110129292A - A kind of Rosa roxburghii Tratt SOD extracting method and device - Google Patents
A kind of Rosa roxburghii Tratt SOD extracting method and device Download PDFInfo
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- CN110129292A CN110129292A CN201910331300.0A CN201910331300A CN110129292A CN 110129292 A CN110129292 A CN 110129292A CN 201910331300 A CN201910331300 A CN 201910331300A CN 110129292 A CN110129292 A CN 110129292A
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- C12M47/00—Means for after-treatment of the produced biomass or of the fermentation or metabolic products, e.g. storage of biomass
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Abstract
The invention discloses a kind of Rosa roxburghii Tratt SOD extracting method and devices, the Rosa roxburghii Tratt SOD extracting method is first to handle Rosa roxburghii Tratt, is processed into freeze-drying Ribes burejense powder, then extracts, successively be ultrasonically treated, heated again, pH is adjusted, acetone treatment and drying steps, obtain SOD;The method of the present invention operation is controllable, SOD high income.Described device includes cleaning plant, the first grinding device, vacuum freezing drying device, the second grinding device, reaction unit, drying device;Apparatus of the present invention according to process requirements use tinuous production lay structure, can flow line production SOD, easy to operate, controllable, labor intensity is low.
Description
Technical field
The invention belongs to enzyme extractive technique fields, and in particular to a kind of Rosa roxburghii Tratt SOD extracting method and device.
Background technique
Rosa roxburghii Tratt is the fruit of rosaceae Rosa rosa roxburghii, yellow, sometimes with blush.Pulp is crisp, has dense virtue after mature
Fragrance.Since rosa roxburghii nutrition is abundant, have especially rich in superoxide dismutase, i.e. SOD is extensive in Southwestern China area at present
Cultivation.SOD have anti-ageing, protective effect on cancer risk active material, also have the function of it is antiviral, anti-radiation, angiocarpy, Digestive
System and various tumor diseases prevention and treatment aspect, application are very extensive.The prior art, which extracts Rosa roxburghii Tratt SOD, has that yield is not high,
And traditional process equipment is suitable only for a small amount of SOD preparations, and it is also more inconvenient to operate, and is unable to satisfy actual production demand.For
This, researching and developing a kind of Rosa roxburghii Tratt SOD extracting method and device is very important.
Summary of the invention
The first object of the present invention is to provide a kind of Rosa roxburghii Tratt SOD extracting method.
The second object of the present invention is to provide a kind of device for realizing Rosa roxburghii Tratt SOD extracting method.
The first object of the present invention be achieved in that the following steps are included:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 1~5h, extraction temperature is 5~25 DEG C, is then filtered
Filtrate, for filtrate through 5~25min of ultrasonication, processing power is 150~500W, and treatment temperature is 30~45 DEG C, then through from
Heart processing, takes supernatant;
S3, supernatant is heated to 50~70 DEG C, keeps the temperature 15~30min, centrifugal treating, takes supernatant and adjust pH after cooling
To 4~6, it is then centrifuged for handling, takes supernatant that the cold acetone of 1~1.3 times of volume is added and stir evenly, stand 5~30min and wait for
Sediment is generated, is then centrifuged for handling, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
The second object of the present invention be achieved in that including successively sequence lay cleaning plant, the first grinding device,
Vacuum freezing drying device, the second grinding device, reaction unit, drying device, the discharge end of the cleaning plant pass through conveying
Device is connect with the feed end of the first grinding device, and the discharge end of first grinding device passes through conveying device and vacuum refrigeration
The feed end of drying device connects, and the discharge end of the vacuum freezing drying device passes through conveying device and the second grinding device
The discharge end of feed end connection, second grinding device is connected by the feed end of conveying device and reaction unit, described anti-
The discharge end of device is answered to connect by the feed end of conveying device and drying device.
