CN106366206B - A kind of method that steam explosion combination biological enzyme technology prepares radix pseudostellariae source polysaccharide - Google Patents
A kind of method that steam explosion combination biological enzyme technology prepares radix pseudostellariae source polysaccharide Download PDFInfo
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Abstract
The invention belongs to Pseudostellaria Polysaccharide preparation fields, specifically disclose a kind of method that steam explosion combination biological enzyme technology prepares radix pseudostellariae source polysaccharide.Including radix pseudostellariae pretreatment, double sections of Steam explosion treatments, biological enzyme enzymatic hydrolysis, water hot extraction, extract liquor CO2Processing, three-stage filtration, detoxification and alcohol precipitation totally eight steps.Two sections of steam explosion technologies in the present invention have not only admirably achieved radix pseudostellariae and have extracted pretreated effect, while the technique can also reduce the noxious material generated in even removal steam blasting；Nonionic surfactant is introduced in the process of biological enzyme enzymatic hydrolysis can be improved enzymolysis efficiency and reduces the addition of exogenous enzymes and then mitigate the work load of subsequent processing；Preparation method of the invention is suitable for the preparation and production of radix pseudostellariae source polysaccharide material, has important dissemination.
Description
Technical field
The invention belongs to Pseudostellaria Polysaccharide preparation fields, and in particular to a kind of steam explosion combination biological enzyme technology prepares radix pseudostellariae
The method of source polysaccharide.
Background technique
Radix pseudostellariae is the root tuber of pinkwort caryophyllaceous ginseng first recorded in " new compilation of materia medica ", main product in Fujian, Jiangsu, Anhui,
Shandong etc. saves.2010 editions " Chinese Pharmacopoeia " description radix pseudostellariaes are sweet in flavor, slight bitter, mild-natured；Returns spleen, lung channel；With replenishing qi to invigorate the spleen, promote the production of body fluid
The effect of moistening lung；Tired, loss of appetite, eak after being ill, deficiency of both vital energy and Yin, spontaneous perspiration and thirst, the dryness of the lung for spleen deficiency body.Radix pseudostellariae system health
The kind of " the article list that can be used for health food " that portion promulgates, to radix pseudostellariae chemical component studies have shown that radix pseudostellariae contains
There are amino acid, carbohydrate, glycoside, phospholipid, cyclic peptide, fatty acid, grease type, volatile component, sterols and micro member
Element etc., wherein Pseudostellaria Polysaccharide is an important component of radix pseudostellariae biological active agents.Modern pharmacology research proves: too
Sub- gracilis polysaccharide has the effects that enhance immune function, improves ability of learning and memory, is antifatigue, delay senescence, is anti-inflammatory.
At present people to the utilization of radix pseudostellariae also in the starting exploratory stage, it is also constantly deep to the pharmacological research of radix pseudostellariae
Enter.As can the preparation method for developing a kind of Pseudostellaria Polysaccharide has significant meaning.
Summary of the invention
In place of overcoming the above deficiencies in the existing technologies, the purpose of the present invention is intended to provide a kind of steam explosion combination life
The method that object zymotechnic prepares radix pseudostellariae source polysaccharide.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of method that steam explosion combination biological enzyme technology prepares radix pseudostellariae source polysaccharide, steps are as follows:
S1, radix pseudostellariae pretreatment: by drying radix pseudostellariae successively after select, go must, bake, be sliced and steam five works
Sequence；Wherein, selecting is to screen current year drying radix pseudostellariae, and the radix pseudostellariae for going mouldy or have impurity is rejected；It goes to refer to
Radix pseudostellariae cercus is removed and is separated using mechanical equipment；Baking refers to that vacuumize baking technology using low temperature removes again
Radix pseudostellariae surface moisture be convenient for subsequent slice, 50 ~ 60 DEG C of baked temperature, baking time 10min ~ 20mim, vacuum pressure 0.03
~0.05MPa；Slice refers to the slice that the radix pseudostellariae after baking is carried out to radix pseudostellariae ginseng body using Chinese herbal medicine slicer, after slice
Radix pseudostellariae piece with a thickness of 0.5 ~ 1.0mm；Steaming is that radix pseudostellariae piece is placed in food steamer to handle, and steams and is heated using vapor,
Steaming time is 20 ~ 30min；
S2, double sections of Steam explosion treatments: using the radix pseudostellariae piece after steaming as blasting substrates, successively pass through Steam explosion treatment
I and Steam explosion treatment II, double sections of Steam explosion treatment interval times are 2 ~ 5min；The condition of Steam explosion treatment I are as follows: explosion
Chamber coefficient is 0.7 ~ 0.9, and for explosion steam pressure up to 0.5 ~ 0.8MPa, it is 10 ~ 15min, explosion that explosion pressure maintaining, which handles the time,
Time is not higher than 0.00875s；The condition of Steam explosion treatment II are as follows: the same cavity explosion treatment of blasting gear on the same stage, explosion are steamed
Steam pressure is up to 1.5 ~ 2.2MPa, and explosion pressure maintaining handles the time as 30 ~ 50s, and blasting time is not higher than 0.00875s；Double sections of steam are quick-fried
Entrainer is added during tear reason, entrainer is detailed catalogue diamond dust and Ca (OH)2The compound of powder, diamond dust: Ca (OH)2
The mass values of powder are 4:1 ~ 1:1；By percentage to the quality, entrainer total addition level accounts for the 1.5 ~ 3% of blasting substrates, and in batches
Addition, the 1/3 ~ 2/5 of Steam explosion treatment I total amount of adding, Steam explosion treatment II adds the entrainer of surplus；
