CN110240625A - A kind of separation method and foam separator of quinoa saponin(e - Google Patents
A kind of separation method and foam separator of quinoa saponin(e Download PDFInfo
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- CN110240625A CN110240625A CN201910537739.9A CN201910537739A CN110240625A CN 110240625 A CN110240625 A CN 110240625A CN 201910537739 A CN201910537739 A CN 201910537739A CN 110240625 A CN110240625 A CN 110240625A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0005—Degasification of liquids with one or more auxiliary substances
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
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Abstract
The invention discloses a kind of separation methods of quinoa saponin(e, are related to chemical technology field.The method of the present invention is to carry out separation and Extraction to quinoa saponin(e using foam separating technology；Concentration of raw material is 0.1324-5.296mg/mL in the foam separating technology, and temperature is 15-25 DEG C, venting flow rate 20-40mL/min, volume of the raw material liquid 150-250mL.Most preferably concentration of raw material is 0.5296mg/mL, and temperature is 25 DEG C, venting flow rate 22mL/min, volume of the raw material liquid 250mL.In foam fraction factor of the present invention, quinoa saponin(e concentration ratio 2.0-2.6, rate of recovery 42%-52%.The method of the present invention has the advantages that environmentally protective, equipment is simple, easy to operate, operating cost is low etc., can promote the use of.
Description
Technical field
The present invention relates to chemical technology field more particularly to a kind of separation methods and foam separator of quinoa saponin(e.
Background technique
Quinoa (scientific name: Chenopodium quinoa Willd), originates in South America andes region, is print plus original inhabitants
The main conventional food of resident has 5000-7000 more years edible and plantation history, with unique nutritive value.Quinoa
Seed color mainly has several cie system of color representation cie such as white, black, red, and nutritional ingredient is not much different, wherein white mouthfeel is best, it is black, red
Mouthfeel relative mistake is a little, and seed is also smaller.Quinoa is divided into sweet tea quinoa and bitter quinoa by saponin content；Quinoa contains protein and human body
Necessary a variety of amino acid are free of seitan, are rich in B family vitamin and microelement, belong to basic food, however it has one
The defect for needing improve the day after tomorrow contains quinoa saponin(e.
Saponin(e is one layer of protective substance outside quinoa seed, and main anti-nutrient substance in saponin(e or quinoa can hinder
Hinder the absorption of certain nutrients, bitter has micro- poison.Therefore, it needs to remove wherein saponin(e before edible quinoa.
The extraction and purification process of traditional saponin(e mainly uses organic solvent to extract, macroporous absorbent resin separation and purification, but deposits
In poor selectivity, the disadvantages of organic solvent consumption is big, and environmental pollution is more serious, higher cost.
Summary of the invention
In view of this, the embodiment of the invention provides the separation methods and foam separator of a kind of quinoa saponin(e, mainly
Purpose be solve the problems, such as separation quinoa saponin(e pollute it is big, at high cost and not easy to operate.
In order to achieve the above objectives, invention broadly provides following technical solutions:
On the one hand, the embodiment of the invention provides a kind of separation method of quinoa saponin(e, the method is using foam point
Separation and Extraction is carried out to quinoa saponin(e from technology；Wherein, the concentration of material liquid is 0.4413- in the foam separating technology
0.6620mg/mL, temperature are 15-25 DEG C, venting flow rate 20-40mL/min, volume of the raw material liquid 150-250mL.
Preferably, the concentration of material liquid is 0.4815-0.5884mg/mL, temperature 20- in the foam separating technology
25 DEG C, venting flow rate 20-35mL/min, volume of the raw material liquid 200-250mL.
Preferably, the concentration of material liquid is 0.4815-0.5296mg/mL, temperature 21- in the foam separating technology
25 DEG C, venting flow rate 20-30mL/min, volume of the raw material liquid 210-250mL.
Preferably, the concentration of material liquid is 0.4996-0.5296mg/mL, temperature 22- in the foam separating technology
25 DEG C, venting flow rate 21-25mL/min, volume of the raw material liquid 220-250mL.
Preferably, the concentration of material liquid is 0.5092-0.5296mg/mL, temperature 23- in the foam separating technology
25 DEG C, venting flow rate 21-23mL/min, volume of the raw material liquid 230-250mL.
Preferably, the concentration of material liquid is 0.5192-0.5296mg/mL, temperature 24- in the foam separating technology
25 DEG C, venting flow rate 21-22mL/min, volume of the raw material liquid 240-250mL.
Preferably, the concentration of material liquid is 0.5296mg/mL in the foam separating technology, temperature is 25 DEG C, ventilation
Flow velocity 22mL/min, volume of the raw material liquid 250mL.