Compared with prior art, the present invention has following technical effect that
1, the method for the present invention is by by Rosa roxburghii Tratt stripping and slicing, then carries out segmented vacuum freeze drying processing, is then comminuted into Ribes burejense powder,
It can not only effectively make Rosa roxburghii Tratt tissue, eucaryotic cell structure sufficiently broken, and be conducive to subsequent reactions and handle, while Rosa roxburghii freeze-dried powder material
Dimensionally stable is suitable for industrialized production convenient for storage;Cooperate ultrasonic treatment after Ribes burejense powder extraction, it is thick to obtain SOD after centrifugation
Liquid has the advantages that crude liquid SOD recovery rate is high;After supernatant heat treatment, precipitate foreign protein, and separated;Pass through tune again
Supernatant pH value is saved, plays the role of purifying SOD;Then foreigh protein removing is further removed by acetone, thus purified
SOD has the advantages that purify efficient, high income;
2, the fresh Rosa roxburghii Tratt cleaning of apparatus of the present invention collection, stripping and slicing crushing, vacuum freeze drying, powder crushing process, thick purification reaction with
And functions/drying, the structure laid using tinuous production is easy to operate, controllable, can be used for industrializing continuous production SOD;Instead
It answers device that can be extracted, be ultrasonically treated to Ribes burejense powder, obtains SOD crude liquid;Centrifugal separating device can be not only used for SOD crude liquid
Centrifuge separation, and thermal denaturation, isoelectric point, acetone treatment reaction purification process can be carried out automatically, each according to process requirements
Reaction treatment process, centrifugal separating device can be automatically separated solid sediment and liquid, while carry out to tophan box clear
It washes, it is easy to operate, substantially reduce labor intensity.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention;
Fig. 2 is the schematic diagram of internal structure of reaction unit;
Fig. 3 is the structural schematic diagram of centrifugal separating device;
In figure: 1- cleaning plant, the first grinding device of 2-, 3- vacuum freezing drying device, the second grinding device of 4-, 5- reaction dress
It sets, 6- drying device, 7- cabinet, 8- pot for solvent extraction, 9- filter, 10- ultrasound tank, 11a- tophan box, 11b- keeps off liquid set, and 11c- connects
Pendular ring, 11d- supernatant holding tank, 11e- catheter, 11f- drain pipe, 11g- centrifugal driving device, 11h- connection frame, 11i-
First helix transporting device, 11j- mobile drive deivce, the second helix transporting device of 11k-, 11l- discharge nozzle, 11m- waste material row
Put pipe, 11o- liquid back pipe, 11p- guide runner, 12- feeder trough, 13- leaching liquor liquid-feeding tube, 14- heat exchanger, 15- stirring motor,
16- ultrasonic generator, 17- heating device, 18a- high-pressure wash pipeline, 18b- connection frame, 18c- rope, 18d- lifting are driven
Dynamic device, 18e- high pressure feed liquor hose, 18f- high pressure liquid spray head, 18g- electric heater.
Specific embodiment
The present invention will be further described below with reference to the drawings, but the present invention is limited in any way, base
In present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
The present invention the following steps are included:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 1~5h, extraction temperature is 5~25 DEG C, is then filtered
Filtrate, for filtrate through 5~25min of ultrasonication, processing power is 150~500W, and treatment temperature is 30~45 DEG C, then through from
Heart processing, takes supernatant;
S3, supernatant is heated to 50~70 DEG C, keeps the temperature 15~30min, centrifugal treating, takes supernatant and adjust pH after cooling
To 4~6, it is then centrifuged for handling, takes supernatant that the cold acetone of 1~1.3 times of volume is added and stir evenly, stand 5~30min and wait for
Sediment is generated, is then centrifuged for handling, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Preferably, the vacuum freeze drying processing is first to freeze 4~8h, and cryogenic temperature is -30~-25 DEG C, then with 2
Temperature is risen to -5~5 DEG C by the speed of~4 DEG C/min, keeps the temperature 6~8h, then temperature risen to 20 with the speed of 3~5 DEG C/min~
30 DEG C, 3~6h is kept the temperature, then temperature is risen to 50~60 DEG C with the speed of 3~5 DEG C/min, keep the temperature 3~6h, vacuum freeze drying
In the process, vacuum degree is 30~40Pa.
Preferably, the leaching liquor is water or inorganic salt solution.
Preferably, the inorganic salt solution is sodium chloride solution,
Preferably, the speed of centrifugal treating described in S2 step is 8000~9000r/min, and the time is 15~30min, and temperature is
2~6 DEG C.
Preferably, the centrifugal speed of centrifugal treating described in S3 step is 12000~13000r/min, and the time is 15
~30min.
Preferably, the temperature of the cold acetone is 2~10 DEG C.
The device of Rosa roxburghii Tratt SOD extracting method as described in the realization shown in attached FIG. 1 to FIG. 3, including the cleaning that successively sequence is laid
Device 1, the first grinding device 2, vacuum freezing drying device 3, the second grinding device 4, reaction unit 5, drying device 6, it is described
The discharge end of cleaning plant 1 is connect by conveying device with the feed end of the first grinding device 2, first grinding device 2
Discharge end is connect by conveying device with the feed end of vacuum freezing drying device 3, the discharging of the vacuum freezing drying device 3
End is connect by conveying device with the feed end of the second grinding device 4, and the discharge end of second grinding device 4 passes through conveying dress
It sets and is connect with the feed end of reaction unit 5, the discharge end of the reaction unit 5 passes through the charging of conveying device and drying device 6
End connection.