S3, biological enzyme enzymatic hydrolysis: by after explosion treatment and when temperature is down to room temperature radix pseudostellariae material matrix and water with solid-liquid
It is mixed than 1kg:1L ~ 1kg:3L, the pH value of solidliquid mixture is adjusted to 4.5 ~ 5.0, is then added at one time non-ionic surface
Activating agent adds cellulase, zytase and pectase and is digested, and 50 ~ 55 DEG C of hydrolysis temperature, enzymolysis time 30 ~
45min, the stage for digesting preceding 20 ~ 25min are at the uniform velocity stirred (100 ~ 120rpm/min of revolving speed), wait digest at the end of adjusting mix
The pH value of object is closed to neutrality；Wherein, (the crown prince after drying radix pseudostellariae piece, that is, S1 slice, before steaming in terms of the drying radix pseudostellariae piece of every g
Join piece), cellulase, zytase, pectase and nonionic surfactant additive amount be respectively as follows: 10 ~ 15FPU/g, 100
~150U/g,80~110U/g,0.003~0.05g/g；The nonionic surfactant is Berol, PEG, Tween-80 and BSA
One of or a variety of, the preferably equal mass mixings of ratio when a variety of uses；
S4, water hot extraction: it is dosed in water hot extraction's tank after the radix pseudostellariae matrix after explosion treatment is collected, hot water in tank
The mass values of amount and radix pseudostellariae matrix are 15:1 ~ 20:1, extract 90 ~ 100 DEG C of hot water temperature, 2 ~ 3h of extraction time, extraction time
Number 1 time；The phase is at the uniform velocity stirred before extraction, to be extracted to stop stirring when carrying out to 3/5 extraction time；
S5, extract liquor CO2Processing: after to water hot extraction, obtained extract liquor is cooled to first with heat exchanger
Room temperature then moves in clean rustless steel container, sterile CO is then passed through into extract liquor after cooling2Gas, CO2Flow velocity is
10~15m3/ min, is passed through CO25 ~ 15min of gas time；It is passed through CO2When gas, CO2Gas is by pipeline through rustless steel container bottom
Gas distributor enter inside extract liquor；
S6, three-stage filtration: extract liquor CO2After processing respectively by the grade one filter of tandem compound, secondary filter and
Tertiary filter realizes filtration operation；Wherein, grade one filter and secondary filter are conventional cartridge filter, level-one mistake
The filter core aperture of filter and secondary filter is respectively 4.5 ~ 5 μm, 0.2 ~ 0.25 μm；Tertiary filter is hollow fibre filtering
Device, the molecular cut off of doughnut are 10000 ~ 30000 dalton；
S7, detoxification: the radix pseudostellariae extract liquor after three-stage filtration is successively passed through into D301 resin packed column and NKAII resin is filled out
Column is filled, extract liquor is 0.15 ~ 0.2MPa into column pressure, collects extract liquor；
S8, alcohol precipitation: depressurize half concentration for the radix pseudostellariae extract liquor after detoxification first, and concentration pressure is 0.01 ~
0.05MPa, 50 ~ 70 DEG C of thickening temperature, 2 ~ 3h of concentration time；Followed by will depressurize half concentrate be cooled to 10 ~ 25 DEG C and to its
The middle 95% edible ethanol liquid that 2 ~ 3 times of volumes are added, stands 8 ~ 10h, and it is radix pseudostellariae source polysaccharide that finally centrifugation, which obtains sediment,；
Wherein, centrifugal rotational speed is 10000 ~ 15000 rpm/min, and centrifuging temperature temperature control is at 10 ~ 15 DEG C, 15 ~ 25min of centrifugation time.
Preferably, carry out three-stage filtration using self-control three-level filter system in S6, the three-level filter system include tubular type from
Scheming, centrifugation liquid storage tank (temperature controlling range is 5~10 DEG C in tank), power transmitting assembly I, power transmitting assembly II, power
Transmission assembly III, grade one filter, secondary filter, tertiary filter and its extraneous subsystem；Power transmitting assembly I by
Kinetic pump I and check-valves I are connected in series；Power transmitting assembly II is connected in series by kinetic pump II and check-valves II；Power transmission
Component III is connected in series by kinetic pump III and check-valves III；Grade one filter and secondary filter are conventional cartridge filter；
Tertiary filter is self-control filter, and structure includes cylinder, doughnut tread assembly, pedestal；Cylinder body bottom and top difference
Equipped with inlet and liquid outlet, interlayer is equipped with outside cylinder, the upper and lower ends of interlayer are respectively equipped with interlayer import and interlayer outlet；
Doughnut tread assembly includes being evenly equipped with porous package shell, several doughnuts (preferably 300 ~ 600), these are hollow
Fiber merges bunchy and is placed in inside package shell；Pedestal is cylindrical body, cylindrical body upper section be it is hollow be cylindrical in shape, middle and lower sections it is solid,
The middle and lower sections of pedestal are solid to be equipped with through-hole compatible with doughnut quantity and its size；Pedestal is located at below liquid outlet,
It is close to cylinder roof and is firmly connected with it；The upper end of doughnut is open and is threaded through in the through-hole of pedestal, and lower end closed is simultaneously
It is fixedly connected with package shell bottom wall；The extraneous subsystem of tertiary filter includes kinetic pump IV, check-valves IV, constant temperature refrigeration
Check-valves IV, constant temperature refrigeration water tank and kinetic pump IV are successively contacted extremely in water tank (controllable temperature range are as follows: 5~15 DEG C), interlayer outlet
Interlayer import forms a closed cycle system；Tube centrifuge is successively contacted by pipeline and is centrifuged liquid storage tank, kinetic pump I, non-return
Valve I, grade one filter, kinetic pump II, check-valves II, secondary filter, kinetic pump III, check-valves III to tertiary filter
Inlet；Grade one filter and be respectively 4.5 ~ 5 μm, 0.2 ~ 0.22 μm with the filter core aperture of secondary filter；Doughnut
Molecular cut off is 10000 ~ 30000 dalton；
Three-stage filtration step are as follows:
(a) start the equipment by S5 treated extract liquor input tube centrifuge inner cavity first and carry out centrifugal work,