Preferably, quinoa saponin(e concentration ratio is 2.0-2.6, rate of recovery 42%- in the foam separating technology
52%.
Preferably, the pH value of the material liquid is 3-5；The kind of the quinoa is green Chenopodiaceae No.1.
Preferably, the pH value of the material liquid is 5.
On the other hand, the embodiment of the invention provides a kind of foam separators, comprising:
On the one hand, the embodiment of the invention provides a kind of foam separators, comprising:
Foam fraction factor unit is made of foam separating tower and recirculated water jacketed pipe, and the foam separating tower is set to described
The inside of recirculated water jacketed pipe is formed between the outer wall of the foam separating tower and the inner wall of the recirculated water jacketed pipe for holding
Receive the cavity of recirculated water；The foam separating tower be used for by quinoa saponin(e crude extract foam and solution separate；It is described to follow
The top of ring water leg pipe is equipped with recirculated water water outlet, and lower part is equipped with recirculated water water inlet；It is set at the top of the foam separating tower
There is foam outlet, bottom is equipped with air inlet；
It supplies gas unit, hose connection is passed sequentially through by air compressor, gas safety bottle and gas flowmeter and is formed, institute
State the air inlet that gas flowmeter is connected to the foam separating tower by hose；
Water unit is recycled, the water outlet of the circulation water unit and the recirculated water water inlet of the recirculated water jacketed pipe connect
Logical, the recirculated water water outlet of the recirculated water jacketed pipe is connected to the water inlet of the circulation water unit, the circulation water unit
Water bath with thermostatic control is provided for the foam separating tower；
Foam collector unit is made of collection elbow and collection vessel；Under use state, described one end for collecting elbow
It is inserted into the foam outlet of the foam fraction factor top of tower and forms close connection, the collection vessel is isolated for collecting to accommodate
Foam；
Separating liquid extracts unit out, is made of oilless vacuum pump and liquid safe bottle；Under use state, the liquid safe
Bottle is inserted into the inside of the foam separating tower, the foam point by hose from the foam outlet of the foam fraction factor top of tower
It is drawn in liquid safe bottle from the separating liquid in tower.
Preferably, the collection elbow is made of inner and outer tubes, outer tube is set to the outside of said inner tube, outer tube with it is interior
It forms cavity, inner tube and outer tube between pipe to be closed at two ports for collecting elbow, the foam of foam fraction factor tower top is from described
It collects and is flowed out in the inner tube of elbow.
Preferably, the first bending place angle for collecting elbow is 90 °, the second bending place folder for collecting elbow
Angle is 90 °.
Preferably, at the blow vent of the foam fraction factor tower bottom be equipped with gas distribution grid, be aperture be 30 microns
Micropore sand core filter plate, is made of sintered frit.
Preferably, the exit diameter for collecting elbow is 20mm, the diameter of the recirculated water jacketed pipe is 60mm,
The diameter of the foam separating tower is 40mm；Valve is equipped at the blow vent；The collection elbow, shown foam separating tower,
The material of the recirculated water jacketed pipe is glass.
Compared with prior art, the beneficial effects of the present invention are:
The present invention is that the separation and purification of saponin(e introduces foam separating technology, simple using the environmentally protective, equipment of the technology,
Easy to operate, operating cost is low and the features such as particularly suitable for processing low concentration medical fluid, in triterpenoid saponin separation and purification process aspect
It is bold in innovation and is attempted；The present invention by investigate different air velocities, feedstock quality concentration, liquid level, temperature etc. because
Influence of the element to quinoa saponin(e foam fraction factor process, and by response surface experiments design optimization foam fraction factor process conditions, to open
The process for cleanly preparing for sending out quinoa saponin(e provides theoretical foundation.
Detailed description of the invention
Fig. 1 is quinoa saponin A chemical molecular structural formula provided in an embodiment of the present invention；
Fig. 2 is material solution extension rate provided in an embodiment of the present invention to quinoa saponin(e foam fraction factor influential effect curve
Figure；
Fig. 3 is temperature provided in an embodiment of the present invention to quinoa saponin(e foam fraction factor influential effect curve graph；
Fig. 4 is gas flow provided in an embodiment of the present invention to quinoa saponin(e foam fraction factor influential effect curve graph；
Fig. 5 is different liquids volume provided in an embodiment of the present invention to quinoa saponin(e foam fraction factor influential effect curve graph；
Fig. 6 is difference pH provided in an embodiment of the present invention to quinoa saponin(e foam fraction factor influential effect curve graph；
Fig. 7 is foam separator structural schematic diagram provided in an embodiment of the present invention；
Fig. 8 is foam fraction factor cellular construction schematic diagram provided in an embodiment of the present invention；
Fig. 9 is collection elbow structure schematic diagram provided in an embodiment of the present invention；
Figure 10 is separating liquid extraction cell schematics provided in an embodiment of the present invention.