Preferably, the reaction unit 5 includes cabinet 7, is successively sequentially laid with pot for solvent extraction 8, filter in the cabinet 7
9, the top of ultrasonic tank 10, centrifugal separating device, the pot for solvent extraction 8 is equipped with feeder trough 12, leaching liquor liquid-feeding tube 13, the extraction
8 lateral surface of tank is equipped with heat exchanger 14, and rabbling mechanism, the stirring electricity at 8 top of rabbling mechanism and pot for solvent extraction are equipped in the pot for solvent extraction 8
Machine 15 connects, and the 8 bottom discharge end of pot for solvent extraction is connected by 9 top feed end of pipe-and-filter, and pipeline is equipped with conveying
Pump, the 9 bottom discharge end of filter is connect by pipeline with 10 top feed end of ultrasonic tank, and pipeline is equipped with delivery pump, institute
It states and is equipped with ultrasonic generator 16 on the outside of ultrasonic tank 10, heating device 17,10 bottom of the ultrasound tank are equipped in ultrasonic tank 10
Discharge end is connect by pipeline with centrifugal separating device feed end, and pipeline is equipped with delivery pump.
Preferably, the ultrasonic tank 10 includes inside and outside tank body, and ultrasonic coupling liquid is housed between inside and outside tank body.
Preferably, the centrifugal separating device includes tophan box 11a, is open design, lower part at the top of the tophan box 11a
Tapered, the bottom end tophan box 11a is equipped with blow-off valve, and the side tophan box 11a is equipped with fluid apertures, and the outer surface tophan box 11a is covered with filtering layer,
The tophan box 11a outer sheath is equipped with gear liquid and covers 11b, and the region between gear liquid set 11b and tophan box 11a is drain area, keeps off liquid
The set bottom 11b and the internally high and externally low outer rim for meeting pendular ring 11c consolidate, and are equipped with supernatant holding tank on the outside of the gear liquid set 11b
11d, the gear liquid set lower part 11b, which is equipped at the top of catheter 11e, catheter 11e and supernatant holding tank 11d, to be connect, the supernatant
The lower part holding tank 11d is equipped with liquid back pipe 11o, and the outlet end of liquid back pipe 11o is located above tophan box 11a, and the supernatant is temporary
The bottom case 11d is equipped with drain pipe 11f, and delivery pipe 11f is equipped with drain valve, is equipped with centrifugal driving device below the tophan box 11a
11g, centrifugal driving device 11g are connect by connection frame 11h with tophan box 11a, and the side the connection frame 11h is equipped with the first spiral
Conveying device 11i, the first bottom helix transporting device 11i are set on sliding rail, are driven on the outside of the first helix transporting device 11i with mobile
Dynamic device 11j connection makes mobile drive deivce 11j be able to drive the first helix transporting device 11i back-and-forth motion, first spiral shell
It revolves the bottom conveying device 11i and is equipped with discharge port, the lower part the first helix transporting device 11i is equipped with the second helix transporting device
To open wide feeding structure at the top of 11k, the second helix transporting device 11k, the discharge end of the second helix transporting device 11k with go out
One end of expects pipe 11l connects, and the discharge nozzle 11l other end is corresponding with the feed end of drying device 6, and the bottom discharge nozzle 11l is equipped with
Trash discharge pipe 11m, trash discharge pipe 11m are equipped with valve.
Preferably, the tophan box 11a outer upper is equipped with a circle guide chute, the corresponding gear liquid set of guide chute
11b inner wall is equipped with guide runner 11p, and guide runner 11p is slidably matched with guide chute, enhances tophan box 11a in the course of work
In stability.
Preferably, the taper frame structure being made of high-pressure wash pipeline 18a, taper are equipped with above the tophan box 11a
Connection frame 18b is equipped at the top of frame structure, connection frame 18b passes through rope 18c and the lifting drive for being set to 7 top of cabinet
The top of 18d connection, the taper frame structure is equipped with high pressure feed liquor hose 18e, and the outside and bottom of taper frame structure are equal
Equipped with high pressure liquid spray head 18f, the connection frame 18b is equipped with electric heater 18g, and the fire end of electric heater 18g is located at taper
In frame structure.
