CN109320576A - A kind of production method of high-content momordica grosvenori glycoside V - Google Patents

A kind of production method of high-content momordica grosvenori glycoside V Download PDF

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CN109320576A
CN109320576A CN201811250821.5A CN201811250821A CN109320576A CN 109320576 A CN109320576 A CN 109320576A CN 201811250821 A CN201811250821 A CN 201811250821A CN 109320576 A CN109320576 A CN 109320576A
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momordica grosvenori
grosvenori glycoside
content
production method
solution
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CN109320576B (en
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连运河
额尔敦巴雅尔
蔡亚园
焦利卫
杨文江
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Chenguang Biotech Group Co Ltd
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Chenguang Biotech Group 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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  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Saccharide Compounds (AREA)
  • Steroid Compounds (AREA)

Abstract

The invention discloses a kind of production methods of high-content momordica grosvenori glycoside V, belong to natural plant extracts production field, to carry out the Siraitia grosvenorii of TRANSIENT HIGH TEMPERATURE heat treatment immediately as raw material after freezing.The present invention has many advantages, such as that the at low cost, high income of extraction, product purity is high, water consumption is small, simple process, large-scale continuous industrial production can be achieved.

Description

A kind of production method of high-content momordica grosvenori glycoside V
Technical field
The invention belongs to extracted form natural plant fields, and in particular to a kind of industrialized preparing process of food ingredient.
Background technique
Siraitia grosvenorii (Siraitia grosvenorii) is a kind of perennial liana of Curcurbitaceae of dual-purpose of drug and food.Chinese medicine Lung heat phlegm-fire cough, pharynx are cured mainly containing medicinal ingredients such as mogroside, a variety of amino acid and vitamins with its fruit medicine Laryngitis, tonsillitis, acute gastritis, constipation etc..Mogroside in Siraitia grosvenorii belongs to cucurbitane triterpene glycosides compound, main To include Momordia grosvenori aglycone IV, momordica grosvenori glycoside V and Simon glycosides I etc., wherein with Mogroside V content highest, account for about fresh fruit weigh 0.4~ 0.5%, sugariness is equivalent to 300 times of sucrose, but it has the characteristics that not induce saprodontia, does not cause blood glucose rise, is ordinary people Group and obesity, hypertension, diabetic excellent sweetener.Clinical test proves, mogroside also have eliminating the phlegm, Antibechic, removes the plurality of health care functions such as free radical and anti-cancer at strengthen immunity.With the improvement of living standards and people are to strong The raising of health degree of concern, momordica glycoside V are also constantly increasing as a kind of domestic demand amount of excellent sweetener.
Currently, the extracting method of momordica grosvenori glycoside V is more in the prior art, but have that complex process, yield are low, product is pure Spend many defects (such as Chinese patent application CN201410190403.7) such as low, water consumption is big.
Therefore it provides a kind of industrial metaplasia for the momordica grosvenori glycoside V that simple process, high income, product purity are high, water consumption is small Production method becomes the technical issues of there is an urgent need to those skilled in the art's solutions.
Summary of the invention
Through long term test, applicant develops a kind of production method of high-content momordica grosvenori glycoside V, at low cost, receipts Rate is high, product purity is high, water consumption is small, simple process, the advantages that large-scale continuous industrial production can be achieved.
Specifically, the present invention provides a kind of production methods of high-content momordica grosvenori glycoside V, including by raw material Siraitia grosvenorii through cold The pre-treatment step of TRANSIENT HIGH TEMPERATURE heating is carried out after jelly immediately.
More specifically, including the following steps: the present invention provides a kind of production method of high-content momordica grosvenori glycoside V
1) pre-process: by raw material Siraitia grosvenorii it is chilled after carry out TRANSIENT HIGH TEMPERATURE heating immediately;
2) it extracts: will be removed the peel by pretreated Siraitia grosvenorii, pulp crushing adds water to carry out circulated in countercurrent extraction, must extract Liquid;
