CN106831931A - A kind of method that two-step method prepares sapindoside - Google Patents
A kind of method that two-step method prepares sapindoside Download PDFInfo
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- CN106831931A CN106831931A CN201710058065.5A CN201710058065A CN106831931A CN 106831931 A CN106831931 A CN 106831931A CN 201710058065 A CN201710058065 A CN 201710058065A CN 106831931 A CN106831931 A CN 106831931A
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- 229930183111 sapindoside Natural products 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000006260 foam Substances 0.000 claims abstract description 36
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 229930182490 saponin Natural products 0.000 claims abstract description 22
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 20
- 150000007949 saponins Chemical class 0.000 claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 claims abstract description 11
- 239000000284 extract Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 240000003377 Shepherdia canadensis Species 0.000 claims description 11
- 235000018324 Shepherdia canadensis Nutrition 0.000 claims description 11
- 238000004821 distillation Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 235000012054 meals Nutrition 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000287 crude extract Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002798 spectrophotometry method Methods 0.000 claims description 3
- 238000005202 decontamination Methods 0.000 claims description 2
- 230000003588 decontaminative effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 8
- 238000003908 quality control method Methods 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- DKVBOUDTNWVDEP-NJCHZNEYSA-N teicoplanin aglycone Chemical group N([C@H](C(N[C@@H](C1=CC(O)=CC(O)=C1C=1C(O)=CC=C2C=1)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)OC=1C=C3C=C(C=1O)OC1=CC=C(C=C1Cl)C[C@H](C(=O)N1)NC([C@H](N)C=4C=C(O5)C(O)=CC=4)=O)C(=O)[C@@H]2NC(=O)[C@@H]3NC(=O)[C@@H]1C1=CC5=CC(O)=C1 DKVBOUDTNWVDEP-NJCHZNEYSA-N 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 230000005587 bubbling Effects 0.000 abstract description 2
- 125000003147 glycosyl group Chemical group 0.000 abstract description 2
- 235000017709 saponins Nutrition 0.000 description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 238000002330 electrospray ionisation mass spectrometry Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- MIJYXULNPSFWEK-GTOFXWBISA-N 3beta-hydroxyolean-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C MIJYXULNPSFWEK-GTOFXWBISA-N 0.000 description 1
- JKLISIRFYWXLQG-UHFFFAOYSA-N Epioleonolsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4CCC3C21C JKLISIRFYWXLQG-UHFFFAOYSA-N 0.000 description 1
- 229930189092 Notoginsenoside Natural products 0.000 description 1
- YBRJHZPWOMJYKQ-UHFFFAOYSA-N Oleanolic acid Natural products CC1(C)CC2C3=CCC4C5(C)CCC(O)C(C)(C)C5CCC4(C)C3(C)CCC2(C1)C(=O)O YBRJHZPWOMJYKQ-UHFFFAOYSA-N 0.000 description 1
- MIJYXULNPSFWEK-UHFFFAOYSA-N Oleanolinsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C MIJYXULNPSFWEK-UHFFFAOYSA-N 0.000 description 1
- 241000580938 Sapindus Species 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 244000248162 Xanthoceras sorbifolium Species 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003254 anti-foaming effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005351 foam fractionation Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229930182494 ginsenoside Natural products 0.000 description 1
- 229940089161 ginsenoside Drugs 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940100243 oleanolic acid Drugs 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- HZLWUYJLOIAQFC-UHFFFAOYSA-N prosapogenin PS-A Natural products C12CC(C)(C)CCC2(C(O)=O)CCC(C2(CCC3C4(C)C)C)(C)C1=CCC2C3(C)CCC4OC1OCC(O)C(O)C1O HZLWUYJLOIAQFC-UHFFFAOYSA-N 0.000 description 1
- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- RXHIKAIVEMAPRU-JRIGQVHBSA-N sequiterpene Natural products C1=C(C)[C@@H](OC(C)=O)[C@H](O)[C@@]2(O)[C@H](C)CC[C@@H](C(C)=C)[C@H]21 RXHIKAIVEMAPRU-JRIGQVHBSA-N 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000008130 triterpenoid saponins Chemical class 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Saccharide Compounds (AREA)
Abstract
A kind of method that two-step method prepares sapindoside, is related to sapindoside.Macroporous resin adsorption is separated；Foam fraction factor, obtains sapindoside.Separating high-purity sapindoside is extracted using macroreticular resin and foam fraction factor two-step method, and design a kind of method simple to operate, energy quick detection total saponin of sapindusmukerossi, for the quality control of sapindoside provides basis, propulsion sapindoside extracts the research for separating industrial applications.Sapindoside is made up of oil loving aglycon part and hydrophilic glycosyl.Its lipophile aglycon part can be adsorbed resin adsorption again, carry out first step separation.Sapindoside is again a kind of natural surfactant, is the necessary condition of foam fraction factor with surface-active, and it produces foam, second step that high-purity sapindoside product are obtained with other impurities separation and purification by foam fraction factor under the effect of air-flow bubbling.