Appended drawing reference:
1 foam fraction factor unit, 101 foam separating towers, 102 circulation water legs, 103 recirculated water water inlets, 104 recirculated waters go out
The mouth of a river, 105 foam outlets, 106 air inlets, 107 gas distribution grids；
2 supply gas unit, 201 air compressors, 202 gas safety bottles, 203 gas flowmeters；
3 circulation water units, 301 water outlets, 302 water inlets；
4 foam collector units, 401 collect elbow, 402 collection vessels；
5 separating liquids extract unit, 501 oilless vacuum pumps, 502 liquid safe bottles out.
Specific embodiment
For further illustrate the present invention to reach the technical means and efficacy that predetermined goal of the invention is taken, below with compared with
Good embodiment, to specific embodiment, technical solution, feature and its effect applied according to the present invention, detailed description is as follows.Under
Stating the special characteristic, structure or feature in multiple embodiments in bright can be combined by any suitable form.
Embodiment 1
Material and reagent:
Quinoa originates from Qinghai Province Hai Xizhou Dulan County 3200 m Above Sea-level, green Chenopodiaceae No.1, by the farsighted bright and beautiful standing grain ecology agriculture and animal husbandry in Qinghai
Science and Technology Ltd. provides；Quinoa saponin A reference substance (content >=98%), by the limited public affairs of the farsighted bright and beautiful standing grain ecology agriculture and animal husbandry science and technology in Qinghai
Department's self-control；Perchloric acid (analysis is pure), vanillic aldehyde (analysis is pure), glacial acetic acid (analysis is pure), ethyl alcohol (analysis is pure), experimental water is to go
Ionized water.
Instrument and equipment:
752 type ultraviolet-uisible spectrophotometers (Shanghai Sunny Hengping Scientific Instrument Co., Ltd.),
RE-52AA Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant),
JP-030S supersonic wave cleaning machine (Jie Meng cleaning equipment Co., Ltd, Shenzhen),
FA2004 assay balance (Shanghai Sunny Hengping Scientific Instrument Co., Ltd.),
101-1S electric drying oven with forced convection (western instrument science and technology (Shanghai) Co., Ltd., nation),
HH-2 water-bath (Changzhou Zhi Borui instrument manufacturing Co., Ltd),
Foam separator can be selected the embodiment of the present invention 2 and make separation equipment (effect is more excellent) by oneself, existing set can also be used
It is standby.
LZB-FB glass rotameter (Suzhou chemical instruments Co., Ltd),
OTS-1500 oil-free air compressor (Taizhou plain Austria dash forward this Trade Co., Ltd.),
HH-501 thermostatic water-circulator bath (Jintan City city east Xin Rui instrument plant).
Experimental method:
(1) draw quinoa saponin(e standard curve: the saponin(e in quinoa seed is triterpenoid saponin, is not having quinoa saponin(e in the past
It is reference substance that oleanolic acid is usually selected in the case where reference substance, but quinoa saponin(e containing aglycone molecular weight because generally existing
700 or more, and oleanolic acid is 456.71 without aglycone molecular weight, therefore laboratory is prepared by high-efficient liquid phase chromatogram purification
Quinoa saponin A, molecular structure is as follows, molecular weight 810.44, and establish content assaying method using quinoa saponin A as reference substance.
Quinoa saponin A reference substance 6.60mg is accurately weighed, sets in 25mL measuring bottle plus methanol dissolves and be diluted to scale, be made
The Standard Stock solutions of 0.264mg/mL.
Accurate each 0,400,600,800,1000,1200, the 1400 μ L of quinoa saponin A Standard Stock solutions that measures is set respectively
In dry tool plug test tube, 60 DEG C are evaporated, and taking-up is let cool, and sequentially add 5% vanillic aldehyde glacial acetic acid solution 0.2mL and perchloric acid
0.8mL shakes up, and keeps the temperature 15min in 60 DEG C of water-baths, takes out, and with the cooling 10min of ice-water bath, 4mL glacial acetic acid is added, shakes up.Choosing
The standard solution for taking 800 μ L of quinoa saponin A, is scanned in 400~760nm range, selectes a length of measurement wave of maximum absorption wave
It is long；The absorbance A of each standard solution is measured in maximum absorption wave strong point, using absorbance A as ordinate, with corresponding reference substance concentration
(mg/mL) it is abscissa, draws standard curve, obtain regression equation are as follows: Y=10.206X-0.0236, r=0.9994, linear model
It encloses: 0.02112~0.07392mg/mL.