3) filter: extracting solution is centrifuged, and the supernatant being centrifuged obtains filtered fluid through ceramic membrane filter;
4) absorption and parsing: filtered fluid is parsed after macroporous resin column is adsorbed with ethanol solution, obtains desorbed solution;
5) decolourize: desorbed solution passes sequentially through cation exchange resin, anion exchange resin, collects column liquid;
6) it concentration and drying: crosses column liquid and is concentrated, is dry, obtain momordica grosvenori glycoside V.
Wherein, content >=50% of the momordica grosvenori glycoside V.
A further improvement of the present invention is that the column liquid of crossing is handled through continuous chromatography separation system, refined liquid is obtained;Essence Liquid processed is concentrated, is dry, obtains momordica grosvenori glycoside V;Wherein, content >=98% of the momordica grosvenori glycoside V.The wherein continuous chromatography The filler of separation system is selected from one of C30, C18, C8, C4 or silica gel, eluent be water, selected from one of ethyl alcohol, acetonitrile, methanol or The organic solvent of its mixture or its aqueous solution.
The pre-treatment step are as follows: after freezing raw material Siraitia grosvenorii 1~2 hour under the conditions of -25 DEG C~-10 DEG C, stand Heated 5~50 seconds, preferably 10~40 seconds, more preferable 20~30 seconds under the conditions of 105 DEG C~120 DEG C.
Wherein, the preferably new fresh fructus momordicae of the raw material Siraitia grosvenorii of the step 1).
Wherein, when the pulp crushing of the step 2), seed is not destroyed, and is preferably maintained in good working condition;Circulated in countercurrent is extracted When, the mass ratio of pulp and water is 1:2.5~6, and Extracting temperature is 50~90 DEG C.
Wherein, the step 3) carries out centrifugally operated using decanter centrifuge or decanter centrifuge series connection disk plate centrifuge, The separation factor of the decanter centrifuge is 2500~6000, and the separation factor of the disk plate centrifuge is 8000~30000;Institute The membrane tube aperture for stating ceramic membrane is 50~200nm.
Wherein, the macroreticular resin model of the step 4) is selected from one of T-28, HDP-100 or DA201-H;Described in wherein The mass concentration of ethanol solution is 55~70%, and volume is 1.5~2.5BV;Prewashing is carried out before the ethanol solution parsing, first The aqueous slkali prewashing for being 2~6 ‰ with the mass concentration of 1~3BV, then it is pre- with the acid solution that the mass concentration of 1~3BV is 2~6 ‰ It washes, it is neutral for being finally washed till column liquid with the pure water of 2~4BV.Wherein the aqueous slkali is sodium hydroxide solution or hydroxide Potassium solution, acid solution are hydrochloric acid solution or sulfuric acid solution.
Wherein, the model 001 × 16 or 001 × 7 of the cation exchange resin of the step 5), the anion exchange The model of resin is selected from one of 700B, D941, T-5 or D900.
The present invention has by the way that raw material Siraitia grosvenorii to be carried out to the pre-treatment step of TRANSIENT HIGH TEMPERATURE heat treatment immediately after chilled Improve to effect the content and yield of momordica grosvenori glycoside V in target product.
According to the needs of target product purity, the present invention can produce Mogroside V content >=50% and >=98% two kind not The momordica grosvenori glycoside V product of same specification.That is, column liquid is directly concentrated dry if Mogroside V content >=50% of target product Dry, yield is up to 95% or more;If Mogroside V content >=98% of target product, by column liquid through continuous chromatography It after separation, then is concentrated and dried, yield is up to 90% or more.
Specific embodiment
A specific embodiment of the invention is only to be explained further and illustrate the present invention, supplementary material used in the examples, Equipment etc. is commercially available.
Embodiment 1
1) it pre-processes: new fresh fructus momordicae being placed in -25 DEG C of cryogenic freezing case, after freezing 1 hour, immediately with 105 DEG C Steam heat 20 seconds;
2) it extracts: will be removed the peel by pretreated Siraitia grosvenorii, pulp quality 2.5 is added in pulp crushing (seed keeps complete) Water again carries out circulated in countercurrent extraction, and Extracting temperature is 50 DEG C, obtains extracting solution;
3) filter: after the decanter centrifuge centrifugation that separation factor is 3000, supernatant is extracting solution through membrane tube aperture The ceramic membrane filter of 50nm, obtains filtered fluid;
