CN104558088A - Method for extracting mogroside V from momordica grosvenori - Google Patents

Method for extracting mogroside V from momordica grosvenori Download PDF

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CN104558088A
CN104558088A CN201510033531.5A CN201510033531A CN104558088A CN 104558088 A CN104558088 A CN 104558088A CN 201510033531 A CN201510033531 A CN 201510033531A CN 104558088 A CN104558088 A CN 104558088A
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momordica
extracting
grosvenor momordica
grosvenor
momordica grosvenori
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唐方华
黄华学
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JIANGXI HAIFU BIOENGINEERING CO Ltd
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JIANGXI HAIFU BIOENGINEERING CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J17/00Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
    • C07J17/005Glycosides

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Abstract

The invention provides a method for extracting mogroside V from momordica grosvenori. The method comprises the steps of carrying out pretreatment on raw materials, carrying out microwave countercurrent extraction, carrying out multistage filtering, carrying out macroreticular resin adsorption separation, carrying out nanofiltration, concentrating and drying. The method integrates the advantages of multiple extracting ways, and is used for continuously and efficiently extracting the mogroside V. Products obtained by adopting the method are proved that the mogroside V is 63-65% and the final yield of the mogroside V is 70-74% after being detected by adopting a high performance liquid chromatography. Except ethyl alcohol, in the method, other organic solvents which are harmful to the human body are not used, thus the products are environmentally friendly; the products contain less than 10ppm of ethyl alcohol residue, thus being safe and high in quality.

Description

A kind of method extracting momordica grosvenori glycoside V from Grosvenor Momordica
Technical field
The present invention relates to a kind of extracting method of plant constituent, particularly relate to the method extracting momordica grosvenori glycoside V from Grosvenor Momordica, it can the extraction momordica grosvenori glycoside V of continuous high-efficient.
Background technology
Grosvenor Momordica as the endemic plant of China, because of advantage geographically, for the research of Grosvenor Momordica each side is provided convenience, to its research except Grosvenor Momordica composite except, mainly concentrate on the extraction and purification process aspect of momordica glycoside V.CN101863946A discloses a kind of method extracting high-content Momordica grosvenori mogroside V in dried fructus momordicae, the method be by alcohol extracting after the fragmentation of Grosvenor Momordica dry fruit, concentrated, macroporous resin adsorption is separated, ion-exchange resin decolorization, product is obtained through concentrate drying, the method process is simple, adapt to plant produced, but product purity is low, resin utilization rate is low.CN101690573A discloses a kind of Mogroside V content and is greater than 60% production method of fructus, the method is separated and alumina column chromatography enzymolysis after Grosvenor Momordica fragmentation, water extraction, concentrated, ion-exchange resin decolorization, macroporous resin adsorption, product is obtained finally by concentrate drying, the method can realize product sweet glycosides V purity and be greater than 60%, because of through more chromatographic enrichment, make the yield of the finished product lower.CN10140266A discloses the preparation method of momordica grosvenori glycoside V, the method is for raw material with Grosvenor Momordica crude extract, product is obtained through silica gel column chromatography, C18 post reversed phase chromatography, concentrate drying, product purity can reach more than 70%, the major defect of the method is use a large amount of organic solvents in process, product yield is low, and cost is high, is unsuitable for industrial production.CN101177444A discloses a kind of method extracting Momordica-Glycosides from Grosvenor Momordica, the method be the fragmentation of Grosvenor Momordica fresh fruit, enzymolysis, multi-stage countercurrent are extracted, centrifugal, ultrafiltration, concentrated, macroporous resin adsorption separation, ion-exchange resin decolorization, C18 reversed-phase silica gel chromatography, through concentrate drying, obtained product, the defect of the method is that product yield is low, product purity is low, complex process, is unfavorable for industrial production.CN104086615A discloses a kind of method preparing mogroside V from Grosvenor Momordica, the method be by autoclaving after Grosvenor Momordica fragmentation, supercritical fluid extraction, through HP-20ss resin chromatography, concentrated, dry product, sweet glycosides V purity more than 70% in product, the method technique is simple, purity is high, but due to supercritical fluid extraction equipment primary treatment quantitative limitation, be unfavorable for continuous print scale production.Given this, be necessary to improve prior art.
Summary of the invention
The present invention proposes a kind of method extracting momordica grosvenori glycoside V from Grosvenor Momordica, and the method has organically combined multiple purification mode, realizes the extraction momordica grosvenori glycoside V of continuous high-efficient.