(2) it prepares sample solution: taking quinoa kind skin powder, weigh 25g, add water 250mL, ultrasonic wave extraction 1h, stand 2h,
It takes supernatant liquid filtering again after taking upper solution to be centrifuged, sample solution is made (medical fluid contains crude drug 0.1g/mL).
(3) it is added the diluted sample solution of different multiples as material liquid in foam separator, then ventilates from tower bottom,
Obtained foam is enriched with to be discharged by tower top, and the Liquid Residue after foam fraction factor is then discharged by tower bottom；Material liquid, bubble are measured respectively
Quinoa saponin(e in foam liquid and Liquid Residue calculates the rate of recovery, concentration ratio to filter out the best foam fraction factor technique of quinoa total saposins
Condition.
(4) foam fraction factor effect evaluation index: is evaluated with the rate of recovery, concentration ratio
In the rate of recovery/%=foam solution in gross mass/material liquid of quinoa saponin(e quinoa saponin(e gross mass × 100%；
In concentration ratio=foam solution in mass concentration/material liquid of quinoa saponin(e quinoa saponin(e mass concentration.
(5) foamet purifies quinoa saponin(e single factor experiment: respectively with initial concentration, temperature, air velocity, loading
Liquid volume, pH value and ionic strength are that single factor test carries out single factor experiment, investigate each single factor test and purify Chenopodiaceae to foamet
The influence of wheat saponin(e effect, is repeated 3 times.
(6) response surface experiments design: according to Box-Behnken principle design experiment, adopting on the basis of single factor experiment
It is further tested with the horizontal Response surface methodology of four factor three；Select extension rate, temperature, gas flow, liquid volume 4
A factor is independent variable, using the quinoa saponin(e rate of recovery and concentration ratio as response, determines that this 4 independents variable recycle quinoa saponin(e
The influence of rate and concentration ratio and optimum process condition combination；Experimental factor and level design are shown in Table 1.
Triterpenoid saponin content is higher in quinoa, and the aqueous solution foaming characteristic after extraction is good, due to quinoa saponin compound molecule
Aqueous solution slant acidity is caused containing carboxyl and hydroxyl in structure, pH value is 5.0 or so, it is contemplated that pH value of solution is to bubble when practical operation
The influence of foam separating resulting and adjusting solution ph need to use acid-base material easily entrain the reasons such as impurity, final to choose dilution again
4 number, temperature, gas flow, liquid volume factors carry out response surface experiments.
Table 1.Box-Behnken experimental design factor and level
As a result with analysis-single factor experiment result:
(1) it influence of the material solution extension rate to saponin(e foam fraction factor effect: on same foam separator, is added
The sample solution 200ml of different extension rates, is carried out under conditions of flotation throughput 30mL/min intermittent by 20 DEG C of flotation temperature
Floating operation, until the volume of residual solution and foam solution after foam fraction factor is measured there is no flotation is stopped when foam overflow, and
The concentration of quinoa saponin(e in two kinds of solution is measured, influence of the initial concentration to separating effect is investigated.
As shown in Figure 2, quinoa saponin(e concentration ratio increases with the increase of material solution extension rate, and the rate of recovery is molten with sample
The increase of liquid extension rate, which first increases, then to be reduced；With the mass concentration of saponin(e in the increase feed liquid of sample solution extension rate
Reduce, makes the stability reduction of foam, the amount of liquid of foam entrained with is reduced, therefore quinoa saponin(e concentration ratio increases and the rate of recovery
It first increases and reaches maximum when extension rate is 20 times, then as the increase of extension rate is gradually reduced；Comprehensively consider, works as dilution
For multiple at 50 times or so, foam fraction factor effect is preferable.
(2) on same foam separator, 50 times of diluted samples influence of the temperature to quinoa saponin(e foam fraction factor: are added
Product solution 200mL, flotation throughput 30mL/min carry out intermittent floating operation under conditions of different temperatures, until there is no bubbles
Foam stops flotation when overflowing, measure the volume of residual solution and foam solution after foam fraction factor, and measure quinoa in two kinds of solution
The concentration of saponin(e investigates influence of the temperature to separating effect.