The working principle and the course of work of apparatus of the present invention: fresh Rosa roxburghii Tratt is packed into cleaning plant 1,1 pair of cleaning plant thorn
Pears are handled, and are then sent into the first grinding device 2 through conveying device and are ground into Rosa roxburghii Tratt block, Rosa roxburghii Tratt block is sent into through conveying device
Vacuum freezing drying device 3, the Rosa roxburghii Tratt freeze-drying block handled through vacuum freeze drying are sent into the second grinding device 4 and are ground into thorn
Pears powder;
Ribes burejense powder is conveyed through conveying device, is entered in pot for solvent extraction 8 by feeder trough 12, and leaching liquor liquid-feeding tube 13 adds into pot for solvent extraction 8
Enter the leaching liquor of set amount, while stirring motor 15 drives rabbling mechanism to be stirred continuously material to uniform, heat exchanger 14 plays pair
Feed liquid adjusts the effect of temperature, and feed liquid temperature is made to keep set temperature;After extraction, feed liquid is pumped into filter 9 through conveying
In, filtrate is sent into ultrasonic tank 10;Liquid is heated to set temperature by heating device 17, then 16 work of ultrasonic generator
Make, liquid is ultrasonically treated;Then liquid is pumped into tophan box 11a through conveying again;
It is then centrifuged for driving device 11g work, tophan box 11a rotation, to material first time centrifugal treating, centrifuged supernatant is through liquid
Hole, filtering layer are blocked by gear liquid set 11b, and are accumulated in and connect on pendular ring 11c, by catheter 11e that supernatant feeding supernatant is temporary
Deposit case 11d collection;After centrifugation, centrifugal driving device 11g is shut down, and mobile drive deivce 11j starting pushes the first spiral transferring
Device 11i is sent, the top feed mouth of the first helix transporting device 11i is moved to below tophan box 11a bottom discharge valve;Then it rises
Drop driving device 18d starting, taper frame structure is fallen into tophan box 11a, high pressure liquid spray head 18f spray cleaning solution to from
Sediment impact in heart tank 11a, sediment fall into the feed inlet of the first helix transporting device 11i, the first spiral through blow-off valve
Conveying device 11i conveys sediment, and is discharged into the second helix transporting device from the discharge port of the first helix transporting device 11i
In 11k, sediment is discharged through discharge nozzle 11k, trash discharge pipe 11m;After tophan box 11a is cleaned, taper frame structure is stopped
Only hydrojet;First helix transporting device 11i returns to initial position;
Then the liquid in supernatant holding tank 11d sends tophan box 11a back to by liquid back pipe 11o, and electric heater 18g adds liquid
Heat is to set temperature, and after heat treatment, the rise of taper frame structure returns to initial position;Then second of centrifugal treating,
The supernatant of collection is sent into supernatant holding tank 11d;After centrifugation, taper frame structure is fallen again to tophan box 11a
Interior sediment is cleared up, and sediment is discharged from trash discharge pipe 11m;After tophan box 11a is cleaned, taper frame structure
Stop hydrojet, taper frame structure returns to initial position;First helix transporting device 11i returns to initial position;
Then the liquid in supernatant holding tank 11d sends tophan box 11a back to by liquid back pipe 11o, and passes through acid adding pipe to centrifugation
Acid adding adjusts liquid pH value in the liquid of tank 11a, then third time centrifugal treating, and it is temporary that the supernatant of collection is sent into supernatant
In case 11d;After centrifugation, taper frame structure is fallen again clears up the sediment in tophan box 11a, sediment from
Trash discharge pipe 11m discharge;After tophan box 11a is cleaned, taper frame structure stops hydrojet, and taper frame structure has returned to
Beginning position;First helix transporting device 11i returns to initial position;
Then the liquid in supernatant holding tank 11d sends tophan box 11a back to by liquid back pipe 11o, and passes through acetone pipe to centrifugation
Quantitative cold acetone is added in tank 11a, is then centrifuged for tank 11a with the certain time that slowly runs, is uniformly mixed feed liquid, stops centrifugation
Tank 11a rotation after standing setting time, carries out the 4th centrifugal treating, and the supernatant of collection is sent into supernatant holding tank 11d
And pass through drain pipe 11f outlet;After centrifugation, taper frame structure is fallen again carries out the sediment in tophan box 11a
Cleaning, sediment are sent into drying device 6 and are dried in vacuo to get SOD through discharge nozzle 11, conveying device;Tophan box 11a is clear
After washing, taper frame structure stops hydrojet, and taper frame structure returns to initial position;First helix transporting device 11i is returned
To initial position.
Below with reference to 1~embodiment of embodiment 15, the invention will be further described.