Technical scheme of the present invention is achieved in that
From Grosvenor Momordica, extract a method for momordica grosvenori glycoside V, it is characterized in that comprising the following steps:
Raw material pre-treatment: Grosvenor Momordica is clean, broken;
Microwave counter current extracts: carry out microwave counter current extraction to the Grosvenor Momordica after pre-treatment, Extraction solvent is deionized water, and the flowing of material and water is reverse continuous dynamic flow, extrudes simultaneously, extrude debris and mix with feed liquid slag, obtains extracting solution after filtration;
Cascade filtration: extracting solution is centrifugal through horizontal screw centrifugal, tubular type first, after the first ultrafiltration and the second ultrafiltration filtrate, wherein, the rotating speed of described horizontal screw centrifugal is 2500 ~ 5000r/min, the centrifugal rotating speed of tubular type is 12000 ~ 16000r/min, first ultrafiltration is through the ultra-filtration membrane that molecular weight cut-off is 30k ~ 50kDa, and the second ultrafiltration is through the ultra-filtration membrane that molecular weight cut-off is 4k ~ 6kDa;
Macroporous resin adsorption is separated: the Ph value regulating filtrate, and on normal temperature, macroporous resin column is adsorbed, and upper column flow rate is 0.5 ~ 1.5 BV/h, leaves standstill 1 ~ 2h after upper prop completes; Under being equivalent to resin cumulative volume 6 ~ 8 times of deionized water normal temperature, carry out wash-out, elution flow rate is 2 ~ 3BV/h, and then use hydrophilic solvent to carry out wash-out to macroporous resin column, elution flow rate is 1 ~ 2 BV/h, collects elutriant;
Cascade filtration: used by elutriant nanofiltration membrane to carry out nanofiltration process, then till the sharp degree 30 ~ 35 of vacuum concentration to hundred, obtains concentrated solution;
Dry: after concentrated solution is carried out drying, to obtain momordica glycoside V.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, during the extraction of microwave counter current process, Extracting temperature is 70 ~ 90 DEG C, and extraction time is 50 ~ 70 min, and microwave power is 600 ~ 800W, frequency 6000 ~ 8000MHz.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, filtrate Ph is 8 ~ 9.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, the reagent regulating filtrate Ph is sodium hydroxide or sodium carbonate.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, described macroporous resin is D-101, AB-8 or HPD-100, and the blade diameter length ratio of resin column is 1:6.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, described hydrophilic solvent is volume fraction is 60 ~ 80% ethanolic solns, and the consumption of hydrophilic solvent is 2 ~ 3 BV.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, the molecular weight cut-off of described nanofiltration is 150 ~ 300Da.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, the thickening temperature of described vacuum concentration is 70 ~ 80 DEG C, and vacuum tightness is-0.08Mpa ~-0.04Mpa.
Thisly to extract from Grosvenor Momordica in the method for momordica grosvenori glycoside V of the present invention, the mode of drying treatment is spraying dry.
This method extracting momordica grosvenori glycoside V from Grosvenor Momordica carried out an invention, has following beneficial effect: the present invention combines the advantage of multiple extracting mode, completes the extraction momordica grosvenori glycoside V of continuous high-efficient rate.According to the product that the inventive method obtains, detect through high performance liquid chromatography, momordica glycoside V 63 ~ 65%, momordica glycoside V ultimate yield 70 ~ 74%.Except ethanol, present method does not use other harmful organic solvent solvent, and to environment environmental protection, in product, alcohol residue is at below 10ppm, product safety, and quality is high.
Microwave counter current extracts and replaces traditional circumfluence distillation, achieves the continuity of extraction on the one hand, improves industrial scale, while ensureing yield on the other hand, decrease the use of extraction time and solvent, extraction time is kept to original 1/5, and solvent usage quantity is original less than 50%.
Cascade filtration mode eliminates particle in feed liquid and macromole impurity further, purifying feed liquid.Employ in process and centrifugally to filter with the mode of combining ultrafiltration, first the horizontal screw centrifugal of low speed in adopting, eliminate oarse-grained suspended particle in feed liquid, and then use tubular type at a high speed centrifugal, eliminate solid particulate tiny in feed liquid, then 30k ~ 50kDa is respectively through molecular weight cut-off successively, the ultra-filtration membrane of 4k ~ 6kDa, eliminate most carbohydrate, protein, the macromolecular substance such as tannin, because filter type collocation is reasonable step by step, ensure that the continuity of filtration simultaneously, eliminate the partial impurities in feed liquid, make the utilization ratio of follow-up resin higher, be conducive to the enrichment of active substance.