4) absorption and parsing: filtered fluid is first 2 ‰ with the mass concentration of 1BV after the absorption of DA201-H macroporous resin column Sodium hydroxide solution prewashing, then the hydrochloric acid solution prewashing for being 2 ‰ with the mass concentration of 1BV, were then washed till column with the pure water of 2BV Liquid is neutrality, is finally parsed with the ethanol solution that the mass concentration of 1.5BV is 55%, obtains desorbed solution;
5) decolourize: desorbed solution first passes through 001 × 16 cation exchange resin, then is carried out by T-5 anion exchange resin Processing, collected column liquid;
6) it concentration and drying: crosses column liquid and is concentrated into solid content 35%, then be spray-dried, obtain momordica grosvenori glycoside V.
Embodiment 2
1) it pre-processes: new fresh fructus momordicae being placed in -10 DEG C of cryogenic freezing case, after freezing 1.5 hours, immediately with 120 DEG C steam heat 30 seconds;
2) it extracts: will be removed the peel by pretreated Siraitia grosvenorii, pulp crushing (seed keeps complete) is added 6 times of pulp quality Water carry out circulated in countercurrent extraction, Extracting temperature be 90 DEG C, obtain extracting solution;
3) filter: extracting solution is 8500 after the decanter centrifuge centrifugation that separation factor is 3500, then through separation factor Disk plate centrifuge centrifugation, supernatant through membrane tube aperture be 200nm ceramic membrane filter, obtain filtered fluid;
4) absorption and parsing: filtered fluid is after the absorption of T-28 macroporous resin column, the hydrogen for being first 6 ‰ with the mass concentration of 3BV Sodium hydroxide solution prewashing, then the hydrochloric acid solution prewashing for being 6 ‰ with the mass concentration of 3BV, were then washed till column liquid with the pure water of 4BV For neutrality, is finally parsed with the ethanol solution that the mass concentration of 1.5BV is 60%, obtain desorbed solution;
5) decolourize: desorbed solution first passes through 001 × 7 cation exchange resin, then is carried out by D900 anion exchange resin Processing, collected column liquid;
6) it refines: the continuous chromatography separation system that column liquid is C18 through separating column packing is crossed, with 70% ethanol aqueous wash It is de-, obtain refined liquid;
7) concentration and drying: refined liquid is concentrated into solid content 20%, and spray drying obtains momordica grosvenori glycoside V.
Embodiment 3~4
The preparation method of embodiment 3~4 is similar to Example 2, and difference is only that specific technological parameter is different and (is detailed in down Table, wherein " amount of water " is the multiple of raw material Siraitia grosvenorii pulp quality).
Reference examples 1~4
The preparation method of reference examples 1~4 is similar with Examples 1 to 4 respectively, and difference is only that: reference examples 1,2 are not using cold The pre-treatment step of TRANSIENT HIGH TEMPERATURE heating is carried out after jelly immediately;The cryogenic temperature of reference examples 3 is -30 DEG C, and cooling time is 1 small When, high-temperature heating temperature is 130 DEG C, and heating time is 30 seconds;The cryogenic temperature of reference examples 4 is -5 DEG C, and cooling time is 3 small When, high-temperature heating temperature is 110 DEG C, and heating time is 60 seconds.
Test example
Momordica grosvenori glycoside V prepared by Example 1~4, reference examples 1~4, (GB1886.77-2016) is examined according to national standards Survey the content of momordica grosvenori glycoside V, and calculated yield according to the following formula: (momordica grosvenori glycoside V in quality/Siraitia grosvenorii of momordica grosvenori glycoside V in product Quality) × 100%, it is as a result as follows:
Content Yield
Embodiment 1 55.0% 96%
Embodiment 2 98.5% 91%
Embodiment 3 98.0% 90%
Embodiment 4 98.2% 91%
Reference examples 1 47.2% 76%
Reference examples 2 92.3% 85%
Reference examples 3 94.3% 87%
Reference examples 4 93.5% 84%
As it can be seen that the content and yield of the momordica grosvenori glycoside V (such as Examples 1 to 2 2) of two specifications prepared by the present invention are obvious Better than the reference examples 1~2 for not using pre-treatment step accordingly;In particular, momordica grosvenori glycoside V (such as embodiment 3 prepared by the present invention ~4) content and yield is also significantly better than that corresponding freezing, heating technique parameter value are claimed outside range in the present invention Reference examples 3~4.

