CN107163098B - A kind of extracting method of natural high-purity mogroside - Google Patents
A kind of extracting method of natural high-purity mogroside Download PDFInfo
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- CN107163098B CN107163098B CN201710509741.6A CN201710509741A CN107163098B CN 107163098 B CN107163098 B CN 107163098B CN 201710509741 A CN201710509741 A CN 201710509741A CN 107163098 B CN107163098 B CN 107163098B
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- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
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Abstract
The invention discloses a kind of extracting methods of natural high-purity mogroside, this method is after mangosteen powder to be broken into nanoscale fine powder, medicinal extract is concentrated to get after water ultrasonic extraction, the oil-soluble impurities in medicinal extract are removed with the supermolecule solvent that tetrahydrofuran and water are formed again after medicinal extract is dissolved with water, the extract for being dried to obtain high-purity mogroside is finally washed with ethyl acetate.This method does not need to chromatograph using special seperation film and column, and extraction procedure is simple, and extraction time is short and significantly reduces the usage amount of organic solvent, highly efficient and environmentally friendly.In addition, the high-purity mogroside compound obtained through the present invention can be directly as food sweetening agent.
Description
Technical field
The present invention relates to effective ingredients in plant extractive technique fields, are related to a kind of extraction side of natural high-purity mogroside
Method, obtained high-purity mogroside can be directly as in the natural sweetener of food.
Background technique
The mountain area of Siraitia grosvenorii main product China hazard prevention Lingui County and Yongfu county, saving at other occasionally has plantation.Arhat
Fruits nutritive value is very high, is rich in the various nutrients such as vitamin C, E, fructose, human body necessary amino acid, microelement,
And a variety of active ingredients such as flavones, polysaccharide, sweet tea glucoside and polyphenol.Japanese scholars bamboo Ben Changsong the study found that Siraitia grosvenorii to various
What disease played a major role is exactly 300 times than granulated sugar sweet tea contained in fruit of substance --- Momordica-Glycosides, and scientific name is " cucurbit
Plain alkane triterpene " is one of the sweet substance other than the granulated sugar for belonging to triterpene system, due to the sweet taste of Siraitia grosvenorii be a kind of non-saccharide at
Point, so diabetes patient can also take.Currently, replacing the other sweeteners in part for making various foods using the high sweet taste of Siraitia grosvenorii
Product, including beverage, Yoghourt, fruit vinegar, ice cream, wine, rock sugar, nutrient powder etc..
But the traditional extracting method of mogroside uses a large amount of organic solvents, extraction efficiency is not high, high-purity Siraitia grosvenorii
Glucoside preparation method usually requires in such a way that column chromatographs and film filters, these method production cycles are long and at high cost.Patent
CN103570789 A " a kind of preparation method of high-purity mogroside " mentions-is condensed into medicinal extract-ether using water, ethyl acetate mixes
Close liquid two-phase liquid-liquid extraction-ether, ethyl acetate mixtures/dipotassium hydrogen phosphate aqueous two-phase extraction-high molecular polymer back extraction-just
Butanol liquid-liquid extraction-concentrate drying preparation flow has obtained high-purity mogroside, but this method complex steps, time-consuming consume
Power, and a large amount of organic solvent has been used, it causes serious pollution to the environment.Therefore, exploitation is efficient, convenient, green high-purity mogroside
Extracting method played an important role to production efficiency and environmental protection is improved.
Summary of the invention
The purpose of the present invention is open a kind of efficient, convenient, the extracting method of green high-purity mogroside.