The PH of the liquid of upper prop is adjusted to 8 ~ 9 by alkalescence upper prop, the acidic substance such as most coloring matters, flavones in feed liquid are existed in the form of an ion, do not flowed out with upper prop effluent liquid by macroporous resin adsorption in upper prop process, be further purified target component, also improve the adsorptive capacity of resin to activeconstituents simultaneously, improve the utilising efficiency of resin.
A large amount of solvents is mainly sloughed in nanofiltration, as ethanol, water, inorganic salt etc., reaches certain concentrated object, while employing nanofiltration mode carries out purifying, also to a certain degree reduces the energy consumption of subsequent concentration, reduces production cost.
Accompanying drawing explanation
Fig. 1 is the schematic diagram extracting the method for momordica grosvenori glycoside V from Grosvenor Momordica of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.
As shown in Figure 1, this method extracting momordica grosvenori glycoside V from Grosvenor Momordica of the present invention comprises: raw material pre-treatment, microwave counter current process, cascade filtration process, macroporous resin adsorption process, and nanofiltration, concentration, drying treatment, described in specific as follows.
S1: by the removal of impurities of Grosvenor Momordica fresh fruit, cleans, suitably broken, is advisable not smash Grosvenor Momordica fruit seed.
S2: microwave counter current extracts and uses microwave counter current extraction element to extract the Grosvenor Momordica after fragmentation, and during extraction, Extracting temperature is 70 ~ 90 DEG C, and extraction time is 50 ~ 70 min, and microwave power is 600 ~ 800W, frequency 6000 ~ 8000MHz.Extraction solvent is deionized water, forward feeding, anti-phase water inlet, the flowing of material and water is reverse continuous dynamic flow, and filter residue is forced to push to slag notch through spiral conveyer, and spiral of slagging tap extrudes slag simultaneously, residue is discharged, and debris is extruded and mixed with feed liquid, obtains extracting solution after filtration.
S3: undertaken centrifugal by S2 gained extracting solution, be first through horizontal screw centrifugal, rotating speed is 2500 ~ 5000r/min, then centrifugal through tubular type, and rotating speed is 12000 ~ 16000r/min.Carrying out ultrafiltration after centrifugal, is 30k ~ 50kDa ultra-filtration membrane through molecular weight cut-off, and being then through molecular weight cut-off is 4k ~ 6kDa, is hollow-fibre membrane, finally obtains filtrate.
S4: regulate in S3 behind gained filtrate Ph to 8 ~ 9, on normal temperature, macroporous resin column is adsorbed, and upper column flow rate is 0.5 ~ 1.5 BV/h, leaves standstill 1 ~ 2h after upper prop completes.Under being equivalent to resin cumulative volume 6 ~ 8 times of deionized water normal temperature, carry out wash-out, elution flow rate is 2 ~ 3BV/h, and then use hydrophilic solvent to carry out wash-out to macroporous resin column, elution flow rate is 1 ~ 2 BV/h, collects elutriant.The reagent regulating filtrate Ph is sodium hydroxide or carbonic acid.Described macroporous resin is D-101, AB-8 or HPD-100, and the blade diameter length ratio of resin column is 1:6.Wherein, D-101, AB-8 manufacturer is resin company limited of Shanghai Nankai, and DM130 manufacturer is Anhui Samsung resin Science and Technology Ltd..Described hydrophilic solvent is volume fraction is 60 ~ 80% ethanolic solns, and the consumption of hydrophilic solvent is 2 ~ 3 BV.
S5: use nanofiltration membrane to carry out nanofiltration process gained elutriant in S4, molecular weight cut-off is 150 ~ 300Da.Then till the sharp degree 30 ~ 35 of vacuum concentration to hundred, thickening temperature is 70 ~ 80 DEG C, and vacuum tightness is-0.08Mpa ~-0.04Mpa, finally obtains concentrated solution.
S6: after gained concentrated solution carries out spraying dry in S5, the product of momordica glycoside V.