Centrifugal rotational speed is centrifuged 20 ~ 30min up to 4000 ~ 6000rpm/min；The centrifugal clear liquid that will acquire in time after centrifugation be transferred to
It is centrifuged in liquid storage tank, and temperature controlling range is 5 ~ 10 DEG C in the tank；
(b) the cooling centrifugate that upper process obtains is crossed check-valves I by the road and is delivered to grade one filter by starting kinetic pump I
Interior, 0.2 ~ 0.6 Mpa of input pressure realizes first time coarse filtration；
(c) the by-pass filtration liquid obtained after grade one filter is crossed check-valves II by the road and is delivered to by starting kinetic pump II
In secondary filter, 0.2 ~ 0.6 Mpa of input pressure realizes second of coarse filtration；
(d) start kinetic pump IV, by temperature obtained in constant temperature refrigeration water tank be 5 ~ 15 DEG C cold water by the road from folder
Layer import enters in interlayer, and crosses check-valves IV by the road by interlayer outlet and be recycled in constant temperature refrigeration water tank；To in cylinder
Chamber temperature restarts kinetic pump III and the secondary filtration liquid obtained after secondary filter is crossed non-return by the road when reaching 5 ~ 15 DEG C
Valve III is delivered in tertiary filter by inlet, 0.2 ~ 0.6 MPa of input pressure, and secondary filtration liquid is first from package shell
It is porous enter package shell inside, due to the crown_interception of doughnut, the impurity in secondary filtration liquid is blocked in hollow fibre
The outside of dimension, and extract liquor then passes through doughnut and enters pedestal from doughnut top opening, then comes out from liquid outlet.
Further, S6 further includes that step (e) is instead cleaned: at the end of work to be filtered, can carry out the reverse cleaning of the system
Operation, manual 180 ° of integrated regulation power transmitting assemblies I, power transmitting assembly II, power transmitting assembly III direction, that is, it is original
Import become exporting, reconnect corresponding pipeline, while starting above-mentioned kinetic pump I, kinetic pump II, kinetic pump III, will clean
Purified water enter in cylinder through barrel liquid discharge mouth, then ejected wash water is finally from centrifugation liquid storage tank discharge, each filter pressure in operation
Power list index must not be higher than 0.3 MPa, repeat 2 ~ 3 times.
Preferably, be centrifuged between liquid storage tank and kinetic pump I, between check-valves I and grade one filter, grade one filter and dynamic
Power pumps between II, between check-valves II and secondary filter, between secondary filter and kinetic pump III, check-valves III and three-level
Pipeline between filter takes movable connection method.
Further, the movable connection method is clamp connection.
Preferably, tube centrifuge is GF- divergence type.
Steam explosion technology can will infilter the sudden release of inside plant tissues gas compressed short time and finish, purpose
It is to be decomposed raw material as required with less energy.Steam blasting by whole raw materials in container in Millisecond time range,
Airspace is suspended in the form for frying scattered.Since its action time is short, energy density is high and concentrates, and gas molecule can permeate
To between the macromoleculars such as cellulose and lignin, adequately material is decomposed on macromolecular level.Therefore, steam blasting process
The copolymer for lignin, hemicellulose and the cellulose that plant cell wall pectin is inlayed can be broken up as lignin, pectin, half
The dispersion of cellulose and cellulose.The present invention, which is just allowing for steam explosion technology, can destroy plant cell wall natural barrier
System, thus using steam explosion technology by the pretreatment process before being extracted as radix pseudostellariae, so that it is effective to be conducive to radix pseudostellariae
The extraction and separation of component.But there are still subproblems for steam explosion technology pretreatment radix pseudostellariae, such as in the height of steam blasting
The lignocellulosic of plant cell wall can generate certain noxious material in warm high-pressure process, such as formic acid, furfural, phenolic compound
Deng.Therefore, it is added to entrainer again in double section steam blasting stages of the invention, diamond dust is presented in the moment of steam blasting
Stronger shear action further strengthens the cell natural barrier system for breaking radix pseudostellariae, Ca (OH)2Addition it is then quick-fried in steam
It is unfavorable for the generation of noxious material in broken process environment, reduces the conversion of noxious material.CO is passed through in extract liquor2Processing, CO2With
Ca(OH)2Reaction generates CaCO3Precipitating, is conducive in three-stage filtration process and diamond dust removes together, while adjusting extract liquor
PH value, so that D301 resin packed column and NKAII resin packed column slant acidity, improve detoxification efficiency.In addition, the present invention steams
Addition enzyme preparation enzymatic hydrolysis is remarkably improved the recovery rate of effective component after steam explosion is broken, and cellulase, wood have been arrived in use in the present invention
The mixing enzyme system of three kinds of enzymes of dextranase and pectase, but Cellulase Unit enzyme activity is lower, enzyme dosage is higher and enzyme itself is easy
Inactivation, while during ligocellulose degradation, a large amount of hydrophobic groups on lignin can be with the carbon of molecule on cellulase
Hydrophobic interaction occurs for chain, adsorbs to it, reduces effective enzyme amount in enzymolysis process, hinders the enzymatic hydrolysis of cellulose.Cause
This, adds nonionic surface active agent in lignocellulosic Matrix lysis to reduce cellulase dosage, and utilize these
Nonionic surface active agent promotes enzymolysis efficiency to improve.Therefore, the radix pseudostellariae pretreatment of preparation method of the present invention, double sections of steam
Explosion treatment, biological enzyme enzymatic hydrolysis, water hot extraction, extract liquor CO2Processing, three-stage filtration, detoxification and alcohol precipitation are between totally eight steps
It is complementary, the positive synergistic effect of presentation.