As seen from Figure 3, as temperature increases, the quinoa saponin(e rate of recovery is decreased, and concentration ratio but increases with it, and works as temperature
Foam overflow is no longer had when reaching 30 DEG C.In experimentation, the raising of temperature can reduce the surface viscosity of bubble film, reduce
Diffusional resistance, absorption resistance reduce, and adsorbance increases, but surface viscosity is the major influence factors of foam stability, when glutinous
When degree reduces, bubble film is easily thinning, and foam is unstable, is easily broken, and concentration ratio, which increases the rate of recovery simultaneously, to be reduced；The drop of temperature
The low surface viscosity that can make bubble film, which increases the excessive liquid that foam is carried under one's arms, reduces concentration ratio by rate of recovery increase simultaneously, mistake
High or too low temperature is all unfavorable for foam fraction factor operation, only the foam fraction factor effect that can just be got well of proper temperature.It is comprehensive
Consider relationship between operating cost and concentration ratio and the rate of recovery, when material liquid temperature is 20 DEG C or so, separating effect is preferable.
(3) on same foam separator, 50 times of dilutions influence of the gas flow to quinoa saponin(e foam fraction factor: are added
Sample solution 200mL, 20 DEG C of flotation temperature, intermittent floating operation is carried out under conditions of different gas flow, until there is no
Stop flotation when foam overflow, measures the volume of residual solution and foam solution after foam fraction factor, and measure Chenopodiaceae in two kinds of solution
The concentration of wheat saponin(e investigates influence of the gas flow to separating effect.
From fig. 4, it can be seen that quinoa saponin(e concentration ratio reduces with the increase of gas flow, the rate of recovery but increases therewith.It is lower
Gas flow under the conditions of, due to foam reach tower top time it is longer, the foaming water discharge time is longer, the liquid for carrying under one's arms foam
Amount is reduced, and causing concentration ratio to increase the rate of recovery simultaneously reduces；Under higher gas flow, the amount of liquid carried under one's arms in foam increases
Add, making to be adsorbed in the quinoa saponin concentrations in foam reduces, and reduces concentration ratio by the rate of recovery simultaneously and increases.Comprehensively consider, works as gas
Foam fraction factor effect is preferable when body flow is 30mL/min.
(4) on same foam separator, 50 times of dilutions influence of the liquid volume to quinoa saponin(e foam fraction factor: are added
Sample solution 200mL, 20 DEG C of flotation temperature, flotation throughput 30mL/min, interval is carried out under conditions of different liquids volume
Formula floating operation, until the volume of residual solution and foam solution after foam fraction factor is measured there is no flotation is stopped when foam overflow,
And the concentration of quinoa saponin(e in two kinds of solution is measured, investigate influence of the liquid volume to separating effect.
As shown in Figure 5, downward trend after the rate of recovery first rises as the increase of liquid volume is presented, when liquid volume is
The rate of recovery reaches maximum when 300mL, and concentration ratio is on a declining curve with the increase of liquid volume.This is because with liquid bulk
Long-pending increase, become larger corresponding foam fraction factor area of bubbling area reduce, and the liquid carried under one's arms in foam is bloated before not yet reflux,
Therefore increased trend is presented in the rate of recovery before 300mL, since foam is in uphill process after liquid volume is more than 300mL
Extending with the time of contact of liquid makes saponin(e diffuse into the reduction of liquid concentration ratio, although the foam volume of bulging increases and liquid
The incrementss of volume are still in downward trend compared to the rate of recovery.Two indices are comprehensively considered, when the liquid volume of loading is in 200mL
When, foam fraction factor effect is preferable.
(5) on same foam separator, 50 times of diluted samples influence of the pH value to quinoa saponin(e foam fraction factor: are added
Product solution 200mL, is carried out under conditions of different pH value liquid intermittent floating by 20 DEG C of flotation temperature, flotation throughput 30mL/min
Selection operation, until the volume of residual solution and foam solution after foam fraction factor is measured there is no flotation is stopped when foam overflow, and
The concentration of quinoa saponin(e in two kinds of solution is measured, influence of the solution ph to separating effect is investigated.
It will be appreciated from fig. 6 that fluctuation downward trend is presented with the increase of solution ph in the rate of recovery, returned when pH value is 3.0
Yield reaches maximum value 71.7%, and concentration ratio is presented fluctuating change with the increase of solution ph, reaches most when pH value is 5.0
Big value 2.22.It is 5.0 when 50 times of diluted sample solution pH value are unjustified, the rate of recovery is 50.6% under this pH value.It considers
The factors such as operating cost, post-processing and environmental protection, foam fraction factor is not to adjust preferably solution ph.
Response surface experiments result:
(1) response surface experiments design and result: selection extension rate, temperature, gas flow, 4 factors of liquid volume into
Row response surface experiments, response surface Box-Behnken experimental design and the results are shown in Table 2.