For more clearly understanding the present invention, below provide five embodiments.
embodiment 1
S1 raw material pre-treatment: get 1000 kg Grosvenor Momordica fresh fruit removal of impurities, cleans, suitably broken, is advisable not smash Grosvenor Momordica fruit seed;
S2 microwave counter current extracts: use microwave counter current extraction element to extract the Grosvenor Momordica after fragmentation, Extraction solvent is deionized water, forward feeding, anti-phase water inlet, the flowing of material and water is reverse continuous dynamic flow, and Extracting temperature is 90 DEG C, extraction time is 70 min, microwave power is 800w, and frequency is 6000MHz, and filter residue is forced to push to slag notch through spiral conveyer, spiral of slagging tap extrudes slag simultaneously, residue is discharged, and debris is extruded and mixed with feed liquid, obtains extracting solution after filtration;
S3 cascade filtration: use horizontal spiral centrifuge to carry out centrifugal gained extracting solution in step s2, centrifugal rotational speed is 5000 r/min, then tubular-bowl centrifuge is crossed, centrifugal rotational speed is 14000 r/min, it is 50kDa, 6kDa hollow fiber ultrafiltration membrane that gained centrifugate crosses molecular weight cut-off successively, obtains filtrate;
S4 macroporous resin adsorption is separated: use in sodium hydroxide regulating step s3 after gained filtrate Ph to 8.98, on normal temperature, D-101 resin column adsorbs, and resin column blade diameter length ratio is 1:6, and upper column flow rate is 0.5BV/h, standing 2h after upper prop completes; Under being equivalent to resin cumulative volume 8 times of deionized water normal temperature, carry out wash-out, elution flow rate is 2BV/h, and then use 80% ethanol of 3BV to carry out wash-out to macroporous resin column, elution flow rate is 1BV/h, collects elutriant;
S5 nanofiltration, concentrated: to use 300Da nanofiltration membrane to carry out nanofiltration process gained elutriant in step s4, be then 80 DEG C in temperature, vacuum tightness is under the condition of-0.08Mpa ~-0.04Mpa, till the sharp degree 35 of vacuum concentration to hundred, obtains concentrated solution;
S6 is dry: gained concentrated solution in step s5 is carried out spraying dry, obtains the product of momordica glycoside V, weigh 6.422 kg.
Result through liquid chromatograph detects: momordica glycoside V content is 63.21%, and momordica glycoside V total recovery is 73.80%.
embodiment 2
S1 raw material pre-treatment: get 1000 kg Grosvenor Momordica fresh fruit removal of impurities, cleans, suitably broken, is advisable not smash Grosvenor Momordica fruit seed;
S2 microwave counter current extracts: use microwave counter current extraction element to extract the Grosvenor Momordica after fragmentation, Extraction solvent is deionized water, forward feeding, anti-phase water inlet, the flowing of material and water is reverse continuous dynamic flow, and Extracting temperature is 70 DEG C, extraction time is 50 min, microwave power is 600w, and frequency is 8000MHz, and filter residue is forced to push to slag notch through spiral conveyer, spiral of slagging tap extrudes slag simultaneously, residue is discharged, and debris is extruded and mixed with feed liquid, obtains extracting solution after filtration;
S3 cascade filtration: use horizontal spiral centrifuge to carry out centrifugal gained extracting solution in step s2, centrifugal rotational speed is 5000 r/min, then tubular-bowl centrifuge is crossed, centrifugal rotational speed is 14000 r/min, it is 30kDa, 4kDa hollow fiber ultrafiltration membrane that gained centrifugate crosses molecular weight cut-off successively, obtains filtrate;
S4 macroporous resin adsorption is separated: use in sodium carbonate regulating step s3 after gained filtrate Ph to 8.03, on normal temperature, HPD-100 resin column adsorbs, and resin column blade diameter length ratio is 1:6, and upper column flow rate is 1.5BV/h, standing 1h after upper prop completes; Under being equivalent to resin cumulative volume 6 times of deionized water normal temperature, carry out wash-out, elution flow rate is 2BV/h, and then use 50% ethanol of 3BV to carry out wash-out to macroporous resin column, elution flow rate is 2BV/h, collects elutriant;
S5 nanofiltration, concentrated: to use 150Da nanofiltration membrane to carry out nanofiltration process gained elutriant in step s4, be then 80 DEG C in temperature, vacuum tightness is under the condition of-0.08Mpa ~-0.04Mpa, till the sharp degree 30 of vacuum concentration to hundred, obtains concentrated solution;
S6 is dry: gained concentrated solution in step s5 is carried out spraying dry, obtains the product of momordica glycoside V, weigh 5.951kg.