Embodiment 1
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate,
Filtrate is through ultrasonication 5min, and processing power 150W, treatment temperature is 30 DEG C, then through centrifugal treating, takes supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, centrifugal treating, takes supernatant and adjust pH to 4, then after cooling
Centrifugal treating takes supernatant that the cold acetone of 1 times of volume is added and stirs evenly, stands 5min sediment to be generated, be then centrifuged for
Processing, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 2
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 5h, extraction temperature is 25 DEG C, then filters to get filtrate,
Filtrate is through ultrasonication 25min, and processing power 500W, treatment temperature is 45 DEG C, then through centrifugal treating, takes supernatant;
S3, supernatant is heated to 70 DEG C, keeps the temperature 30min, centrifugal treating, takes supernatant and adjust pH to 6, then after cooling
Centrifugal treating, take supernatant be added 1.3 times of volumes cold acetone and stir evenly, stand 30min sediment to be generated, then from
Heart processing, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 3
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 3h, extraction temperature is 15 DEG C, then filters to get filtrate,
Filtrate is through ultrasonication 15min, and processing power 325W, treatment temperature is 37 DEG C, then through centrifugal treating, takes supernatant;
S3, supernatant is heated to 60 DEG C, keeps the temperature 22min, centrifugal treating, takes supernatant and adjust pH to 5, then after cooling
Centrifugal treating takes supernatant that the cold acetone of 1.15 times of volumes is added and stirs evenly, stands 17min sediment to be generated, then
Centrifugal treating, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 4
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, vacuum freeze drying processing is first to freeze 4h, and cryogenic temperature is -30 DEG C, then with the speed of 2 DEG C/min by temperature liter
To -5 DEG C, 6h is kept the temperature, then temperature is risen to 20 DEG C with the speed of 3 DEG C/min, keep the temperature 3h, then with the speed of 3 DEG C/min by temperature
It rises to 50 DEG C, keeps the temperature 3h, during vacuum freeze drying, vacuum degree 30Pa, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate,
Filtrate is through ultrasonication 5min, and processing power 150W, treatment temperature is 30 DEG C, then through centrifugal treating, takes supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, centrifugal treating, takes supernatant and adjust pH to 4, then after cooling
Centrifugal treating takes supernatant that the cold acetone of 1 times of volume is added and stirs evenly, stands 5min sediment to be generated, be then centrifuged for
Processing, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 5
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, vacuum freeze drying processing is first to freeze 8h, and cryogenic temperature is -25 DEG C, then with the speed of 4 DEG C/min by temperature liter
To 5 DEG C, 8h is kept the temperature, then temperature is risen to 30 DEG C with the speed of 5 DEG C/min, keep the temperature 6h, then with the speed of 5 DEG C/min by temperature liter
To 60 DEG C, 6h is protected, during vacuum freeze drying, vacuum degree 40Pa, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 5h, extraction temperature is 25 DEG C, then filters to get filtrate,
Filtrate is through ultrasonication 25min, and processing power 500W, treatment temperature is 45 DEG C, then through centrifugal treating, takes supernatant;
S3, supernatant is heated to 70 DEG C, keeps the temperature 30min, centrifugal treating, takes supernatant and adjust pH to 6, then after cooling
Centrifugal treating, take supernatant be added 1.3 times of volumes cold acetone and stir evenly, stand 30min sediment to be generated, then from
Heart processing, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 6
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, vacuum freeze drying processing is first to freeze 6h, and cryogenic temperature is -27 DEG C, then with the speed of 3 DEG C/min by temperature liter
To 0 DEG C, 7h is kept the temperature, then temperature is risen to 25 DEG C with the speed of 4 DEG C/min, keep the temperature 4.5h, then with the speed of 4 DEG C/min by temperature
It rises to 55 DEG C, keeps the temperature 4.5h, during vacuum freeze drying, vacuum degree 35Pa, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 3h, extraction temperature is 15 DEG C, then filters to get filtrate,
Filtrate is through ultrasonication 15min, and processing power 325W, treatment temperature is 37 DEG C, then through centrifugal treating, takes supernatant;
S3, supernatant is heated to 60 DEG C, keeps the temperature 22min, centrifugal treating, takes supernatant and adjust pH to 5, then after cooling
Centrifugal treating takes supernatant that the cold acetone of 1.15 times of volumes is added and stirs evenly, stands 17min sediment to be generated, then
Centrifugal treating, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 7
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to water in S2, Ribes burejense powder and stirs evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate, filtrate
Through ultrasonication 5min, processing power 150W, treatment temperature is 30 DEG C, then through centrifugal treating, speed 8000r/min,
Time is 15min, and temperature is 2 DEG C, takes supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, centrifugal treating, takes supernatant and adjust pH to 4, then after cooling