Description
Technical field
The present invention relates to sapindoside, a kind of method that sapindoside is prepared more particularly, to two-step method.
Background technology
Sapindoside mainly includes the triterpenoid saponin and part sequiterpene glucosides with ivy sapogenin as basic framework.
They are a kind of natural nonionic surface active agent, with antibacterial, sterilization, anti-inflammatory, foaming and stronger dirt-removing power, can
As detergent.Isolating and purifying for soapberry is basis that it is developed, and current extraction separation method has macroreticular resin to separate
Method, extraction and ultrafiltration etc..(extraction of [1] Wei Fengyu, Yu Jincheng, Xie Hui Natural Sapindus Saponins is separated Wei Fengyu etc.
[J] Anhui chemical industry, 2007,33 (3):15-17) using water extraction-macroporous resin adsorption partition method and ultrafiltration to sapindoside
Isolated and purified, total saposins purity can respectively up to 85% and 67%.But the solvent-oil ratio of the method is big, the operation cycle
It is long.
Foam fraction factor is a kind of method for using the surface-active difference of component separate with bubble as medium.By drum
Bubble is gathered in liquid-vapor interface with making solute selectivity, and virtue of buoyancy rises to solution main body top and forms froth bed, so as to reach
To process ([2] Yan J, Wu Z, Zhao Y, et al.Separation of tea saponin by two- of enrichment saponin(e
stage foam fractionation[J].Separation and Purification Technology,2011,80
(2):300-305).In recent years, achieved in the natural saponins such as ginsenoside, notoginsenoside and shiny-leaved yellowhorn pericarp are separated compared with
Good effect.
The content of the invention
Sold without soapberry quality-control product on the market it is an object of the invention to be directed to, total saponin of sapindusmukerossi detection method missing
And the few problem of real application research, there is provided a kind of method that two-step method prepares sapindoside.
The present invention is comprised the following steps：
1) macroporous resin adsorption is separated (macroreticular resin is separated)；
In step 1) in, the specific method that the macroporous resin adsorption is separate can be：
With soapberry pericarp as raw material, crush, alcohol extracting, merge soapberry extract, spray drying obtains sapindoside
Corase meal, then constant volume, upper resin column after ultrasound, washing removes decontamination except sugar, alcohol, then alcohol washes collection saponin(e, and rotary evaporation is waved
After dry solvent, saponin(e corase meal is obtained.
The alcohol extracting can alcohol extracting 2~3 times；The time of the ultrasound can be 15min；The resin column can use D101 resins
Post；The washing can use deionized water except sugar；The alcohol wash can use mass percentage concentration for 20% ethanol；The alcohol again
Wash can use mass percentage concentration for 70% ethanol.
2) foam fraction factor, obtains sapindoside.
In step 2) in, the specific method of the foam fraction factor can be：
Naval stores powder obtained aqueous solution, the top from chromatographic column of the bottom equipped with core (as gas distributor) is former
Liquor inlet sample introduction, air through air pump air inlet flowmeter, after entering back into surge flask and humidifier, by chromatographic column bottom
Air intlet, then by the core of chromatographic column bottom, be dispersed into bubble by the sapindoside crude extract at chromatographic column bottom,
Enter outer layer after foam overflow and be passed through 60 DEG C of straight types steamings of circulating hot water from the foam solution import on distillation cascade top again from down to up
Pipe is evaporated, accelerates lather collapse, collect its bottom foam solution, after the volume that solution is surveyed after froth breaking, use spectrophotometry foam
Sapindoside content in liquid, solids level concentration is surveyed after volatilizing solvent, calculates its purity.
The sample introduction can sample introduction in three times；The gas velocity of the air can be 2min/L.
The internal diameter of the chromatographic column can be 25mm, and height can be 300mm；The internal diameter of the distillation cascade can be 35mm, a height of
600mm。
The present invention extracts separating high-purity sapindoside using macroreticular resin with foam fraction factor two-step method, and designs one
The method for planting energy quick detection total saponin of sapindusmukerossi simple to operate, for the quality control of sapindoside provides basis, advances nothing
Suffer from the research that sub- saponin extraction separates industrial applications.
Operation principle of the invention is：
Sapindoside is made up of oil loving aglycon part and hydrophilic glycosyl.Again can its lipophile aglycon part
Adsorbed resin adsorption, carries out first step separation.Sapindoside is again a kind of natural surfactant, with surface-active,
It is the necessary condition of foam fraction factor, it produces foam, second step to pass through foam fraction factor and other impurities under the effect of air-flow bubbling
Separation and purification is obtained high-purity sapindoside product.