Result through liquid chromatograph detects: momordica glycoside V content is 64.87%, and momordica glycoside V total recovery is 70.19%.
embodiment 3
S1 raw material pre-treatment: get 1000 kg Grosvenor Momordica fresh fruit removal of impurities, cleans, suitably broken, is advisable not smash Grosvenor Momordica fruit seed;
S2 microwave counter current extracts: use microwave counter current extraction element to extract the Grosvenor Momordica after fragmentation, Extraction solvent is deionized water, forward feeding, anti-phase water inlet, the flowing of material and water is reverse continuous dynamic flow, and Extracting temperature is 85 DEG C, extraction time is 60 min, microwave power is 700w, and frequency is 7000MHz, and filter residue is forced to push to slag notch through spiral conveyer, spiral of slagging tap extrudes slag simultaneously, residue is discharged, and debris is extruded and mixed with feed liquid, obtains extracting solution after filtration;
S3 cascade filtration: use horizontal spiral centrifuge to carry out centrifugal gained extracting solution in step s2, centrifugal rotational speed is 5000 r/min, then tubular-bowl centrifuge is crossed, centrifugal rotational speed is 14000 r/min, it is 40kDa, 5kDa hollow fiber ultrafiltration membrane that gained centrifugate crosses molecular weight cut-off successively, obtains filtrate;
S4 macroporous resin adsorption is separated: use in sodium carbonate regulating step s3 after gained filtrate Ph to 8.47, on normal temperature, AB-8 resin column adsorbs, and resin column blade diameter length ratio is 1:6, and upper column flow rate is 1.0BV/h, leaves standstill 1.5 h after upper prop completes; Under being equivalent to resin cumulative volume 7 times of deionized water normal temperature, carry out wash-out, elution flow rate is 2.5 BV/h, and then use 60% ethanol of 2BV to carry out wash-out to macroporous resin column, elution flow rate is 1.5BV/h, collects elutriant;
S5 nanofiltration, concentrated: to use 200Da nanofiltration membrane to carry out nanofiltration process gained elutriant in step s4, be then 75 DEG C in temperature, vacuum tightness is under the condition of-0.08Mpa ~-0.04Mpa, till the sharp degree 33 of vacuum concentration to hundred, obtains concentrated solution;
S6 is dry: gained concentrated solution in step s5 is carried out spraying dry, obtains the product of momordica glycoside V, weigh 6.248kg.
Result through liquid chromatograph detects: momordica glycoside V content is 63.71%, and momordica glycoside V total recovery is 72.38%.
embodiment 4
S1 raw material pre-treatment: get 1000 kg Grosvenor Momordica fresh fruit removal of impurities, cleans, suitably broken, is advisable not smash Grosvenor Momordica fruit seed;
S2 microwave counter current extracts: use microwave counter current extraction element to extract the Grosvenor Momordica after fragmentation, Extraction solvent is deionized water, forward feeding, anti-phase water inlet, the flowing of material and water is reverse continuous dynamic flow, and Extracting temperature is 78 DEG C, extraction time is 63 min, microwave power is 800w, and frequency is 6000MHz, and filter residue is forced to push to slag notch through spiral conveyer, spiral of slagging tap extrudes slag simultaneously, residue is discharged, and debris is extruded and mixed with feed liquid, obtains extracting solution after filtration;
S3 cascade filtration: use horizontal spiral centrifuge to carry out centrifugal gained extracting solution in step s2, centrifugal rotational speed is 5000 r/min, then tubular-bowl centrifuge is crossed, centrifugal rotational speed is 14000 r/min, it is 50kDa, 4kDa hollow fiber ultrafiltration membrane that gained centrifugate crosses molecular weight cut-off successively, obtains filtrate;
S4 macroporous resin adsorption is separated: use in sodium hydroxide regulating step s3 after gained filtrate Ph to 8.62, on normal temperature, D-101 resin column adsorbs, and resin column blade diameter length ratio is 1:6, and upper column flow rate is 0.75BV/h, leaves standstill 2 h after upper prop completes; Under being equivalent to resin cumulative volume 8 times of deionized water normal temperature, carry out wash-out, elution flow rate is 3 BV/h, and then use 70% ethanol of 2BV to carry out wash-out to macroporous resin column, elution flow rate is 1.25BV/h, collects elutriant;
S5 nanofiltration, concentrated: to use 150Da nanofiltration membrane to carry out nanofiltration process gained elutriant in step s4, be then 73 DEG C in temperature, vacuum tightness is under the condition of-0.08Mpa ~-0.04Mpa, till the sharp degree 31 of vacuum concentration to hundred, obtains concentrated solution;
S6 is dry: gained concentrated solution in step s5 is carried out spraying dry, obtains the product of momordica glycoside V, weigh 6.122kg.