Centrifugal treating takes supernatant that the cold acetone of 1 times of volume is added and stirs evenly, stands 5min sediment to be generated, be then centrifuged for
Processing, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 8
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to inorganic salt solution in S2, Ribes burejense powder and stirs evenly, extracts 5h, extraction temperature is 25 DEG C, is then filtered
Filtrate, filtrate is through ultrasonication 25min, and processing power 500W, treatment temperature is 45 DEG C, then through centrifugal treating, speed is
9000r/min, time 30min, temperature are 6 DEG C, take supernatant;
S3, supernatant is heated to 70 DEG C, keeps the temperature 30min, centrifugal treating, takes supernatant and adjust pH to 6, then after cooling
Centrifugal treating, take supernatant be added 1.3 times of volumes cold acetone and stir evenly, stand 30min sediment to be generated, then from
Heart processing, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 9
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, vacuum freeze drying processing is first to freeze 4h, and cryogenic temperature is -30 DEG C, then with the speed of 2 DEG C/min by temperature liter
To -5 DEG C, 6h is kept the temperature, then temperature is risen to 20 DEG C with the speed of 3 DEG C/min, keep the temperature 3h, then with the speed of 3 DEG C/min by temperature
It rises to 50 DEG C, keeps the temperature 3h, during vacuum freeze drying, vacuum degree 30Pa, then it is ground into Ribes burejense powder;
Slowly adding water in S2, Ribes burejense powder and stir evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate, filtrate warp
Ultrasonication 5min, processing power 150W, treatment temperature are 30 DEG C, then through centrifugal treating, speed 8500r/min, when
Between be 22min, temperature be 4 DEG C, take supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, centrifugal treating, takes supernatant and adjust pH to 4, then after cooling
Centrifugal treating takes supernatant that the cold acetone of 1 times of volume is added and stirs evenly, stands 5min sediment to be generated, be then centrifuged for
Processing, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 10
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to water in S2, Ribes burejense powder and stirs evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate, filtrate
Through ultrasonication 5min, processing power 150W, treatment temperature is 30 DEG C, then through centrifugal treating, speed 8000r/min,
Time is 15min, and temperature is 2 DEG C, takes supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, after cooling centrifugal treating, centrifugal speed 12000r/min, when
Between be 15min, take supernatant and adjust pH to 4, be then centrifuged for handling, centrifugal speed 12000r/min, time 15min,
It takes supernatant that the cold acetone of 1 times of volume is added and stirs evenly, stand 5min sediment to be generated, be then centrifuged for handling, be centrifuged
Speed is 12000r/min, time 15min, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 11
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to inorganic salt solution in S2, Ribes burejense powder and stirs evenly, extracts 5h, extraction temperature is 25 DEG C, is then filtered
Filtrate, filtrate is through ultrasonication 25min, and processing power 500W, treatment temperature is 45 DEG C, then through centrifugal treating, speed is
9000r/min, time 30min, temperature are 6 DEG C, take supernatant;
S3, supernatant is heated to 70 DEG C, keeps the temperature 30min, after cooling centrifugal treating, centrifugal speed 13000r/min, when
Between be 30min, take supernatant and adjust pH to 6, be then centrifuged for handling, centrifugal speed 13000r/min, time 30min,
It takes supernatant that the cold acetone of 1.3 times of volumes is added and stirs evenly, stand 30min sediment to be generated, be then centrifuged for handling, from
Heart speed is 13000r/min, time 30min, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 12
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, vacuum freeze drying processing is first to freeze 4h, and cryogenic temperature is -30 DEG C, then with the speed of 2 DEG C/min by temperature liter
To -5 DEG C, 6h is kept the temperature, then temperature is risen to 20 DEG C with the speed of 3 DEG C/min, keep the temperature 3h, then with the speed of 3 DEG C/min by temperature
It rises to 50 DEG C, keeps the temperature 3h, during vacuum freeze drying, vacuum degree 30Pa, then it is ground into Ribes burejense powder;
Slowly adding water in S2, Ribes burejense powder and stir evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate, filtrate warp
Ultrasonication 5min, processing power 150W, treatment temperature are 30 DEG C, then through centrifugal treating, speed 8500r/min, when
Between be 22min, temperature be 4 DEG C, take supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, after cooling centrifugal treating, centrifugal speed 12500r/min, when
Between be 22min, take supernatant and adjust pH to 4, be then centrifuged for handling, centrifugal speed 12500r/min, time 22min,
It takes supernatant that the cold acetone of 1 times of volume is added and stirs evenly, stand 5min sediment to be generated, be then centrifuged for handling, be centrifuged
Speed is 12500r/min, time 22min, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 13
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to water in S2, Ribes burejense powder and stirs evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate, filtrate
Through ultrasonication 5min, processing power 150W, treatment temperature is 30 DEG C, then through centrifugal treating, speed 8000r/min,