The utility model has the advantages that
1, two sections of steam explosion technologies in the present invention have not only admirably achieved radix pseudostellariae and have extracted pretreated effect, together
When the technique can also reduce the noxious material that generates in even removal steam blasting；
2, CO is passed through in extract liquor2Processing, CO2With Ca (OH)2Reaction generates CaCO3Precipitating, not only effectively removes introduction
Calcium ion may also be advantageous in three-stage filtration process and diamond dust removes together, while adjust extract liquor pH value, so that D301
Resin packed column and NKAII resin packed column slant acidity improve detoxification efficiency；
3, there is the present invention technique precision, the scale process standard of being easy to operate with, continuous operation, significantly improve
The characteristics of extraction efficiency of radix pseudostellariae source polysaccharide, reduction labor intensity；
4, nonionic surfactant is introduced in the process of biological enzyme enzymatic hydrolysis can be improved enzymolysis efficiency and reduces exogenous enzymes
Addition so that mitigate subsequent processing work load；Preparation method of the invention be suitable for radix pseudostellariae source polysaccharide material preparation with
Production has important dissemination.
Detailed description of the invention
Fig. 1: the radix pseudostellariae matrix photo after explosion treatment；
Fig. 2: the structural schematic diagram of three-level filter system is made in the present invention by oneself；
Fig. 3: structural schematic diagram when three-level filter system is in anti-cleaning state is made in the present invention by oneself；
Description of symbols: 1- tube centrifuge, 2- are centrifuged liquid storage tank, 31- kinetic pump I, 41- check-valves I, 32- power
Pump II, 42- check-valves II, 33- kinetic pump III, 43- check-valves III, 34- kinetic pump IV, 44- check-valves IV, 5- by-pass filtration
Device, 6- secondary filter, 7- cylinder, 8- inlet, 9- liquid outlet, 10- interlayer, 11- interlayer import, the outlet of 12- interlayer, 13-
Pedestal, 14- package shell, 15- doughnut, 16- constant temperature refrigeration water tank.
Specific embodiment
The contents of the present invention are described in further detail with reference to the accompanying drawings and detailed description:
Embodiment 1
A kind of method that steam explosion combination biological enzyme technology prepares radix pseudostellariae source polysaccharide, steps are as follows:
S1, radix pseudostellariae pretreatment: by drying radix pseudostellariae successively after select, go must, bake, be sliced and steam five works
Sequence；Wherein, selecting is to screen current year drying radix pseudostellariae, and the radix pseudostellariae for going mouldy or have impurity is rejected；It goes to refer to
Radix pseudostellariae cercus is removed and is separated using mechanical equipment；Baking refers to that vacuumize baking technology using low temperature removes again
Radix pseudostellariae surface moisture be convenient for subsequent slice, 50 DEG C of baked temperature, baking time 15mim, vacuum pressure 0.04MPa；Slice
Refer to the slice that the radix pseudostellariae after baking is carried out to radix pseudostellariae ginseng body using Chinese herbal medicine slicer, the radix pseudostellariae piece thickness after slice
For 0.8mm；Steaming is that radix pseudostellariae piece is placed in food steamer to handle, and steams and is heated using vapor, steaming time 25min；
S2, double sections of Steam explosion treatments: using the radix pseudostellariae after cutting off as blasting substrates, successively pass through Steam explosion treatment I
With Steam explosion treatment II, double sections of Steam explosion treatment interval times are 3min；The condition of Steam explosion treatment I are as follows: explosion chamber
Coefficient is 0.8, and explosion steam pressure reaches 0.6MPa, and explosion pressure maintaining handles the time as 12min, and blasting time is not higher than
0.00875s；The condition of Steam explosion treatment II are as follows: the same cavity explosion treatment of blasting gear, explosion steam pressure reach on the same stage
2.0MPa, explosion pressure maintaining handle the time as 40s, and blasting time is not higher than 0.00875s；It is equal during double sections of Steam explosion treatments
Entrainer is added, entrainer is detailed catalogue diamond dust and Ca (OH)2The compound of powder, diamond dust: Ca (OH)2The mass values of powder are
1:1；By percentage to the quality, entrainer total addition level accounts for the 2% of blasting substrates, and is added batch-wise, Steam explosion treatment I addition
The 1/3 of total amount, Steam explosion treatment II add the entrainer of surplus；Radix pseudostellariae matrix photo after explosion treatment is shown in Fig. 1；
S3, biological enzyme enzymatic hydrolysis: by after explosion treatment and when temperature is down to room temperature radix pseudostellariae material matrix and water with solid-liquid
It is mixed than 1kg:2L, the pH value of solidliquid mixture is adjusted to 5.0, be then added at one time nonionic surfactant, then plus
Enter cellulase, zytase and pectase to be digested, 50 DEG C of hydrolysis temperature, enzymolysis time 45min, 25min before digesting
Stage is at the uniform velocity stirred (revolving speed 110rpm/min), wait digest at the end of adjust the pH value of mixture to neutrality；Wherein, with every
The drying radix pseudostellariae piece meter of g (the radix pseudostellariae piece after drying radix pseudostellariae piece, that is, S1 slice, before steaming), cellulase, zytase, fruit
The additive amount of glue enzyme and nonionic surfactant is respectively as follows: 12FPU/g, 130U/g, 100U/g, 0.02g/g；The nonionic
Surfactant is the mixture of the quality such as Berol, Tween-80 and BSA；