The technical scheme is that a kind of extracting method of natural high-purity mogroside, it is characterised in that including following
Step:
(1) Siraitia grosvenorii is cleaned with clear water, it is after natural drying, 10-12 hours dry in vacuum oven at 40-50 DEG C
Afterwards, after being smashed it through 60 meshes using medicinal herb grinder, the powder after sieving is further crushed and obtains partial size and is less than
The nanoscale micropowders of 200nm；
(2) after Siraitia grosvenorii micropowders being mixed with water by the mass volume ratio of 1:5-20, in 200-300W, 30-40 DEG C
Under conditions of ultrasound after 15-25 minutes, by filter residue ultrasonic extraction 2-3 times again after filtering, combined extract, vacuum distillation is obtained
Extract medicinal extract；
(3) after mixing by a certain amount of tetrahydrofuran, alkanol, water, after standing 1-2 hours naturally, system split-phase is taken
The supermolecule solvent of nano-scale is mutually obtained on out, alkanol is one of n-hexyl alcohol, n-octyl alcohol, Decanol, tetrahydrofuran, alkane
Alcohol, water account for the 15-20 of total system volume respectively;5-15;65-85%, the sum of three's percent by volume are 100%.；
(4) medicinal extract being dissolved in after water and a certain amount of supermolecule solvent is added, vortex is centrifuged after 10-20 seconds, clear liquid is removed, on
After clear liquid uses supermolecule solvent extraction 2-3 times again, clear liquid is evaporated under reduced pressure to obtain medicinal extract, medicinal extract is done after being washed with ethyl acetate
It is dry, obtain the extract of high-purity mogroside.
Further, there are the micellas that partial size is 50-200nm in nano-scale supermolecule described in step (3).
Further, the concentration of medicinal extract aqueous solution described in step (4) is 0.2-0.4g/mL；The supermolecule solvent with
The volume ratio of medicinal extract aqueous solution is 1:10.
Further, the total sweet tea glucoside purity of Siraitia grosvenorii is not less than in the extract of high-purity mogroside described in step (4)
95%, Momordica grosvenori mogroside V purity is not less than 68%.
The features of the present invention is
Mangosteen powder is broken into nanometer grade powder using superfine communication technique by high-purity mogroside prepared by the present invention, is reinforced
The leaching rate of effective component improves extraction efficiency；Extraction procedure is reduced using ultrasonic wave assisted extraction.Using tetrahydrofuran, alkane
The supermolecule solvent that alcohol, water are formed removes fat-soluble compound in Fructus Monordicae extract；Extracting method of the invention and traditional
Method is not needed to be chromatographed using special seperation film and column, reduces production cost compared to easy to operate；With existing patent skill
Art is compared, and this method extraction procedure is simple, and extraction time is short and significantly reduces the usage amount of organic solvent, it is highly efficient and
Environmental protection.In addition, the high-purity mogroside compound obtained through the present invention can be directly as food sweetening agent.
Specific embodiment
Embodiment one
Siraitia grosvenorii is cleaned with clear water, after natural drying, after 11 hours dry in 40 DEG C of vacuum ovens, utilizes Chinese medicine
After pulverizer is smashed it through 60 meshes, the powder after sieving is further crushed and obtains nanoscale micropowders；By 300g
After Siraitia grosvenorii micropowders are mixed with 3L water, ultrasound after twenty minutes, surpasses filter residue after filtering again under conditions of 200W, 45 DEG C
Sound extracts 2 times, combined extract, and vacuum distillation obtains extracting medicinal extract；A certain amount of 200mL tetrahydrofuran, 100mL is just pungent
Alcohol, 700mL water after mixing, naturally stand 1 hour after, system split-phase, remove phase obtain nano-scale supermolecule it is molten
Agent；Medicinal extract is dissolved in after water and obtains 0.3g/mL medicinal extract aqueous solution, the water-soluble supermolecule solvent that 75mL is added of 1L medicinal extract is taken, is vortexed
It is centrifuged after 20 seconds, removes clear liquid and be evaporated under reduced pressure clear liquid to obtain medicinal extract after supernatant uses the solvent extraction of 50mL supermolecule 3 times again,
Medicinal extract is dry after being washed with ethyl acetate, obtains the extract of high-purity mogroside, and wherein the total sweet tea glucoside purity of Siraitia grosvenorii is 97%,
Momordica grosvenori mogroside V purity is 70%.