Brief description of the drawings
Fig. 1 is foam separator structural representation.
Fig. 2 is sapindoside sample drawing prepared by the embodiment of the present invention.
Fig. 3 is sapindoside ESI-MS chromatograms prepared by the embodiment of the present invention.
Specific embodiment
Embodiment 1
1) macroporous resin adsorption is separated (macroreticular resin is separated)
With soapberry pericarp as raw material, crush, alcohol extracting 2~3 times, merge soapberry extract, spray drying is obtained without trouble
Sub- saponin(e corase meal.0.5001g sample powders accurately are weighed, deionized water is settled to 100ml, ultrasonic 15min, upper D101 resins
Post, is washed except sugar with deionized water 300ml, and 20% alcohol washes 100ml except other impurities, and 70% alcohol washes 100ml and collects saponin(e, rotation
Evaporation, after volatilizing solvent, receives saponin(e corase meal.70% alcohol is washed can be using 2 times, and 2 70% alcohol are washed and take 0.5ml and 0.1ml
Saponin(e and total reducing sugar absorbance are surveyed respectively with ultraviolet specrophotometer, in the respective relational expression of substitution：
Absorbance (A) is A=48.9228C+0.0353 with the relational expression of oleanolic acid concentration of standard solution (C), related
Coefficients R=0.9995.
Absorbance (A) is A=25.525C+0.0186, coefficient R with the relational expression of total reducing sugar concentration of standard solution (C)
=0.9900.
70% alcohol washes middle saponin concentrations 1.533mg/ml, saponin content=0.01022g, solid content=0.0495g, purity
=20.64%.
Each stage sapindoside concentration of macroreticular resin is referring to table 1.
Table 1
2) foam fraction factor, obtains sapindoside (referring to Fig. 1).
The specific method of the foam fraction factor can be：
Naval stores powder obtained aqueous solution, from the upper of chromatographic column 1 of the bottom equipped with core 11 (as gas distributor)
The square sample introduction of material liquid import 13, air after entering back into surge flask 5 and humidifier 6, passes through through the air inlet flowmeter 4 of air pump 3
The air intlet 12 of the bottom of chromatographic column 1, then by the core 11 of the bottom of chromatographic column 1, is dispersed into bubble by chromatographic column bottom
Sapindoside crude extract, is passed through after foam overflow into foam solution import 21 of the outer layer from down to up again from the top of distillation cascade 2
60 DEG C of straight type distillation cascades 2 of circulating hot water, accelerate lather collapse, collect its bottom foam solution, after the volume that solution is surveyed after froth breaking,
With sapindoside content in spectrophotometry foam solution, solids level concentration is surveyed after volatilizing solvent, calculate its purity.The product
The final sapindoside purity of product is 92%.
The sample introduction can sample introduction in three times；The gas velocity of the air can be 2min/L.
The internal diameter of the chromatographic column can be 25mm, and height can be 300mm；The internal diameter of the distillation cascade can be 35mm, a height of
600mm。
In Fig. 1, mark 22 is foam solution outlet, and 23 is foam solution receiver, and 24 is hot water outlet, and 25 enter for hot water
Mouthful.
Embodiment 2
1) macroporous resin adsorption separates (macroreticular resin separation twice)
With soapberry pericarp as raw material, crush, alcohol extracting 2~3 times, merge soapberry extract, spray drying is obtained without trouble
Sub- saponin(e corase meal.Accurate to weigh 1.0g sample powders, deionized water is settled to 250ml, ultrasonic 15min, upper D101 resin columns,
Washed except sugar with deionized water 300ml, 20% alcohol washes 100ml except other impurities, 70% alcohol washes 100ml and collects saponin(e, rotation is steamed
Hair, after volatilizing solvent, acetone sedimentation, centrifugation volatilizes acetone, plus deionized water dissolving, with saturation water extracting n-butyl alcohol three times, takes
After organic layer volatilizes solvent, the 20mg/mL sapindoside aqueous solution is prepared, with D101 macroreticular resins, 3BV in 1mL/min speed
With 70% ethanol elution of 1BV after deionization washing, volatilize solvent and collect powder, saponin(e takes 0.1ml and surveys absorbance, and surveys solid
Content, D101 resins reach 481.57mg/mL, purity about 35.51% to the saturated extent of adsorption of sapindoside.
