CN106943447A - A kind of preparation method of Fructus Monordicae extract - Google Patents

A kind of preparation method of Fructus Monordicae extract Download PDF

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CN106943447A
CN106943447A CN201710212466.1A CN201710212466A CN106943447A CN 106943447 A CN106943447 A CN 106943447A CN 201710212466 A CN201710212466 A CN 201710212466A CN 106943447 A CN106943447 A CN 106943447A
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momordica grosvenori
extract
resin
fructus monordicae
monordicae extract
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谢海峰
胡云岭
罗明锋
谢期林
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Chengdu Universal Drug Development Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/42Cucurbitaceae (Cucumber family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Botany (AREA)
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  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
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  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses a kind of method that Continuous Countercurrent Extraction prepares Fructus Monordicae extract, this method is inputted after directly Momordica grosvenori is crushed and extracted in Continuous Countercurrent Extraction equipment, then by filtering and impurity removing, except color, absorption exquisiteness, concentrated spray drying, finally give Fructus Monordicae extract, wherein Mogroside V content >=40% in Fructus Monordicae extract.The preparation method that the present invention is provided, whole process is simply used as Hydrolysis kinetics solvent, safety non-toxic with pure water or hydrous ethanol.Method used herein is simplified, can continuous operation, saved a large amount of manpower and materials, required Preparation equipment and site requirements is low, be adapted to industrialized production.