Embodiment two
Siraitia grosvenorii is cleaned with clear water, after natural drying, after 10 hours dry in 45 DEG C of vacuum ovens, utilizes Chinese medicine
After pulverizer is smashed it through 60 meshes, the powder after sieving is further crushed and obtains nanoscale micropowders；By 500g
After Siraitia grosvenorii micropowders are mixed with 12L water, under conditions of 250W, 50 DEG C after ultrasound 25 minutes, after filtering again by filter residue
Ultrasonic extraction 3 times, combined extract, vacuum distillation obtains extracting medicinal extract；By a certain amount of 350mL tetrahydrofuran, the 200mL positive last of the ten Heavenly stems
Alcohol, 1000mL water after mixing, naturally stand 1 hour after, system split-phase, remove phase obtain nano-scale supermolecule it is molten
Agent；Medicinal extract is dissolved in after water and obtains 0.35g/mL medicinal extract aqueous solution, takes the water-soluble supermolecule solvent that 150mL is added of 1.5L medicinal extract,
It is centrifuged after being vortexed 15 seconds, removes clear liquid and be evaporated under reduced pressure to obtain by clear liquid after supernatant uses the solvent extraction of 100mL supermolecule 2 times again
Medicinal extract, medicinal extract is dry after being washed with ethyl acetate, obtains the extract of high-purity mogroside, wherein the total sweet tea glucoside purity of Siraitia grosvenorii is
96.2%, Momordica grosvenori mogroside V purity is 71%.
Embodiment three
Siraitia grosvenorii is cleaned with clear water, after natural drying, after 12 hours dry in 40 DEG C of vacuum ovens, utilizes Chinese medicine
After pulverizer is smashed it through 60 meshes, the powder after sieving is further crushed and obtains nanoscale micropowders；By 400g
After Siraitia grosvenorii micropowders are mixed with 10L water, under conditions of 300W, 40 DEG C after ultrasound 25 minutes, after filtering again by filter residue
Ultrasonic extraction 2 times, combined extract, vacuum distillation obtains extracting medicinal extract；By a certain amount of 200mL tetrahydrofuran, 150mL just oneself
Alcohol, 800mL water after mixing, naturally stand 1 hour after, system split-phase, remove phase obtain nano-scale supermolecule it is molten
Agent；Medicinal extract is dissolved in after water and obtains 0.25g/mL medicinal extract aqueous solution, takes the water-soluble supermolecule solvent that 100mL is added of 1.5L medicinal extract,
It is centrifuged after being vortexed 20 seconds, removes clear liquid and be evaporated under reduced pressure to obtain by clear liquid after supernatant uses the solvent extraction of 80mL supermolecule 2 times again
Medicinal extract, medicinal extract is dry after being washed with ethyl acetate, obtains the extract of high-purity mogroside, wherein the total sweet tea glucoside purity of Siraitia grosvenorii is
97.2%, Momordica grosvenori mogroside V purity is 72%.
Comparative example one
500g Siraitia grosvenorii is cleaned with clear water, after being mixed after its grinding and sieving with 3L water using medicinal herb grinder,
It is extracted repeatedly under the conditions of 100 DEG C 3 times, 1 hour every time, combined extract, vacuum distillation obtained extracting medicinal extract；Medicinal extract is soluble in water
It is made into 500mL aqueous solution, 500mL ether is added: ethyl acetate mixtures volume ratio is 7:3, is extracted 4 times, and combining extraction liquid returns
Receive, into aqueous solution be added 50g dipotassium hydrogen phosphate, then plus 500mL ethyl alcohol: ethyl acetate mixtures volume ratio be 9:1 mixing
Liquid, concussion stand, formed aqueous two-phase, obtain phase be ethyl alcohol, ethyl acetate hybrid extraction liquid, hybrid extraction liquid with
The poly- propionamide aqueous solution extraction of 500mL1.5% is primary, ethyl alcohol, ethyl acetate hybrid extraction liquid evaporated under reduced pressure, both high-purity arhat
The extract of fruit glucoside, wherein the total sweet tea glucoside purity of Siraitia grosvenorii is 95%, and Momordica grosvenori mogroside V purity is 65%.
The comparison difference that embodiment 1-3 and comparative example 1 prepare high-purity mogroside is as shown in table 1.