2) foam fraction factor
Naval stores powder prepares the 0.2mg/mL aqueous solution, from top sample introduction of the bottom equipped with chromatographic column, feeds in three times,
Common 100mL, air gas velocity 2min/L, through air pump air inlet flowmeter, into after a surge flask and humidifier, by layer
The core of analysis post bottom, is dispersed into sapindoside crude extract of the bubble by post bottom, is arrived by down into outer layer after foam overflow
On be passed through the straight types distillation of 60 DEG C of circulating hot waters, accelerate lather collapse, after the volume that solution is surveyed after froth breaking, examined with AAS
Sapindoside content in foam solution is surveyed, solids level concentration is surveyed after volatilizing solvent, its purity is sought in calculating.Experimental provision is shown in specification
Fig. 1.Foam fraction factor sapindoside yield 19.68%, concentration ratio 1.96, purity 92.92%.
In order to judge the composition of quality-control product, selection positive ion mode carries out the ESI-MS detections of sapindoside, goes out in figure
Existing each saponin(e【M+Na】+Quasi-molecular ion point.
Sapindoside quality-control product constituent analysis is shown in Table 2.
Table 2
It is right that the quality-control product that high-purity is obtained by the use of foam fraction factor and macroreticular resin combination can be detected as sapindoside
According to product, by various collection of illustrative plates structural characterizations, it was demonstrated that self-control sapindoside quality-control product main component is that Sapindosides C (divide
Son amount is 882).
The soapberry soap that sapindoside sample drawing prepared by the embodiment of the present invention is prepared referring to Fig. 2, the embodiment of the present invention
Glycosides ESI-MS chromatograms are referring to Fig. 3.
Claims (10)
1. a kind of method that two-step method prepares sapindoside, it is characterised in that comprise the following steps：
1) macroporous resin adsorption is separated；
2) foam fraction factor, obtains sapindoside.
2. a kind of method that two-step method prepares sapindoside as claimed in claim 1, it is characterised in that in step 1) described in
Macroporous resin adsorption separate specific method be：
With soapberry pericarp as raw material, crush, alcohol extracting, merge soapberry extract, spray drying obtains sapindoside meal
End, then constant volume, upper resin column after ultrasound, washing removes decontamination except sugar, alcohol, then alcohol washes collection saponin(e, and rotary evaporation is volatilized molten
After agent, saponin(e corase meal is obtained.
3. a kind of method that two-step method prepares sapindoside as claimed in claim 2, it is characterised in that the alcohol extracting is alcohol extracting 2
~3 times.
4. a kind of method that two-step method prepares sapindoside as claimed in claim 2, it is characterised in that the time of the ultrasound
It is 15min.
5. a kind of method that two-step method prepares sapindoside as claimed in claim 2, it is characterised in that the resin column is used
D101 resin columns.
6. a kind of method that two-step method prepares sapindoside as claimed in claim 2, it is characterised in that the washing is adopted except sugar
Use deionized water；The alcohol wash use mass percentage concentration for 20% ethanol；The alcohol again wash use mass percentage concentration for
70% ethanol.
7. a kind of method that two-step method prepares sapindoside as claimed in claim 1, it is characterised in that in step 2) in, it is described
The specific method of foam fraction factor is：
Naval stores powder obtained aqueous solution, from the top material liquid import sample introduction of chromatographic column of the bottom equipped with core, air warp
Air pump air inlet flowmeter, after entering back into surge flask and humidifier, by the air intlet of chromatographic column bottom, then passes through
The core of chromatographic column bottom, is dispersed into sapindoside crude extract of the bubble by chromatographic column bottom, and outer layer is entered after foam overflow
60 DEG C of straight type distillation cascades of circulating hot water are passed through from the foam solution import on distillation cascade top again from down to up, accelerate lather collapse,
Its bottom foam solution is collected, after the volume that solution is surveyed after froth breaking, with sapindoside content in spectrophotometry foam solution,
Solids level concentration is surveyed after volatilizing solvent, its purity is calculated.
8. a kind of method that two-step method prepares sapindoside as claimed in claim 7, it is characterised in that the sample introduction is in three times
Sample introduction；The gas velocity of the air is 2min/L.
9. a kind of two-step method method for preparing sapindoside as claimed in claim 7, it is characterised in that the chromatographic column it is interior
Footpath is 25mm, a height of 300mm.
10. a kind of two-step method method for preparing sapindoside as claimed in claim 7, it is characterised in that the distillation cascade it is interior
Footpath is 35mm, a height of 600mm.
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| CN201710058065.5A CN106831931A (en) | 2017-01-23 | 2017-01-23 | A kind of method that two-step method prepares sapindoside |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107375503A (en) * | 2017-08-02 | 2017-11-24 | 瑞阳制药有限公司 | The preparation method of soapberry pericarp activity extract and its antimycotic application |
| CN111423485A (en) * | 2020-05-09 | 2020-07-17 | 颜克顺 | Preparation method of soapberry saponin |
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