S4, water hot extraction: it is dosed in water hot extraction's tank after the radix pseudostellariae matrix after explosion treatment is collected, hot water in tank
The mass values of amount and radix pseudostellariae matrix are 18:1, extract 95 DEG C of hot water temperature, extraction time 2.5h, extraction times 1 time；Extracting
Take at the uniform velocity stirred (revolving speed 100rpm/min) early period, it is to be extracted to stop stirring when carrying out to 3/5 extraction time；
S5, extract liquor CO2Processing: after to water hot extraction, obtained extract liquor is cooled to first with heat exchanger
Room temperature then moves in clean rustless steel container, sterile CO is then passed through into extract liquor after cooling2Gas, CO2Flow velocity is
13m3/ min, is passed through CO2Gas time 10min；It is passed through CO2When gas, CO2Gas of the gas by pipeline through rustless steel container bottom
Body distributor enters inside extract liquor；
S6, three-stage filtration: three-stage filtration is carried out using self-control three-level filter system, as shown in Fig. 2, the three-level filter system
Including GF- divergence type tube centrifuge 1, centrifugation liquid storage tank 2(tank in temperature controlling range be 5~10 DEG C), power transmitting assembly
I, power transmitting assembly II, power transmitting assembly III, grade one filter 5, secondary filter 6, tertiary filter and its external world are attached
Category system；
Power transmitting assembly I is connected in series by kinetic pump I 31 and check-valves I 41；Power transmitting assembly II is by kinetic pump
II 32 and check-valves II 42 are connected in series；Power transmitting assembly III by kinetic pump III 33 and check-valves III 43 series winding and
At；
Grade one filter 5 and secondary filter 6 are conventional cartridge filter；Tertiary filter is self-control filter, knot
Structure includes cylinder 7, doughnut tread assembly, pedestal 13；7 bottom and top of cylinder are respectively equipped with inlet 8 and liquid outlet 9, cylinder
Interlayer 10 is equipped with outside body 7, the upper and lower ends of interlayer 10 are respectively equipped with interlayer import 11 and interlayer outlet 12；Hollow fiber bundle group
Part includes being evenly equipped with porous package shell 14, quantity 600, molecular cut off for the doughnut 15 of 10000 dalton, this
A little doughnuts 15 merge bunchy and are placed in inside package shell 14；Pedestal 13 be cylindrical body, cylindrical body upper section be it is hollow be cylindrical in shape,
Middle and lower sections are solid, and the middle and lower sections of pedestal 13 are solid to be equipped with through-hole compatible with 15 quantity of doughnut and its size；Pedestal
13 are located at 9 lower section of liquid outlet, are close to 7 roof of cylinder and are firmly connected with it；The upper end of doughnut 15 is open and is threaded through base
In the through-hole of seat 13, lower end closed is simultaneously fixedly connected with 14 bottom wall of package shell；
The extraneous subsystem of tertiary filter includes kinetic pump IV 34, check-valves IV 44, constant temperature refrigeration water tank 16, folder
Successively contact check-valves IV 44, constant temperature refrigeration water tank 16 (controllable temperature range are as follows: 5~15 DEG C) and kinetic pump IV 34 for layer outlet 12
A closed cycle system is formed to interlayer import 11；
Tube centrifuge 1 is successively contacted by pipeline and is centrifuged liquid storage tank 2, kinetic pump I 31, check-valves I 41, by-pass filtration
Device 5, kinetic pump II 32, check-valves II 42, secondary filter 6, kinetic pump III 33, check-valves III 43 to tertiary filter
Inlet 8；Wherein, be centrifuged between liquid storage tank 2 and kinetic pump I 31, between check-valves I 41 and grade one filter 5, level-one mistake
Between filter 5 and kinetic pump II 32, between check-valves II 42 and secondary filter 6, secondary filter 6 and kinetic pump III 33
Between, the pipeline between check-valves III 43 and tertiary filter take clamp connection；
Aforementioned grade one filter 5 and secondary filter 6 pass through commercially available acquisition, the filter of grade one filter 5 and secondary filter 6
Core is folding type filter element, grade one filter 5 and be respectively 5 and 7, by-pass filtration with the filter core number of secondary filter 6
The filter core aperture of device 5 and secondary filter 6 is respectively 5 μm, 0.22 μm；The filter core material of grade one filter 5 and secondary filter 6
For polypropylene, frame of filter element (support frame) is rigid plastics, filter core can compression resistance be 0.4 MPa；
Three-stage filtration step are as follows:
(a) in extract liquor input 1 inner cavity of tube centrifuge first obtained S5, start the equipment and carry out centrifugal work,
Centrifugal rotational speed reaches 5000rpm/min, is centrifuged 30min；The centrifugal clear liquid that will acquire in time after centrifugation is transferred to centrifugate and stores up
In tank 2, and temperature controlling range is 10 DEG C in the tank；
(b) the cooling centrifugate that upper process obtains is crossed check-valves I 41 through pipeline and is delivered to level-one by starting kinetic pump I 31
In filter 5,0.2 Mpa of input pressure realizes first time coarse filtration；
(c) the by-pass filtration liquid obtained after grade one filter 5 is crossed check-valves II through pipeline by starting kinetic pump II 32
42 are delivered in secondary filter 6,0.2 Mpa of input pressure, realize second of coarse filtration；
(d) start kinetic pump IV 34, by temperature obtained in constant temperature refrigeration water tank 16 be 5 DEG C cold water through pipeline from
Interlayer import 11 enters in interlayer 10, and crosses check-valves IV 44 through pipeline by interlayer outlet 12 and be recycled to constant temperature refrigeration water tank