Result through liquid chromatograph detects: momordica glycoside V content is 64.19%, and momordica glycoside V total recovery is 71.46%.
embodiment 5
S1 raw material pre-treatment: get 1000 kg Grosvenor Momordica fresh fruit removal of impurities, cleans, suitably broken, is advisable not smash Grosvenor Momordica fruit seed;
S2 microwave counter current extracts: use microwave counter current extraction element to extract the Grosvenor Momordica after fragmentation, Extraction solvent is deionized water, forward feeding, anti-phase water inlet, the flowing of material and water is reverse continuous dynamic flow, and Extracting temperature is 83 DEG C, extraction time is 57 min, microwave power is 700w, and frequency is 8000MHz, and filter residue is forced to push to slag notch through spiral conveyer, spiral of slagging tap extrudes slag simultaneously, residue is discharged, and debris is extruded and mixed with feed liquid, obtains extracting solution after filtration;
S3 cascade filtration: use horizontal spiral centrifuge to carry out centrifugal gained extracting solution in step s2, centrifugal rotational speed is 5000 r/min, then tubular-bowl centrifuge is crossed, centrifugal rotational speed is 14000 r/min, it is 40kDa, 3kDa hollow fiber ultrafiltration membrane that gained centrifugate crosses molecular weight cut-off successively, obtains filtrate;
S4 macroporous resin adsorption is separated: use in sodium hydroxide regulating step s3 after gained filtrate Ph to 8.33, on normal temperature, AB-8 resin column adsorbs, and resin column blade diameter length ratio is 1:6, and upper column flow rate is 0.5BV/h, leaves standstill 2 h after upper prop completes; Under being equivalent to resin cumulative volume 8 times of deionized water normal temperature, carry out wash-out, elution flow rate is 3 BV/h, and then use 65% ethanol of 2BV to carry out wash-out to macroporous resin column, elution flow rate is 1.0BV/h, collects elutriant;
S5 nanofiltration, concentrated: to use 200Da nanofiltration membrane to carry out nanofiltration process gained elutriant in step s4, be then 78 DEG C in temperature, vacuum tightness is under the condition of-0.08Mpa ~-0.04Mpa, till the sharp degree 34 of vacuum concentration to hundred, obtains concentrated solution;
S6 is dry: gained concentrated solution in step s5 is carried out spraying dry, obtains the product of momordica glycoside V, weigh 6.213kg.
Result through liquid chromatograph detects: momordica glycoside V content is 63.93%, and momordica glycoside V total recovery is 72.21%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (9)

1. from Grosvenor Momordica, extract a method for momordica grosvenori glycoside V, it is characterized in that comprising the following steps:
Raw material pre-treatment, Grosvenor Momordica is clean, broken;
Microwave counter current extracts: carry out microwave counter current extraction to the Grosvenor Momordica after pre-treatment, Extraction solvent is deionized water, and the flowing of material and water is reverse continuous dynamic flow, extrudes simultaneously, extrude debris and mix with feed liquid slag, obtains extracting solution after filtration;
Cascade filtration: extracting solution is centrifugal through horizontal screw centrifugal, tubular type first, after the first ultrafiltration and the second ultrafiltration filtrate, wherein, the rotating speed of described horizontal screw centrifugal is 2500 ~ 5000r/min, the centrifugal rotating speed of right tubular type is 12000 ~ 16000r/min, first ultrafiltration is through the ultra-filtration membrane that molecular weight cut-off is 30k ~ 50kDa, and the second ultrafiltration is through the ultra-filtration membrane that molecular weight cut-off is 4k ~ 6kDa;
Macroporous resin adsorption is separated: the Ph value regulating filtrate, and on normal temperature, macroporous resin column is adsorbed, and upper column flow rate is 0.5 ~ 1.5 BV/h, leaves standstill 1 ~ 2h after upper prop completes; Under being equivalent to resin cumulative volume 6 ~ 8 times of deionized water normal temperature, carry out wash-out, elution flow rate is 2 ~ 3BV/h, and then use hydrophilic solvent to carry out wash-out to macroporous resin column, elution flow rate is 1 ~ 2 BV/h, collects elutriant;
Nanofiltration, concentrated: to be used by elutriant nanofiltration membrane to carry out nanofiltration process, then till the sharp degree 30 ~ 35 of vacuum concentration to hundred, obtain concentrated solution;
Dry: after concentrated solution is carried out drying, to obtain momordica glycoside V.
2. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 1, it is characterized in that, during the extraction of microwave counter current process, Extracting temperature is 70 ~ 90 DEG C, and extraction time is 50 ~ 70 min, microwave power is 600 ~ 800W, frequency 6000 ~ 8000MHz.
3. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 1, is characterized in that, filtrate Ph is 8 ~ 9.
4. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 3, is characterized in that, the reagent regulating filtrate Ph is sodium hydroxide or sodium carbonate.
5. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 1, is characterized in that, described macroporous resin is D-101, AB-8 or HPD-100, and the blade diameter length ratio of resin column is 1:6.
6. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 5, is characterized in that, described hydrophilic solvent is volume fraction is 60 ~ 80% ethanolic solns, and the consumption of hydrophilic solvent is 2 ~ 3 BV.
7. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 1, is characterized in that, the molecular weight cut-off of described nanofiltration is 150 ~ 300Da.
8. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 7, is characterized in that, the thickening temperature of described vacuum concentration is 70 ~ 80 DEG C, and vacuum tightness is-0.08Mpa ~-0.04Mpa.
9. the method extracting momordica grosvenori glycoside V from Grosvenor Momordica according to claim 1 or 8 any one, is characterized in that, the mode of drying treatment is spraying dry.
CN201510033531.5A 2015-01-23 2015-01-23 Method for extracting mogroside V from momordica grosvenori Pending CN104558088A (en)

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Cited By (20)

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CN104892717A (en) * 2015-06-18 2015-09-09 湖南华诚生物资源有限公司 Industrial-grade preparative liquid chromatographic separation method of mogroside V
CN105685755A (en) * 2016-02-03 2016-06-22 桂林亦元生现代生物技术有限公司 Preparation method and preservation method of instant momordica grosvenori beverage
CN106008645A (en) * 2016-06-06 2016-10-12 江西海富生物工程有限公司 Method for extracting high-purity mogroside V from siraitia grosvenorii
CN107397103A (en) * 2017-08-25 2017-11-28 湖南华诚生物资源股份有限公司 A kind of preparation method of Momordica grosvenori decolouring flavor inspissated juice
CN107936079A (en) * 2017-11-28 2018-04-20 河南科恩生物科技有限公司 A kind of method for preparing high-purity momordica glycoside V
WO2018077147A1 (en) * 2016-10-24 2018-05-03 桂林吉福思罗汉果有限公司 Siraitia grosvenorii flavor instant drink and preparation method therefor
WO2018149065A1 (en) * 2017-02-20 2018-08-23 湖南华诚生物资源股份有限公司 Natural compound sweetener and preparation method therefor
WO2018196476A1 (en) * 2017-04-25 2018-11-01 广西甙元植物制品有限公司 Process for preparing decolored concentrated fresh momordica grosvenori juice
CN109247561A (en) * 2018-09-06 2019-01-22 湖南绿蔓生物科技股份有限公司 A kind of method and its application preparing Siraitia grosvenorii sweetener composition from Siraitia grosvenorii
CN110669095A (en) * 2019-10-14 2020-01-10 广西壮族自治区科学技术情报研究所 Extraction method of high-purity mogroside V
WO2020103798A1 (en) * 2018-11-19 2020-05-28 桂林吉福思罗汉果有限公司 Fermented monk fruit flavored beverage and method for preparation thereof
CN111978365A (en) * 2020-09-10 2020-11-24 上海诺德生物实业有限公司 Preparation method of mogroside V-containing mogroside
CN112121462A (en) * 2020-10-23 2020-12-25 张洪江 A reciprocal extraction equipment of multilayer for crops fermentation product
CN113603742A (en) * 2021-08-06 2021-11-05 湖南华诚生物资源股份有限公司 Preparation method of mogroside V
CN113861260A (en) * 2021-09-07 2021-12-31 桂林三棱生物科技有限公司 Preparation method of momordica grosvenori sweet glycoside compounds
CN113956322A (en) * 2021-11-17 2022-01-21 湖南华诚生物资源股份有限公司 Method for removing harmful substances in momordica grosvenori extract
CN115109112A (en) * 2022-08-10 2022-09-27 刘庚贵 Industrial production method of mogroside for improving mogroside V content
US11464247B2 (en) 2006-09-07 2022-10-11 Guilin Gfs Monk Fruit Corp. Sweetening compositions and processes for preparing them
CN115403647A (en) * 2022-08-23 2022-11-29 刘庚贵 Method for industrially producing mogroside, momordica fructose/wine and mannitol by using fresh momordica grosvenori