Table 2.Box-Behnken experimental design and result
(2) foundation and inspection of regression model: after carrying out multiple regression fitting to 2 test data of table, quinoa saponin(e is obtained
Concentration ratio, the rate of recovery and extension rate, temperature, gas flow, liquid volume regression equation:
Concentration ratio=+ 1.75+0.16*A+0.41*B-0.39*C-0.026*D+0.002250*A*B+
0.018*A*C+0.018*A*D+0.019*B*C+0.087*B*D-0.029*C*D+0.012*A2-0.018*B2-
0.014*C2+0.015*D2；
The rate of recovery=+ 0.53-0.053*A-0.035*B+0.087*C+0.066*D+0.000*A*B-0.004.250 * A*C
+ 0.003750*A*D+0.010*B*C+0.010*B*D+0.018*C*D-0.007458*A2-0.010*B2+ 0.005542*
C2-0.016*D2；
Wherein, A indicates extension rate；B indicates temperature, unit DEG C；C indicates gas flow, Unit/mL/min；D indicates liquid
Body volume, Unit/mL.
Variance analysis is carried out to two regression equations: the results are shown in Table 3, table 4.
The analysis of variance in regression of 3. concentration ratio of table
Note: * significant difference (P < 0.05), the extremely significant difference of * * (P < 0.01).
As shown in Table 3, which reaches extremely significant horizontal (P < 0.01), and the adjustment of model determines coefficients R 2=0.9843,
The model can explain the variation of 98.43% response, correct coefficient of determination R2Adj=0.9674, it is known that regression equation fitting
Degree and confidence level are very high, thus the models fitting degree is relatively good, and test error is small, therefore can be used for pre- in scope of design
It surveys.To the significance analysis of 3 regression model coefficient of table as it can be seen that in first order, A, B, C are extremely significant；BD is significant in interaction item, explanation
There are significant reciprocations between BD.
The analysis of variance in regression of 4. rate of recovery of table
As shown in Table 4, which reaches extremely significant horizontal (P < 0.01), and the adjustment of model determines coefficients R2=0.9720,
The model can explain the variation of 97.20% response, correct coefficient of determination R2 Adj=0.9418, it is known that the regression equation degree of fitting
It is very high with confidence level, thus the models fitting degree is relatively good, test error is small, therefore can be used for the prediction in scope of design.
To the significance analysis of 4 regression model coefficient of table as it can be seen that in first order, A, B, C, D are extremely significant.
By the above experimental data: quinoa saponin(e concentration ratio is with extension rate, the variation meeting of temperature, gas flow
Generate large change；Extension rate is bigger, and temperature is higher, and the smaller quinoa saponin(e concentration ratio of gas flow is higher.Similarly, quinoa soap
The glycosides rate of recovery can generate large change with the variation of extension rate, temperature, gas flow and liquid volume；Extension rate is got over
Small, temperature is lower, and gas flow is bigger, and liquid volume is bigger, and the quinoa saponin(e rate of recovery is higher.
In above-described embodiment, when material liquid extension rate is 40-60 times, being converted into concentration of raw material is 0.4413-
0.6620mg/mL；When extension rate is 45-55 times, concentration of raw material 0.4815-0.5884mg/mL；When extension rate is
At 50-55 times, concentration of raw material 0.4815-0.5296mg/mL；When 50-53 times of extension rate, concentration of raw material is
0.4996-0.5296mg/mL；When extension rate is 50-52, concentration of raw material 0.5092-0.5296mg/mL；Work as dilution
When multiple is 50-51, concentration of raw material 0.5192-0.5296mg/mL；When extension rate is 50 times, concentration of raw material is
0.5296mg/mL。
The present invention obtains foam fraction factor quinoa by Design-Expert software according to the response surface model of above-mentioned establishment
The optimal separation condition (under the premise of establishing maximum concentration ratio, preferably the rate of recovery is larger) of saponin(e saponin(e: extension rate 50.78,
25.00 DEG C of temperature, gas flow 21.73mL/min, liquid volume 250.00mL；Prediction quinoa saponin(e optimal concentration ratio be
2.56, the rate of recovery 45.00%.
The present invention is the optimum process condition that the above-mentioned test of verifying is established, and in conjunction with actual demand, controls (the original of extension rate 50
Feed concentration 0.5296mg/mL), 25 DEG C of temperature, gas flow 22mL/min, liquid volume 250m L；Under the above conditions, it puts down
Row experiment 3 times, obtaining quinoa saponin(e concentration ratio is 2.53, and the rate of recovery 46.08% absolutely proves that above-mentioned test of the invention is excellent
The process conditions of change are reliably feasible, can industrialized production.