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention,
Obviously the present invention specific implementation is not subject to the restrictions described above, as long as use the inventive concept and technical scheme of the present invention into
The improvement of capable various unsubstantialities, or not improved the conception and technical scheme of the invention are directly applied to other occasions
, it is within the scope of the present invention.
Claims (4)
1. a kind of extracting method of natural high-purity mogroside, it is characterised in that include the next steps following steps:
(1) Siraitia grosvenorii is cleaned with clear water, after natural drying, after 10-12 hours dry in vacuum oven at 40-50 DEG C,
After being smashed it through 60 meshes using medicinal herb grinder, the powder after sieving is further crushed and obtains partial size less than 200nm
Nanoscale micropowders；
(2) after mixing Siraitia grosvenorii micropowders by the mass volume ratio of 1:5-20 with water, in 200-300W, 30-40 DEG C of item
Ultrasound is after 15-25 minutes under part, and by filter residue ultrasonic extraction 2-3 times again after filtering, combined extract is evaporated under reduced pressure and is extracted
Medicinal extract；
(3) after mixing by a certain amount of tetrahydrofuran, alkanol, water, standing is after 1-2 hours naturally, system split-phase, in taking-up
Mutually obtain the supermolecule solvent of nano-scale, alkanol is one of n-hexyl alcohol, n-octyl alcohol, Decanol, tetrahydrofuran, alkanol,
Water accounts for the 15-20:5-15:65-85% of total system volume respectively, and the sum of three's percent by volume is 100%.；
(4) medicinal extract is dissolved in after water and a certain amount of supermolecule solvent is added, vortex is centrifuged after 10-20 seconds, removes clear liquid, supernatant
After using supermolecule solvent extraction 2-3 times again, clear liquid is evaporated under reduced pressure to obtain medicinal extract, medicinal extract is dry after being washed with ethyl acetate, obtains
To the extract of high-purity mogroside.
2. a kind of extracting method of natural high-purity mogroside according to claim 1, it is characterised in that institute in step (3)
State the micella in nano-scale supermolecule there are partial size for 50-200nm.
3. a kind of extracting method of natural high-purity mogroside according to claim 1, it is characterised in that institute in step (4)
The concentration for stating medicinal extract aqueous solution is 0.2-0.4g/mL；The volume ratio of the supermolecule solvent and medicinal extract aqueous solution is 1:10.
4. a kind of extracting method of natural high-purity mogroside according to claim 1, it is characterised in that institute in step (4)
The total sweet tea glucoside purity of Siraitia grosvenorii in the extract of high-purity mogroside is stated not less than 95%, Momordica grosvenori mogroside V purity is not less than 68%.
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| CN107970156B (en) * | 2017-12-16 | 2020-04-24 | 广东美宝化妆品有限公司 | Preparation method of ginsenoside extract for daily chemical products |
| CN107854533A (en) * | 2018-01-01 | 2018-03-30 | 广东汇群中药饮片股份有限公司 | A kind of green safe coptis process of preparing technique |
| CN108042574A (en) * | 2018-01-01 | 2018-05-18 | 广东汇群中药饮片股份有限公司 | A kind of earthworm processing procedure of high hypoxanthine and protein content |
| CN108445099B (en) * | 2018-03-12 | 2020-12-29 | 中国检验检疫科学研究院 | Method for measuring 12 local anesthetics in cosmetics |
| CN108978260B (en) * | 2018-06-18 | 2021-11-12 | 广东欣薇尔服装有限公司 | Dyeing method of natural beet red pigment |
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| CN101029071B (en) * | 2007-04-05 | 2010-05-19 | 上海交通大学 | Method for preparing high-purity Momordia grosvenori aglycone from Momordia grosvenori |
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Denomination of invention: A Method of Extracting Natural High Purity Siraitin Effective date of registration: 20230907 Granted publication date: 20190809 Pledgee: Dongtai Jiangsu rural commercial bank Limited by Share Ltd. Pledgor: JIANGSU YOUZHI FOOD CO.,LTD. Registration number: Y2023320000466 |
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