In 16；Restart the second level mistake that kinetic pump III 33 will be obtained after secondary filter 6 when 7 inner cavity temperature of cylinder reaches 5 DEG C
Filtrate is crossed check-valves III 43 through pipeline and is delivered in tertiary filter by inlet 8,0.2 Mpa of input pressure, secondary filtration
Liquid elder generation is inside the porous entrance package shell 14 on package shell 14, due to the crown_interception of doughnut 15, secondary filtration
Impurity in liquid is blocked in the outside of doughnut 15, and extract liquor then pass through doughnut 15 and from 15 top opening of doughnut into
Enter pedestal 13, is then come out from liquid outlet 9；
(e) device is counter cleans: at the end of work to be filtered, can carry out the reverse cleaning operation of the equipment series, i.e., first
Between disassembly centrifugation liquid storage tank 2 and kinetic pump I 31, between check-valves I 41 and grade one filter 5, grade one filter 5 and power
Pump between II 32, between check-valves II 42 and secondary filter 6, between secondary filter 6 and kinetic pump III 33, check-valves
The clip on pipeline between III 43 and tertiary filter, manual 180 ° of integrated regulation power transmitting assemblies I, power transmission group
The direction (original import becomes exporting) of part II, power transmitting assembly III, then pass through the corresponding pipeline of clamp connection, adjustment
Rear state, will be clean pure as shown in figure 3, start above-mentioned kinetic pump I 31, kinetic pump II 32, kinetic pump III 33 simultaneously
Change water to enter in cylinder 7 through 7 liquid outlet 9 of cylinder, then ejected wash water is finally discharged from centrifugation liquid storage tank 2, each filter pressure in operation
Power list index must not be higher than 0.3 MPa, be repeated 2 times；
S7, detoxification: the radix pseudostellariae extract liquor after three-stage filtration is successively passed through into D301 resin packed column and NKAII resin is filled out
Column is filled, extract liquor is 0.15MPa into column pressure, collects extract liquor；
S8, alcohol precipitation: the radix pseudostellariae extract liquor after detoxification is carried out depressurizing half concentration first, concentration pressure is 0.03MPa, dense
Contracting temperature 60 C, concentration time 2.5h；It is cooled to 20 DEG C followed by half concentrate will be depressurized and 2.5 times of volumes is added thereto
95% edible ethanol liquid stands 9h, and it is radix pseudostellariae source polysaccharide that finally centrifugation, which obtains sediment,；Wherein, centrifugal rotational speed is
13000rpm/min, centrifuging temperature temperature control is at 10 DEG C, centrifugation time 20min.
Reference examples 1
Difference from example 1 is that S2: Steam explosion treatment I and II do not add entrainer；Other steps are same
Embodiment 1.
Reference examples 2
Difference from example 1 is that S2: only implementing Steam explosion treatment I, and add the entrainer of full dose；It is other
Step is the same as embodiment 1.
Reference examples 3
Difference from example 1 is that S2: only implementing Steam explosion treatment II, and add the entrainer of full dose；Its
Its step is the same as embodiment 1.
Reference examples 4
Difference from example 1 is that omitting S3, i.e., biological enzyme is not added and is digested；Other same embodiments of step
1。
Reference examples 5
Difference from example 1 is that S3: only adding cellulase by the additive amount of cellulase；Other steps are same
Embodiment 1.
Reference examples 6
Difference from example 1 is that S3: only adding zytase by the additive amount of zytase；Other steps are same
Embodiment 1.
Reference examples 7
Difference from example 1 is that S3: only adding pectase by the additive amount of pectase；Other steps are the same as implementation
Example 1.
With polysaccharide extraction yield=(quality of the radix pseudostellariae source polysaccharide prepared/drying radix pseudostellariae piece quality) × 100%
It counts, the radix pseudostellariae piece after drying radix pseudostellariae piece therein, that is, S1 slice, before steaming, to 1 ~ 7 gained crown prince of embodiment 1 and reference examples
The extraction yield of ginseng source polysaccharide, which counts, to be calculated, the result is as follows:
As can be seen from the above table:
(1), compared with Example 1, the polysaccharide extraction yield of reference examples 1 is significantly lower than the polysaccharide extraction yield of embodiment 1, explanation
" addition entrainer " is remarkably improved the extraction yield of radix pseudostellariae source polysaccharide compared with " not adding entrainer "；
(2), compared with Example 1, the polysaccharide extraction yield of reference examples 2 and 3 is significantly lower than the polysaccharide extraction yield of embodiment 1,
Illustrate that " two section type steam blasting " is remarkably improved the extraction yield of radix pseudostellariae source polysaccharide compared with " one-part form steam blasting "；
(3), compared with reference examples 4, the polysaccharide extraction yield of embodiment 1 and reference examples 5 ~ 7 is apparently higher than the more of reference examples 4
Sugared extraction yield, " addition biological enzyme " it is more compared with " not adding biological enzyme " can to mention significantly high radix pseudostellariae source after illustrating two section type steam blasting
The extraction yield of sugar；Meanwhile compared with Example 1, the polysaccharide extraction yield of reference examples 5 ~ 7 is significantly lower than the polysaccharide extraction of embodiment 1 again
Rate is taken, illustrates that the compound use of three kinds of enzymes, more single enzyme can more improve the extraction yield of radix pseudostellariae source polysaccharide.