Description

A kind of preparation method of Fructus Monordicae extract
Technical field
Separation preparation field is extracted the invention belongs to active ingredient of natural plant, is related to a kind of preparation of Fructus Monordicae extract Method, more particularly to a kind of Mogroside V content are more than the preparation method of 40% Fructus Monordicae extract.
Background technology
Momordica grosvenori is the fruit that Momordica grosvenori belongs to cucurbitaceous plant, is a kind of multipurpose integration of drinking and medicinal herbs medicinal material.Arhat fruity pole It is sweet, cool in nature, nontoxic, enter spleen and lung warp, with removing heat from the lung to relieve cough, relax bowel, clearing heat and detoxicating, beneficial liver spleen, calmness are quenched the thirst, promote stomach A variety of pharmacological effects such as enteron aisle function, antiviral, antitumor, hypoglycemic step-down.Numerous studies data shows that Momordica grosvenori not only contains A variety of pharmacological components, and can be used as the sweetener of low sugar contents, therefore it is widely used in food, health care at present Product, medicine, beverage, cosmetic industry.
Contain a variety of saponin(e active components in Momordica grosvenori, wherein momordica grosvenori glycoside V is one of leading indicator composition, arhat Fruit saponin(e aglycon has typical cucurbitane type tetracyclic triterpene structure.Momordica grosvenori glycoside V can be used as evaluation Fructus Monordicae extract matter Measure good and bad index composition because its aglycon combines glycosyl and soluble in water, ethanol polar solvent, be insoluble in acetone, The organic solvents such as ethyl acetate, end-product is white amorphous powder.
The research prepared on Fructus Monordicae extract is concentrated mainly on the country, and Patents documents report is more, but really The less of production can be applied to, the following aspects is mainly reflected in:(1)Process is cumbersome, and yield is low;(2)Using a large amount of Organic solvent, high to equipment requirement, input is big;(3)Technical process energy consumption is big, high cost;(4)Other materials are introduced in process, Influence product quality.As CN101029071B discloses the method that high-purity Momordia grosvenori aglycone V is prepared from Momordica grosvenori, this method It is that Momordica grosvenori dry fruit is subjected to alcohol extracting, concentration, through ethyl acetate, extracting n-butyl alcohol, then using silicagel column, C18 reverse phase silica gels The sweet glycosides V products of high-purity are obtained after column chromatography, drying, this method major defect is technique is cumbersome, solvent loss is big, yield is low, no Beneficial to scale industrial production;CN100572552C discloses Fructus Monordicae extract and its preparation of momordica grosvenori glycoside V >=40% Method, this method is, by the water extraction of Momordica grosvenori fresh fruit, concentration, enzymolysis, macroporous resin adsorption, ion-exchange resin decolorization, most to pass through afterwards Concentrate drying obtains product, and this method causes the subsequent treatment cost of resin larger, be unfavorable for due to not filtered before upper prop Continuous production;CN101407535B discloses a kind of preparation method of high-purity Momordica grosvenori mogroside V, and this method is to use one The Fructus Monordicae extract for determining purity is raw material, is dissolved through methanol, acetone extract, purification on normal-phase silica gel are adsorbed, separated, crystallized and recrystallization Obtain final products, this method technique is simple, but during used substantial amounts of organic solvent, the requirement to Workplace compared with Height, the product obtained in addition also has certain organic solvent residual, influences quality;CN101863946B discloses a kind of dry sieve The method that Chinese fruit extracts high content Momordica grosvenori mogroside V, this method be by Momordica grosvenori dry fruit it is broken after, through alcohol extracting, concentration, centrifugation, Macroporous resin adsorption separation, ion-exchange resin decolorization, last concentrated, drying, obtain finished product, the method is due to filtered place Reason so that big molecular impurity is more in upper prop liquid, influences the absorption property of resin, utilization rate is low and subsequent treatment difficulty relatively Greatly, product cost is higher.
The content of the invention
It is an object of the invention to provide a kind of Fructus Monordicae extract preparation method suitable for industrialized production, this method The defect of above-mentioned existing technology of preparing is can solve the problem that, being capable of continuous production and with low cost, low energy consumption, high income, safety Efficiently the features such as.
A kind of preparation method of Fructus Monordicae extract, comprises the following steps:
(1)Medicinal material pre-treatment:Momordica grosvenori is suitably crushed, the material after crushing is not broken for degree with arhat fruit seed;
(2)Continuous Countercurrent Extraction:By in the Momordica grosvenori input continuous flow upstream tubular type extractor after break process, inversely input pure Water, its reclaimed water is 5-8 with quality of medicinal material ratio:1, and it is 45-85 DEG C to keep Continuous Countercurrent Extraction pipe temperature, extracts 30-60min, Obtain Momordica grosvenori extract solution;
(3)Centrifugal filtration:Obtained Momordica grosvenori extract solution is inputted into liquid-slag separation device, expression separation is carried out by 40-100kg/h Bulky grain material residue is removed, high speed centrifugation device is then inputted, with 2000-6000r/min centrifugation 20-60min, obtains sieve Chinese berry extract centrifugate;
(4)Except color:Centrifugate is imported into strong alkalinity anion macropore decolorizing resin, being eluted to efflux without sweet taste with purified water is Only, Fructus Monordicae extract destainer is obtained, wherein decolorizing resin consumption is 0.01-0.1 times of centrifugate volume, it is therefore preferable to 0.05-0.8 times;
(5)Fluoropolymer resin separation and purification:Destainer is imported into fluoropolymer resin adsorption, 20%-80% ethanol waters are used Untill efflux is eluted to without sweet taste, final Momordica grosvenori pregnant solution is obtained, wherein fluoropolymer resin consumption is the 0.02- of destainer 0.08 times, it is therefore preferable to 0.04-0.06 times;
(6)Concentrated spray is dried:Density will be concentrated to below 85 DEG C of pregnant solution vacuum decompression for 1.12-1.25g/ml, Ran Houzai Spray drying obtains final finished, and finished product is white amorphous powder or off-white color material, wherein Mogroside V content >= 40%.This finished product can further be refining to obtain the higher Fructus Monordicae extract of Mogroside V content.
Further, step(4)Described in decolorizing resin from D151, D303, S-8, D-309, LX-700, D290 or XDA-7 resins, wherein it is preferred that D303, D290 or LX-700 resin;The decolorizing resin post blade diameter length ratio is 1:2-1:10, its In be preferably 1:3-1:5.