The present invention is that the separation and purification of quinoa saponin(e introduces foam separating technology, utilizes environmentally protective, the equipment of the technology
Simply, easy to operate, operating cost is low and the features such as particularly suitable for processing low concentration medical fluid, in triterpenoid saponin separation and purification technique
Aspect is bold in innovation and is attempted.
Wherein, foam separating technology is the prior art, is a kind of difference based on surface-active between solute component in solution
Different isolated new technique, since foamet has, equipment is simple and convenient to operate, operating cost is low, environmental-friendly
The advantages that with large-scale industrial production is suitable for；Technological parameter involved in foam separating technology includes input concentration, pH value of solution
Value, separation temperature, vent gas speed, liquid volume etc.；Foam separation equipment generally uses foam separating tower, and entrance is raw material
Liquid, gas feed mouth are excluded in tower bottom, foam solution by tower top, and the feed liquid after foam fraction factor is discharged by tower bottom discharge port,
Foam separator can be used commonly uses separation equipment in the prior art.
It is one of the necessary condition of foam fraction factor, the present invention containing surface reactive material in foam separating technology, in solution
It was found that quinoa saponin(e has hydrophilic glycosyl and hydrophobic sapogenin, it is a kind of excellent natural non-ionic surfactant
Ingredient has good foaming characteristic, therefore it is considered herein that quinoa saponin(e crude extract has the necessary condition of foam fraction factor, can
To be separated using foam separating technology to saponin(e, the present invention can be greatly reduced organic molten in routine techniques using the technology
The usage amount of agent, at the same also reduce wastewater discharge, it can be achieved that quinoa saponin(e efficiently, easy and environmental-friendly separation mentions
It takes.The present invention extracts in quinoa that also someone does not disclose or uses in the art for the design of saponin(e using foamet.
Embodiment 2
A kind of foam separator, comprising:
Foam fraction factor unit is made of foam separating tower and recirculated water jacketed pipe, and the foam separating tower is set to described
The inside of recirculated water jacketed pipe is formed between the outer wall of the foam separating tower and the inner wall of the recirculated water jacketed pipe for holding
Receive the cavity of recirculated water；The foam separating tower be used for by quinoa saponin(e crude extract foam and solution separate；It is described to follow
The top of ring water leg pipe is equipped with recirculated water water outlet, and lower part is equipped with recirculated water water inlet；It is set at the top of the foam separating tower
There is foam outlet, bottom is equipped with air inlet；
It supplies gas unit, hose connection is passed sequentially through by air compressor, gas safety bottle and gas flowmeter and is formed, institute
State the air inlet that gas flowmeter is connected to the foam separating tower by hose；
Water unit is recycled, the water outlet of the circulation water unit and the recirculated water water inlet of the recirculated water jacketed pipe connect
Logical, the recirculated water water outlet of the recirculated water jacketed pipe is connected to the water inlet of the circulation water unit, the circulation water unit
Water bath with thermostatic control is provided for the foam separating tower；
Foam collector unit is made of collection elbow and collection vessel；Under use state, described one end for collecting elbow
It is inserted into the foam outlet of the foam fraction factor top of tower and forms close connection, the collection vessel is isolated for collecting to accommodate
Foam；
Separating liquid extracts unit out, is made of oilless vacuum pump and liquid safe bottle；Under use state, the liquid safe
Bottle is inserted into the inside of the foam separating tower, the foam point by hose from the foam outlet of the foam fraction factor top of tower
It is drawn in liquid safe bottle from the separating liquid in tower.
As the preferred of above-described embodiment, the collection elbow is made of inner and outer tubes, and outer tube is set to said inner tube
Outside forms cavity, inner tube and outer tube and is closed at two ports for collecting elbow between outer tube and inner tube, foam fraction factor tower top
Foam from it is described collect elbow inner tube in flow out.When the advantages of designing bimetallic tube is to make foam flow through collection elbow,
Accelerate foam flow velocity, promote lather collapse, reduces the collection that foam volume is convenient for container, otherwise collection vessel needs very big appearance
Product.
As the preferred of above-described embodiment, the first bending place angle for collecting elbow is 90 °, the collection elbow
Second bending place angle is 90 °.The advantages of designing 90 degree of angles is because continuous two 90 ° of elbows change the flowing of foam
Direction is that the movement of foam from bottom to top becomes movement from top to bottom, enters convenient under gravity collecting foam
In collection vessel.