Claims (10)

1. a kind of production method of high-content momordica grosvenori glycoside V, including add TRANSIENT HIGH TEMPERATURE is carried out immediately after the freezing of raw material Siraitia grosvenorii The pre-treatment step of heat.
2. the production method of high-content momordica grosvenori glycoside V according to claim 1, includes the following steps:
1) pre-process: by raw material Siraitia grosvenorii it is chilled after carry out TRANSIENT HIGH TEMPERATURE heating immediately;
2) it extracts: will be removed the peel by pretreated Siraitia grosvenorii, pulp crushing adds water to carry out circulated in countercurrent extraction, obtains extracting solution;
3) filter: extracting solution is centrifuged, and the supernatant being centrifuged obtains filtered fluid through ceramic membrane filter;
4) absorption and parsing: filtered fluid is parsed after macroporous resin column is adsorbed with ethanol solution, obtains desorbed solution;
5) decolourize: desorbed solution passes sequentially through cation exchange resin, anion exchange resin, collects column liquid;
6) it concentration and drying: crosses column liquid and is concentrated, is dry, obtain momordica grosvenori glycoside V;
Wherein, content >=50% of the momordica grosvenori glycoside V.
3. the production method of high-content momordica grosvenori glycoside V according to claim 2, wherein described crosses column liquid through continuous chromatography Separation system processing, obtains refined liquid;Refined liquid concentration, drying, obtain momordica grosvenori glycoside V;Wherein, the content of the momordica grosvenori glycoside V ≥98%。
4. the production method of high-content momordica grosvenori glycoside V according to claim 3, wherein the continuous chromatography separation system Filler is selected from one of C30, C18, C8, C4 or silica gel, and eluent is water, selected from or mixtures thereof one of ethyl alcohol, acetonitrile, methanol Organic solvent or its aqueous solution.
5. the production method of high-content momordica grosvenori glycoside V according to any one of claims 1 to 4, wherein the step 1) is pre- Processing step are as follows: after freezing raw material Siraitia grosvenorii 1 ~ 2 hour under the conditions of -25 DEG C~-10 DEG C, immediately in 105 DEG C~120 DEG C items It is heated 5 ~ 50 seconds under part.
6. according to the production method of any high-content momordica grosvenori glycoside V of claim 2~4, wherein the fruit of the step 2 When meat is crushed, seed keeps complete;When circulated in countercurrent is extracted, the mass ratio of pulp and water is 1:2.5~6, Extracting temperature is 50~ 90℃。
7. according to the production method of any high-content momordica grosvenori glycoside V of claim 2~4, wherein the step 3) uses Decanter centrifuge or decanter centrifuge series connection disk plate centrifuge carry out centrifugally operated, and the separation factor of the decanter centrifuge is 2500~6000, the separation factor of the disk plate centrifuge is 8000~30000;The membrane tube aperture of the ceramic membrane be 50~ 200nm。
8. according to the production method of any high-content momordica grosvenori glycoside V of claim 2~4, wherein the step 4) is big Hole resin model is selected from one of T-28, HDP-100 or DA201-H;Wherein the mass concentration of the ethanol solution be 55~ 70%, volume is 1.5~2.5BV;Carry out prewashing before the described ethanol solution parsing, first with the mass concentration of 1~3BV for 2~ 6 ‰ aqueous slkali prewashing, then the acid solution prewashing for being 2~6 ‰ with the mass concentration of 1~3BV, are finally washed with the pure water of 2~4BV It is neutrality to column liquid is crossed.
9. the production method of high-content momordica grosvenori glycoside V according to claim 8, wherein the aqueous slkali is sodium hydroxide Solution or potassium hydroxide solution, the acid solution are hydrochloric acid solution or sulfuric acid solution.
10. according to the production method of any high-content momordica grosvenori glycoside V of claim 2~4, wherein the sun of the step 5) The model of the model 001 × 16 or 001 × 7 of ion exchange resin, the anion exchange resin is selected from 700B, D941, T-5 Or one of D900.
CN201811250821.5A 2018-10-25 2018-10-25 Production method of high-content mogroside V Active CN109320576B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN116941765A (en) * 2023-07-28 2023-10-27 湖南华诚生物资源股份有限公司 An improved co-production method of pesticide-free mogroside composition
WO2025000615A1 (en) * 2023-06-28 2025-01-02 桂林吉福思罗汉果生物技术股份有限公司 Sweetness composition and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923152A (en) * 2014-05-08 2014-07-16 济南汉定生物工程有限公司 Method for extracting mogroside V
CN104312921A (en) * 2014-09-28 2015-01-28 广州英佩尔电子科技有限公司 Comprehensive micro-molecule wall breaking method used for fresh food and drug materials
CN108276465A (en) * 2017-03-14 2018-07-13 桂林莱茵生物科技股份有限公司 A method of isolating and purifying mogroside V with subcritical water desorption techniques

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923152A (en) * 2014-05-08 2014-07-16 济南汉定生物工程有限公司 Method for extracting mogroside V
CN104312921A (en) * 2014-09-28 2015-01-28 广州英佩尔电子科技有限公司 Comprehensive micro-molecule wall breaking method used for fresh food and drug materials
CN108276465A (en) * 2017-03-14 2018-07-13 桂林莱茵生物科技股份有限公司 A method of isolating and purifying mogroside V with subcritical water desorption techniques

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
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
WO2025000615A1 (en) * 2023-06-28 2025-01-02 桂林吉福思罗汉果生物技术股份有限公司 Sweetness composition and preparation method thereof
CN116941765A (en) * 2023-07-28 2023-10-27 湖南华诚生物资源股份有限公司 An improved co-production method of pesticide-free mogroside composition
CN116941765B (en) * 2023-07-28 2025-02-14 湖南华诚生物资源股份有限公司 An improved method for co-producing a pesticide-free mogroside composition

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