US11576412B2 (en) 2016-10-24 2023-02-14 Guilin Gfs Monk Fruit Corporation Extracts from fruits of the Cucurbitaceae family, and methods of preparing thereof

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US11464247B2 (en) 2006-09-07 2022-10-11 Guilin Gfs Monk Fruit Corp. Sweetening compositions and processes for preparing them
CN104892717A (en) * 2015-06-18 2015-09-09 湖南华诚生物资源有限公司 Industrial-grade preparative liquid chromatographic separation method of mogroside V
CN104892717B (en) * 2015-06-18 2017-05-31 湖南华诚生物资源股份有限公司 A kind of technical grade preparative liquid chromatography separation method of momordica glycoside V
CN105685755A (en) * 2016-02-03 2016-06-22 桂林亦元生现代生物技术有限公司 Preparation method and preservation method of instant momordica grosvenori beverage
CN106008645A (en) * 2016-06-06 2016-10-12 江西海富生物工程有限公司 Method for extracting high-purity mogroside V from siraitia grosvenorii
CN106008645B (en) * 2016-06-06 2017-12-15 江西海富生物工程有限公司 A kind of method that momordica grosvenori glycoside V is extracted from Momordica grosvenori
US10743573B2 (en) 2016-06-06 2020-08-18 Jiangxi Haifu Bioengineering Co., Ltd. Method for extracting high-purity mogroside V from Siraitia grosvenorii
WO2018077147A1 (en) * 2016-10-24 2018-05-03 桂林吉福思罗汉果有限公司 Siraitia grosvenorii flavor instant drink and preparation method therefor
US11576412B2 (en) 2016-10-24 2023-02-14 Guilin Gfs Monk Fruit Corporation Extracts from fruits of the Cucurbitaceae family, and methods of preparing thereof
WO2018149065A1 (en) * 2017-02-20 2018-08-23 湖南华诚生物资源股份有限公司 Natural compound sweetener and preparation method therefor
WO2018196476A1 (en) * 2017-04-25 2018-11-01 广西甙元植物制品有限公司 Process for preparing decolored concentrated fresh momordica grosvenori juice
CN107397103A (en) * 2017-08-25 2017-11-28 湖南华诚生物资源股份有限公司 A kind of preparation method of Momordica grosvenori decolouring flavor inspissated juice
CN107936079B (en) * 2017-11-28 2020-05-01 河南中大恒源生物科技股份有限公司 Method for preparing high-purity mogroside V
CN107936079A (en) * 2017-11-28 2018-04-20 河南科恩生物科技有限公司 A kind of method for preparing high-purity momordica glycoside V
CN109247561A (en) * 2018-09-06 2019-01-22 湖南绿蔓生物科技股份有限公司 A kind of method and its application preparing Siraitia grosvenorii sweetener composition from Siraitia grosvenorii
WO2020103798A1 (en) * 2018-11-19 2020-05-28 桂林吉福思罗汉果有限公司 Fermented monk fruit flavored beverage and method for preparation thereof
CN113272414A (en) * 2018-11-19 2021-08-17 桂林吉福思罗汉果股份有限公司 Fermented momordica grosvenori flavored beverage and preparation method thereof
CN110669095B (en) * 2019-10-14 2022-05-27 广西壮族自治区科学技术情报研究所 Extraction method of high-purity mogroside V
CN110669095A (en) * 2019-10-14 2020-01-10 广西壮族自治区科学技术情报研究所 Extraction method of high-purity mogroside V
CN111978365A (en) * 2020-09-10 2020-11-24 上海诺德生物实业有限公司 Preparation method of mogroside V-containing mogroside
CN112121462A (en) * 2020-10-23 2020-12-25 张洪江 A reciprocal extraction equipment of multilayer for crops fermentation product
CN113603742A (en) * 2021-08-06 2021-11-05 湖南华诚生物资源股份有限公司 Preparation method of mogroside V
CN113861260A (en) * 2021-09-07 2021-12-31 桂林三棱生物科技有限公司 Preparation method of momordica grosvenori sweet glycoside compounds
CN113956322A (en) * 2021-11-17 2022-01-21 湖南华诚生物资源股份有限公司 Method for removing harmful substances in momordica grosvenori extract
CN115109112A (en) * 2022-08-10 2022-09-27 刘庚贵 Industrial production method of mogroside for improving mogroside V content
CN115109112B (en) * 2022-08-10 2024-03-15 刘庚贵 Industrial production method of mogroside for improving content of mogroside V
CN115403647A (en) * 2022-08-23 2022-11-29 刘庚贵 Method for industrially producing mogroside, momordica fructose/wine and mannitol by using fresh momordica grosvenori
CN115403647B (en) * 2022-08-23 2023-09-29 刘庚贵 Method for industrially producing mogroside, momordica grosvenori/wine and mannitol from fresh momordica grosvenori

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