As the preferred of above-described embodiment, it is equipped with gas distribution grid at the blow vent of the foam fraction factor tower bottom, is hole
The micropore sand core filter plate that diameter is 30 microns, is made of sintered frit.
As the preferred of above-described embodiment, the exit diameter for collecting elbow is 20mm, the recirculated water jacketed pipe
Diameter be 60mm, the diameter of the foam separating tower is 40mm；Valve is equipped at the blow vent；The collection elbow, institute
Show foam separating tower, the material of the recirculated water jacketed pipe is glass.
The application method of above-mentioned foam separator: in use, first collection bend pipe is not installed, need to saponin(e to be separated mention
Liquid is taken to be added in foam separating tower from the foam outlet of tower top；Circulation water unit is opened, set water temperature reaches recirculated water
The temperature of setting, and temperature is made to keep constant 5min or more；Bend pipe will be collected again to be inserted into the foam outlet and be seated, and puts receipts well
Collect vessel, open unit of supplying gas, start air compressor, adjusting gas flow meter makes to supply gas velocity-stabilization in defined gas stream
Magnitude starts foam fraction factor process；When foam collect winding pipe exit at there is no removed when foam overflow foam trap ware and
Collect elbow；The plastic flexible pipe for being connected with oilless vacuum pump and liquid safe bottle is inserted into from the foam outlet of separation column
It is drawn in liquid safe bottle in separating liquid in foam separating tower and by separating liquid, completes the foam fraction factor mistake of saponin extract solution
Journey；Need to add pure water cleaning foam separating tower after use twice.
Place, those skilled in the art can not select from the prior art to the greatest extent in the embodiment of the present invention.
Disclosed above is only a specific embodiment of the invention, but scope of protection of the present invention is not limited thereto, is appointed
What those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, answer
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be with above-mentioned scope of protection of the claims
It is quasi-.
Claims (9)
1. a kind of separation method of quinoa saponin(e, which is characterized in that the method is using foam separating technology to quinoa saponin(e
Carry out separation and Extraction；
Wherein, the concentration of material liquid is 0.4413-0.6620mg/mL in the foam separating technology, and temperature is 15-25 DEG C, is led to
Gas velocity 20-40mL/min, volume of the raw material liquid 150-250mL.
2. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that the foam separating technology Central Plains
The concentration of feed liquid is 0.4815-0.5884mg/mL, and temperature is 20-25 DEG C, venting flow rate 20-35mL/min, and volume of the raw material liquid is
200-250mL。
3. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that the foam separating technology Central Plains
The concentration of feed liquid is 0.4815-0.5296mg/mL, and temperature is 21-25 DEG C, venting flow rate 20-30mL/min, and volume of the raw material liquid is
210-250mL。
4. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that the foam separating technology Central Plains
The concentration of feed liquid is 0.4996-0.5296mg/mL, and temperature is 22-25 DEG C, venting flow rate 21-25mL/min, and volume of the raw material liquid is
220-250mL。
5. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that the foam separating technology Central Plains
The concentration of feed liquid is 0.5092-0.5296mg/mL, and temperature is 23-25 DEG C, venting flow rate 21-23mL/min, and volume of the raw material liquid is
230-250mL。
6. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that the foam separating technology Central Plains
The concentration of feed liquid is 0.5192-0.5296mg/mL, and temperature is 24-25 DEG C, venting flow rate 21-22mL/min, and volume of the raw material liquid is
240-250mL。
7. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that the foam separating technology Central Plains
The concentration of feed liquid is 0.5296mg/mL, and temperature is 25 DEG C, venting flow rate 22mL/min, volume of the raw material liquid 250mL.
8. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that in the foam separating technology,
Quinoa saponin(e concentration ratio is 2.0-2.6, rate of recovery 42%-52%；The pH value of the material liquid is 3-5.
9. a kind of separation method of quinoa saponin(e as described in claim 1, which is characterized in that the kind of the quinoa is green Chenopodiaceae
No.1；The pH value of the material liquid is 5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910537739.9A CN110240625A (en) | 2019-06-20 | 2019-06-20 | A kind of separation method and foam separator of quinoa saponin(e |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910537739.9A CN110240625A (en) | 2019-06-20 | 2019-06-20 | A kind of separation method and foam separator of quinoa saponin(e |
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| CN114853821B (en) * | 2022-06-08 | 2024-07-05 | 中华全国供销合作总社济南果品研究所 | Method for separating saponin from canned asparagus processing wastewater |
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| CN114853821A (en) * | 2022-06-08 | 2022-08-05 | 中华全国供销合作总社济南果品研究所 | Method for separating saponin from waste water of canned asparagus processing |
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