Further, step(5)Described in fluoropolymer resin refer to styrene, methacrylate or styrene and first Base acrylate copolymer be matrix polymer filler, preferred substrate be styrene and methacrylate copolymer, it is selected Packing material size is 5 μm-300 μm, it is therefore preferable to 50 μm-150 μm, and selected filler aperture is 100-1000, it is therefore preferable to 300-500Å。
Advantage of the present invention:
1. the present invention will directly take the mode of Continuous Countercurrent Extraction to be extracted after Momordica grosvenori break process, letter, which is saved, significantly extracts Step, and can continuously produce, one side sample introduction is while slag tap.The whole pure water or aqueous harmless using low toxicity in preparation process Ethanol produces highly effective and safe as Hydrolysis kinetics solvent, and the requirement for production site, equipment is low, is adapted to industrialization extensive Production.
2. the present invention use strong alkalinity anion macroreticular resin carry out preliminary decolouring and removal of impurities handle after be introduced directly into Styrene and methacrylate copolymer carry out further separation exquisiteness, final concentrated spray for the microspheric filler of matrix End-product is dried to obtain, whole process is carried out continuously, resin regenerating easily recycling used greatly improves preparation effect Rate, saves the time, simplifies process, be conducive to process control and quality control, be especially suitable for industrialized production.
3. end-product active constituent content is high, impurity content is low, Mogroside V content in gained Fructus Monordicae extract >= 40%。
Embodiment
Following examples are intended to further illustrate the present invention, rather than limitation of the present invention, and all are based on institute of the present invention The improvement made is all within the scope of the present invention.
Embodiment 1
(1)Medicinal material pre-treatment:Momordica grosvenori 1000kg is suitably crushed, the material after crushing is not broken for degree with arhat fruit seed;
(2)Continuous Countercurrent Extraction:Momordica grosvenori after break process is inputted in continuous flow upstream tubular type extractor, by solvent medicinal material matter Amount compares 8:1 inversely inputs the pure water of 8 times of quality of medicinal materials, and it is 65 DEG C to keep Continuous Countercurrent Extraction pipe temperature, is extracted 45min, obtains Momordica grosvenori extract solution;
(3)Centrifugal filtration:Obtained Momordica grosvenori extract solution is inputted into liquid-slag separation device, expression separation removing is carried out by 80kg/h Bulky grain material residue, then input high speed centrifugation device, with 4500r/min centrifugation 30min, obtain Fructus Monordicae extract from Heart liquid;
(4)Except color:Centrifugate is imported into D303 decolorizing resins, untill being eluted to efflux without sweet taste with purified water, arhat is obtained Berry extract destainer, wherein decolorizing resin consumption are 0.03 times of centrifugate volume;
(5)Fluoropolymer resin separation and purification:Adsorption during destainer is imported using styrene as the polymer filler of matrix, is used Untill 50% edible ethanol is eluted to efflux without sweet taste, final Momordica grosvenori pregnant solution, wherein styrenic polymer resins are obtained Consumption is 0.04 times of destainer;
(6)Concentrated spray is dried:Density will be concentrated to below 85 DEG C of pregnant solution vacuum decompression for 1.12-1.25g/ml, Ran Houzai Spray drying obtains final finished, and finished product is white amorphous powder or off-white color material, and wherein Mogroside V content is 45.23%。
Embodiment 2
(1)Medicinal material pre-treatment:500kg Momordica grosvenoris are suitably crushed, the material after crushing is not broken for degree with arhat fruit seed;
(2)Continuous Countercurrent Extraction:Momordica grosvenori after break process is inputted in continuous flow upstream tubular type extractor, with solvent medicinal material matter Amount compares 6:1 ratio inversely inputs the pure water of 6 times of quality of medicinal materials, and it is 55 DEG C to keep Continuous Countercurrent Extraction pipe temperature, is carried 30min is taken, Momordica grosvenori extract solution is obtained;
(3)Centrifugal filtration:Obtained Momordica grosvenori extract solution is inputted into liquid-slag separation device, expression separation removing is carried out by 60kg/h Bulky grain material residue, then input high speed centrifugation device, with 2000r/min centrifugation 55min, obtain Fructus Monordicae extract from Heart liquid;
(4)Except color:Centrifugate is imported into D290 decolorizing resins, untill being eluted to efflux without sweet taste with purified water, arhat is obtained Berry extract destainer, wherein decolorizing resin consumption are 0.05 times of centrifugate volume;
(5)Fluoropolymer resin separation and purification:It is enriched with during destainer is imported using methacrylate as the polymer filler of matrix It is refined, untill being eluted to efflux without sweet taste with 35% edible ethanol, final Momordica grosvenori pregnant solution is obtained, wherein styrene gathers Polymer resin consumption is 0.06 times of destainer;
(6)Concentrated spray is dried:Density will be concentrated to below 85 DEG C of pregnant solution vacuum decompression for 1.12-1.25g/ml, Ran Houzai Spray drying obtains final finished, and finished product is white amorphous powder or off-white color material, and wherein Mogroside V content is 49.56%。
Embodiment 3
(1)Medicinal material pre-treatment:Momordica grosvenori 800kg is suitably crushed, the material after crushing is not broken for degree with arhat fruit seed;
(2)Continuous Countercurrent Extraction:Momordica grosvenori after break process is inputted in continuous flow upstream tubular type extractor, with solvent medicinal material matter Amount compares 6:1 reverse input purified water, and it is 45 DEG C to keep Continuous Countercurrent Extraction pipe temperature, extracts 30min, obtains Momordica grosvenori extraction Liquid;
(3)Centrifugal filtration:Obtained Momordica grosvenori extract solution is inputted into liquid-slag separation device, expression separation removing is carried out by 88kg/h Bulky grain material residue, then input high speed centrifugation device, with 6000r/min centrifugation 30min, obtain Fructus Monordicae extract from Heart liquid;
(4)Except color:Centrifugate is imported into LX-700 decolorizing resins, untill being eluted to efflux without sweet taste with purified water, sieve is obtained Chinese berry extract destainer, wherein decolorizing resin consumption are 0.05 times of centrifugate volume;
(5)Fluoropolymer resin separation and purification:Destainer is imported using styrene and methacrylate copolymer as the poly- of matrix Adsorption in compound filler, untill being eluted to efflux without sweet taste with 65% edible ethanol, obtains final Momordica grosvenori enrichment Liquid, wherein styrenic polymer resins consumption are 0.06 times of destainer;
(6)Concentrated spray is dried:Density will be concentrated to below 85 DEG C of pregnant solution vacuum decompression for 1.12-1.25g/ml, Ran Houzai Spray drying obtains final finished, and finished product is white amorphous powder or off-white color material, and wherein Mogroside V content is 42.38%。