Time is 15min, and temperature is 2 DEG C, takes supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, after cooling centrifugal treating, centrifugal speed 12000r/min, when
Between be 15min, take supernatant and adjust pH to 4, be then centrifuged for handling, centrifugal speed 12000r/min, time 15min,
It taking supernatant that the cold acetone of 1 times of volume is added and stirs evenly, the temperature of cold acetone is 2 DEG C, 5min sediment to be generated is stood,
It is then centrifuged for handling, centrifugal speed 12000r/min, time 15min, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 14
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to inorganic salt solution in S2, Ribes burejense powder and stirs evenly, extracts 5h, extraction temperature is 25 DEG C, is then filtered
Filtrate, filtrate is through ultrasonication 25min, and processing power 500W, treatment temperature is 45 DEG C, then through centrifugal treating, speed is
9000r/min, time 30min, temperature are 6 DEG C, take supernatant;
S3, supernatant is heated to 70 DEG C, keeps the temperature 30min, after cooling centrifugal treating, centrifugal speed 13000r/min, when
Between be 30min, take supernatant and adjust pH to 6, be then centrifuged for handling, centrifugal speed 13000r/min, time 30min,
It takes supernatant that the cold acetone of 1.3 times of volumes is added and stirs evenly, the temperature of cold acetone is 10 DEG C, and it is to be generated heavy to stand 30min
Starch is then centrifuged for handling, centrifugal speed 13000r/min, time 30min, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
Embodiment 15
Rosa roxburghii Tratt SOD extracting method, comprising the following steps:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, vacuum freeze drying processing is first to freeze 4h, and cryogenic temperature is -30 DEG C, then with the speed of 2 DEG C/min by temperature liter
To -5 DEG C, 6h is kept the temperature, then temperature is risen to 20 DEG C with the speed of 3 DEG C/min, keep the temperature 3h, then with the speed of 3 DEG C/min by temperature
It rises to 50 DEG C, keeps the temperature 3h, during vacuum freeze drying, vacuum degree 30Pa, then it is ground into Ribes burejense powder;
Slowly adding water in S2, Ribes burejense powder and stir evenly, extracts 1h, extraction temperature is 5 DEG C, then filters to get filtrate, filtrate warp
Ultrasonication 5min, processing power 150W, treatment temperature are 30 DEG C, then through centrifugal treating, speed 8500r/min, when
Between be 22min, temperature be 4 DEG C, take supernatant;
S3, supernatant is heated to 50 DEG C, keeps the temperature 15min, after cooling centrifugal treating, centrifugal speed 12500r/min, when
Between be 22min, take supernatant and adjust pH to 4, be then centrifuged for handling, centrifugal speed 12500r/min, time 22min,
It taking supernatant that the cold acetone of 1 times of volume is added and stirs evenly, the temperature of cold acetone is 6 DEG C, 5min sediment to be generated is stood,
It is then centrifuged for handling, centrifugal speed 12500r/min, time 22min, taking precipitate;S4, after sediment is dried in vacuo
Obtain SOD.
Claims (10)
1. a kind of Rosa roxburghii Tratt SOD extracting method, it is characterised in that the following steps are included:
S1, after cleaning fresh Rosa roxburghii Tratt, fruit thorniness, fruit stone is removed, is then comminuted into Rosa roxburghii Tratt block, then Rosa roxburghii Tratt block is done through vacuum refrigeration
Dry processing, then it is ground into Ribes burejense powder;
It is slowly added to leaching liquor in S2, Ribes burejense powder and stirs evenly, extracts 1~5h, extraction temperature is 5~25 DEG C, is then filtered
Filtrate, for filtrate through 5~25min of ultrasonication, processing power is 150~500W, and treatment temperature is 30~45 DEG C, then through from
Heart processing, takes supernatant;
S3, supernatant is heated to 50~70 DEG C, keeps the temperature 15~30min, centrifugal treating, takes supernatant and adjust pH after cooling
To 4~6, it is then centrifuged for handling, takes supernatant that the cold acetone of 1~1.3 times of volume is added and stir evenly, stand 5~30min and wait for
Sediment is generated, is then centrifuged for handling, taking precipitate;
S4, SOD is obtained after being dried in vacuo sediment.
2. Rosa roxburghii Tratt SOD extracting method according to claim 1, it is characterised in that the vacuum freeze drying processing is first to freeze
4~8h, cryogenic temperature are -30~-25 DEG C, and temperature is then risen to -5~5 DEG C with the speed of 2~4 DEG C/min, keeps the temperature 6~8h,
Temperature is risen to 20~30 DEG C with the speed of 3~5 DEG C/min again, keeps the temperature 3~6h, then with the speed of 3~5 DEG C/min by temperature liter
To 50~60 DEG C, 3~6h is kept the temperature, during vacuum freeze drying, vacuum degree is 30~40Pa.
3. Rosa roxburghii Tratt SOD extracting method according to claim 1, it is characterised in that the leaching liquor is water or inorganic salt solution.
4. Rosa roxburghii Tratt SOD extracting method according to claim 1, it is characterised in that the speed of centrifugal treating described in S2 step is
8000~9000r/min, time are 15~30min, and temperature is 2~6 DEG C.
5. Rosa roxburghii Tratt SOD extracting method according to claim 1, it is characterised in that the centrifugation speed of centrifugal treating described in S3 step
Degree is 12000~13000r/min, and the time is 15~30min.
6. Rosa roxburghii Tratt SOD extracting method according to claim 1, it is characterised in that the temperature of the cold acetone is 2~10 DEG C.