To sum up, the present invention uses two section type steam blasting, and entrainer is added during its, while two section type steam is quick-fried
Biological enzyme enzymatic hydrolysis is added after broken, the polysaccharide extraction yield of radix pseudostellariae can be made to be improved to the greatest extent.
Claims (6)
1. a kind of method that steam explosion combination biological enzyme technology prepares radix pseudostellariae source polysaccharide, which is characterized in that steps are as follows:
S1, radix pseudostellariae pretreatment: by drying radix pseudostellariae successively after select, go must, bake, be sliced and steam five processes；
S2, double sections of Steam explosion treatments: using the radix pseudostellariae piece after steaming as blasting substrates, successively by Steam explosion treatment I and
Steam explosion treatment II, double sections of Steam explosion treatment interval times are 2 ~ 5min；The condition of Steam explosion treatment I are as follows: explosion chamber
Coefficient is 0.7 ~ 0.9, and for explosion steam pressure up to 0.5 ~ 0.8MPa, it is 10 ~ 15min that explosion pressure maintaining, which handles the time, when explosion
Between be not higher than 0.00875s；The condition of Steam explosion treatment II are as follows: the same cavity explosion treatment of blasting gear on the same stage, explosion steam
Pressure is up to 1.5 ~ 2.2MPa, and explosion pressure maintaining handles the time as 30 ~ 50s, and blasting time is not higher than 0.00875s；Double sections of steam blastings
Entrainer is added in treatment process, entrainer is detailed catalogue diamond dust and Ca (OH)2The compound of powder, diamond dust: Ca (OH)2Powder
Mass values be 4:1 ~ 1:1；By percentage to the quality, entrainer total addition level accounts for the 1.5 ~ 3% of blasting substrates, and adds in batches
Add, the 1/3 ~ 2/5 of Steam explosion treatment I total amount of adding, Steam explosion treatment II adds the entrainer of surplus；
S3, biological enzyme enzymatic hydrolysis: by after explosion treatment and when temperature is down to room temperature radix pseudostellariae material matrix and water with solid-to-liquid ratio
1kg:1L ~ 1kg:3L mixing, is adjusted to 4.5 ~ 5.0 for the pH value of solidliquid mixture, is then added at one time auxiliary agent, adds fibre
It ties up plain enzyme, zytase and pectase to be digested, 50 ~ 55 DEG C of hydrolysis temperature, 30 ~ 45min of enzymolysis time, enzymatic hydrolysis preceding 20 ~
The stage of 25min is at the uniform velocity stirred, wait digest at the end of adjust the pH value of mixture to neutrality；Wherein, with every gram it is drying too
Son ginseng piece meter, cellulase, zytase, pectase and auxiliary agent additive amount be respectively as follows: 10 ~ 15FPU, 100 ~ 150U, 80 ~
110U,0.003~0.05g；The auxiliary agent is one of nonionic surfactant, BSA or a variety of, the surfactant
For one of Berol, PEG, Tween-80 or a variety of；
S4, water hot extraction: the radix pseudostellariae matrix after biological enzyme is digested is dosed in water hot extraction's tank after collecting, hot water amount in tank
Mass values with radix pseudostellariae matrix are 15:1 ~ 20:1, extract 90 ~ 100 DEG C of hot water temperature, 2 ~ 3h of extraction time, extraction times 1
It is secondary；The phase is at the uniform velocity stirred before extraction, to be extracted to stop stirring when carrying out to 3/5 extraction time；
S5, extract liquor CO2Processing: after to water hot extraction, obtained extract liquor being cooled to room temperature, and then moves to cleaning not
It becomes rusty in steel container, sterile CO is then passed through into extract liquor after cooling2Gas, CO2Flow velocity is 10 ~ 15m3/ min, is passed through CO2
5 ~ 15min of gas time；
S6, three-stage filtration: extract liquor CO2Pass through grade one filter, secondary filter and the three-level mistake of tandem compound after processing respectively
Filter realizes filtration operation；Wherein, grade one filter and secondary filter are conventional cartridge filter, grade one filter and
The filter core aperture of secondary filter is respectively 4.5 ~ 5 μm, 0.2 ~ 0.25 μm；Tertiary filter is hollow fiber filter, hollow
The molecular cut off of fiber is 10000 ~ 30000 dalton；
S7, detoxification: the radix pseudostellariae extract liquor after three-stage filtration is successively passed through into D301 resin packed column and NKAII resin is filled
Column, extract liquor are 0.15 ~ 0.2MPa into column pressure, collect extract liquor；
S8, alcohol precipitation: carrying out the radix pseudostellariae extract liquor after detoxification to depressurize half concentration first, and concentration pressure is 0.01 ~ 0.05MPa,
50 ~ 70 DEG C of thickening temperature, 2 ~ 3h of concentration time；10 ~ 25 DEG C and thereto addition 2 ~ 3 are cooled to followed by half concentrate will be depressurized
95% edible ethanol liquid of times volume stands 8 ~ 10h, and it is radix pseudostellariae source polysaccharide that finally centrifugation, which obtains sediment,.