Claims (5)

1. a kind of preparation method of Fructus Monordicae extract, it is characterised in that the preparation method of the extract comprises the following steps:
(1)Medicinal material pre-treatment:Momordica grosvenori is suitably crushed, the material after crushing is not broken for degree with arhat fruit seed;
(2)Continuous Countercurrent Extraction:By in the Momordica grosvenori input continuous flow upstream tubular type extractor after break process, reverse input is purified Water, wherein solvent quality of medicinal material ratio are 5-8:1, and it is 45-85 DEG C to keep Continuous Countercurrent Extraction pipe temperature, extracts 30-60min, Obtain Momordica grosvenori extract solution;
(3)Centrifugal filtration:Obtained Momordica grosvenori extract solution is inputted into liquid-slag separation device, expression separation is carried out by 40-100kg/h Bulky grain material residue is removed, high speed centrifugation device is then inputted, with 2000-6000r/min centrifugation 20-60min, obtains sieve Chinese berry extract centrifugate;
(4)Except color:Centrifugate is imported into strong alkalinity anion macropore decolorizing resin, being eluted to efflux without sweet taste with purified water is Only, Fructus Monordicae extract destainer is obtained;
(5)Fluoropolymer resin separation and purification:Destainer is imported into fluoropolymer resin adsorption, it is water-soluble with 20%-80% ethanol Untill liquid is eluted to efflux without sweet taste, final Momordica grosvenori pregnant solution is obtained;
(6)Concentrated spray is dried:Density will be concentrated to below 85 DEG C of pregnant solution vacuum decompression for 1.12-1.25g/ml, Ran Houzai Spray drying obtains final finished, and finished product is white amorphous powder or off-white color material.
2. such as step in claim 1(4)The decolorizing resin, its consumption is 0.01-0.1 times of centrifugate volume, preferably For 0.05-0.8 times.
3. such as step in claim 1(4)Described in decolorizing resin, can from D151, D303, S-8, D-309, LX-700, D290 or XDA-7 resins, wherein it is preferred that D303, D290 or LX-700 resin;The decolorizing resin post blade diameter length ratio is 1:2- 1:10, wherein preferably 1:3-1:5.
4. such as step in claim 1(5)Described fluoropolymer resin, its consumption is 0.02-0.08 times of destainer, preferably For 0.04-0.06 times.
5. such as step in claim 1(5)Described in fluoropolymer resin, refer to styrene, methacrylate or styrene With methacrylate copolymer be matrix polymer filler, preferred substrate be styrene and methacrylate copolymer, Selected packing material size is 5 μm-300 μm, it is therefore preferable to 50 μm-150 μm, and selected filler aperture is 100-1000, preferably Ground is 300-500.
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CN113068815A (en) * 2021-04-14 2021-07-06 湖南华诚生物资源股份有限公司 Momordica grosvenori sugar capable of improving sweet taste and preparation method thereof
CN113634009A (en) * 2021-07-30 2021-11-12 桂林航天工业学院 Preparation method and processing device of mogroside
CN113854533A (en) * 2021-09-30 2021-12-31 湖南华诚生物资源股份有限公司 Method for preparing mogroside, momordica grosvenori phenolic acid and momordica grosvenori concentrated juice from fresh momordica grosvenori
CN114159829A (en) * 2021-12-09 2022-03-11 广西甙元植物制品有限公司 Processing equipment and preparation method of mogroside

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CN113068815A (en) * 2021-04-14 2021-07-06 湖南华诚生物资源股份有限公司 Momordica grosvenori sugar capable of improving sweet taste and preparation method thereof
CN113634009A (en) * 2021-07-30 2021-11-12 桂林航天工业学院 Preparation method and processing device of mogroside
CN113854533A (en) * 2021-09-30 2021-12-31 湖南华诚生物资源股份有限公司 Method for preparing mogroside, momordica grosvenori phenolic acid and momordica grosvenori concentrated juice from fresh momordica grosvenori
CN113854533B (en) * 2021-09-30 2023-09-05 湖南华诚生物资源股份有限公司 A method for preparing mogroside, mogrolic acid, fructus Siraitiae Grosvenorii concentrated juice and fructus Siraitiae Grosvenorii fructose from fresh fructus Siraitiae Grosvenorii
CN114159829A (en) * 2021-12-09 2022-03-11 广西甙元植物制品有限公司 Processing equipment and preparation method of mogroside
CN114159829B (en) * 2021-12-09 2022-06-10 广西甙元植物制品有限公司 Processing equipment and preparation method of mogroside

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Application publication date: 20170714