7. a kind of device for realizing any Rosa roxburghii Tratt SOD extracting method of claim 1~6, it is characterised in that including successively suitable
The cleaning plant (1) of sequence laying, the first grinding device (2), vacuum freezing drying device (3), the second grinding device (4), reaction
Device (5), drying device (6), the discharge end of the cleaning plant (1) by conveying device and the first grinding device (2) into
Expect end connection, the discharge end of first grinding device (2) passes through the feed end of conveying device and vacuum freezing drying device (3)
The discharge end of connection, the vacuum freezing drying device (3) is connected by the feed end of conveying device and the second grinding device (4)
It connects, the discharge end of second grinding device (4) is connect by conveying device with the feed end of reaction unit (5), the reaction
The discharge end of device (5) is connect by conveying device with the feed end of drying device (6).
8. the device of Rosa roxburghii Tratt SOD extracting method according to claim 7, it is characterised in that the reaction unit (5) includes case
Body (7), the cabinet (7) is interior to be successively sequentially laid with pot for solvent extraction (8), filter (9), ultrasonic tank (10), centrifugal separating device,
The top of the pot for solvent extraction (8) is equipped with feeder trough (12), leaching liquor liquid-feeding tube (13), and pot for solvent extraction (8) lateral surface is equipped with and changes
Hot device (14), the pot for solvent extraction (8) is interior to be equipped with rabbling mechanism, and the stirring motor (15) at the top of rabbling mechanism and pot for solvent extraction (8) is even
It connecing, pot for solvent extraction (8) the bottom discharge end is connected by pipe-and-filter (9) top feed end, and pipeline is equipped with delivery pump,
Filter (9) the bottom discharge end is connect by pipeline with ultrasonic tank (10) top feed end, and pipeline is equipped with delivery pump, institute
It states and is equipped with ultrasonic generator (16) on the outside of ultrasonic tank (10), be equipped with heating device (17) in ultrasonic tank (10), the ultrasound
Tank (10) bottom discharge end is connect by pipeline with centrifugal separating device feed end, and pipeline is equipped with delivery pump.
9. the device of Rosa roxburghii Tratt SOD extracting method according to claim 8, it is characterised in that the centrifugal separating device include from
Heart tank (11a), tophan box (11a) top is open design, and lower part is tapered, and the tophan box bottom end (11a) is equipped with blow-off valve,
The tophan box side (11a) is equipped with fluid apertures, and the outer surface tophan box (11a) is covered with filtering layer, and tophan box (11a) outer sheath is equipped with gear
Liquid set (11b), the region kept off between liquid set (11b) and tophan box (11a) are drain area, and the gear liquid set bottom (11b) and interior height are outer
The outer rim consolidation for connecing pendular ring (11c) of low shape, gear liquid set (11b) outside are equipped with supernatant holding tank (11d), keep off liquid set
The lower part (11b) is equipped with catheter (11e), connect at the top of catheter (11e) and supernatant holding tank (11d), the supernatant is temporary
The case lower part (11d) is deposited equipped with liquid back pipe (11o), the outlet end of liquid back pipe (11o) is located above tophan box (11a), the supernatant
The liquid holding tank bottom (11d) is equipped with drain pipe (11f), and delivery pipe (11f) is equipped with drain valve, sets below the tophan box (11a)
Have centrifugal driving device (11g), centrifugal driving device (11g) is connect by connection frame (11h) with tophan box (11a), the company
The frame side (11h) is connect equipped with the first helix transporting device (11i), the first helix transporting device bottom (11i) is set on sliding rail, the
It is connect with mobile drive deivce (11j) on the outside of one helix transporting device (11i), mobile drive deivce (11j) is made to be able to drive the
One helix transporting device (11i) be moved forward and backward, the first helix transporting device bottom (11i) be equipped with discharge port, described first
The helix transporting device lower part (11i) is equipped with the second helix transporting device (11k), is spacious at the top of the second helix transporting device (11k)
Feeding structure is opened, the discharge end of second helix transporting device (11k) is connect with one end of discharge nozzle (11l), discharge nozzle
(11l) other end is corresponding with the feed end of drying device (6), and the discharge nozzle bottom (11l) is equipped with trash discharge pipe (11m), gives up
Expect that delivery pipe (11m) is equipped with valve.
10. the device of Rosa roxburghii Tratt SOD extracting method according to claim 9, it is characterised in that set above the tophan box (11a)
By the taper frame structure being made of high-pressure wash pipeline (18a), taper frame structural top is equipped with connection frame (18b), connection
Frame (18b) is connect by rope (18c) with the lifting drive (18d) being set at the top of cabinet (7), the taper frame structure
Top be equipped with high pressure feed liquor hose (18e), the outside and bottom of taper frame structure are equipped with high pressure liquid spray head (18f), institute
Connection frame (18b) is stated equipped with electric heater (18g), the fire end of electric heater (18g) is located in taper frame structure.
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