2. preparation method as described in claim 1, it is characterised in that: carry out three-level mistake using self-control three-level filter system in S6
Filter, the three-level filter system include tube centrifuge, centrifugation liquid storage tank, power transmitting assembly I, power transmitting assembly II, power
Transmission assembly III, grade one filter, secondary filter, tertiary filter and its extraneous subsystem；Power transmitting assembly I by
Kinetic pump I and check-valves I are connected in series；Power transmitting assembly II is connected in series by kinetic pump II and check-valves II；Power transmission
Component III is connected in series by kinetic pump III and check-valves III；Grade one filter and secondary filter are conventional cartridge filter；
Tertiary filter is self-control filter, and structure includes cylinder, doughnut tread assembly, pedestal；Cylinder body bottom and top difference
Equipped with inlet and liquid outlet, interlayer is equipped with outside cylinder, the upper and lower ends of interlayer are respectively equipped with interlayer import and interlayer outlet；
Doughnut tread assembly includes being evenly equipped with porous package shell, several doughnuts, these doughnuts merge bunchy and set
Inside package shell；Pedestal is cylindrical body, cylindrical body upper section be it is hollow be cylindrical in shape, middle and lower sections it is solid, the middle and lower sections of pedestal are real
It is equipped with through-hole compatible with doughnut quantity and its size in the heart；Pedestal is located at below liquid outlet, is close to cylinder roof simultaneously
It is firmly connected with it；The upper end of doughnut is open to be simultaneously threaded through in the through-hole of pedestal, lower end closed and with package shell bottom wall
It is fixedly connected；The extraneous subsystem of tertiary filter includes kinetic pump IV, check-valves IV, constant temperature refrigeration water tank, interlayer outlet
Successively contact check-valves IV, constant temperature refrigeration water tank and kinetic pump IV to interlayer import forms a closed cycle system；Tubular type centrifugation
Machine is successively contacted by pipeline and is centrifuged liquid storage tank, kinetic pump I, check-valves I, grade one filter, kinetic pump II, check-valves II, two
The inlet of grade filter, kinetic pump III, check-valves III to tertiary filter；Grade one filter and filter with secondary filter
Core bore diameter is respectively 4.5 ~ 5 μm, 0.2 ~ 0.22 μm；The molecular cut off of doughnut is 10000 ~ 30000 dalton；
Three-stage filtration step are as follows:
(a) start the equipment by S5 treated extract liquor input tube centrifuge inner cavity first and carry out centrifugal work, centrifugation
4000 ~ 6000rpm of turn up is centrifuged 20 ~ 30min；The centrifugal clear liquid that will acquire in time after centrifugation is transferred to centrifugate and stores up
In tank, and temperature controlling range is 5 ~ 10 DEG C in the tank；
(b) the cooling centrifugate that upper process obtains is crossed check-valves I by the road and is delivered in grade one filter by starting kinetic pump I,
0.2 ~ 0.6 MPa of input pressure realizes first time coarse filtration；
(c) the by-pass filtration liquid obtained after grade one filter is crossed check-valves II by the road and is delivered to second level by starting kinetic pump II
In filter, 0.2 ~ 0.6 MPa of input pressure realizes second of coarse filtration；
(d) start kinetic pump IV, by temperature obtained in constant temperature refrigeration water tank be 5 ~ 15 DEG C cold water by the road from interlayer into
Mouth enters in interlayer, and crosses check-valves IV by the road by interlayer outlet and be recycled in constant temperature refrigeration water tank；To cylinder lumen temperature
Degree restarts kinetic pump III and the secondary filtration liquid obtained after secondary filter is crossed check-valves by the road when reaching 5 ~ 15 DEG C
III is delivered in tertiary filter by inlet, 0.2 ~ 0.6 MPa of input pressure, and secondary filtration liquid is first from package shell
Porous to enter inside package shell, due to the crown_interception of doughnut, the impurity in secondary filtration liquid is blocked in doughnut
Outside, and extract liquor then passes through doughnut and enters pedestal from doughnut top opening, then comes out from liquid outlet.
3. preparation method as claimed in claim 2, which is characterized in that S6 further includes that step (e) is instead cleaned: work knot to be filtered
Shu Shi carries out the reverse cleaning operation of the system, manual 180 ° of integrated regulation power transmitting assemblies I, power transmitting assembly II, moves
The direction of power transmission assembly III, that is, original import becomes exporting, and reconnects corresponding pipeline, at the same start above-mentioned kinetic pump I,
Kinetic pump II, kinetic pump III enter clean purified water in cylinder through barrel liquid discharge mouth, then ejected wash water is finally from centrifugate
Storage tank is discharged, and each filter pressure list index must not be higher than 0.3 MPa in operation, repeats 2 ~ 3 times.
4. preparation method as claimed in claim 2, it is characterised in that: centrifugation liquid storage tank and kinetic pump I between, check-valves I with
Between grade one filter, between grade one filter and kinetic pump II, between check-valves II and secondary filter, secondary filter with
Pipeline between kinetic pump III, between check-valves III and tertiary filter takes movable connection method.
5. preparation method as claimed in claim 4, it is characterised in that: the movable connection method is clamp connection.
6. preparation method as claimed in claim 2, it is characterised in that: tube centrifuge is GF- divergence type.
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