CN109320576B - Production method of high-content mogroside V - Google Patents
Production method of high-content mogroside V Download PDFInfo
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- CN109320576B CN109320576B CN201811250821.5A CN201811250821A CN109320576B CN 109320576 B CN109320576 B CN 109320576B CN 201811250821 A CN201811250821 A CN 201811250821A CN 109320576 B CN109320576 B CN 109320576B
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- C07—ORGANIC CHEMISTRY
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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
- C07J17/005—Glycosides
Abstract
The invention discloses a production method of high-content mogroside V, belongs to the field of production of natural plant extracts, and takes frozen momordica grosvenori which is subjected to instantaneous high-temperature heating treatment as a raw material. The method has the advantages of low extraction cost, high yield, high product purity, small water consumption, simple process, large-scale continuous industrial production and the like.
Description
Technical Field
The invention belongs to the field of natural plant extraction, and particularly relates to an industrial production method of food ingredients.
Background
Momordica grosvenori (Siraitia grosvenorii) is a medicinal and edible perennial vine plant of Cucurbitaceae. The fruits of the traditional Chinese medicine are used as medicines, contain medicinal components such as mogroside, various amino acids, vitamins and the like, and are mainly used for treating cough caused by lung heat and phlegm fire, sphagitis, tonsillitis, acute gastritis, constipation and the like. Mogroside in fructus momordicae belongs to cucurbitane triterpenoid glycoside compounds, mainly comprises mogroside IV, mogroside V, siamenoside I and the like, wherein the content of the mogroside V is the highest, and accounts for about 0.4-0.5% of the weight of fresh fruits, the sweetness is equal to 300 times of that of cane sugar, but the mogroside V has the characteristics of not inducing decayed teeth and not causing the increase of blood sugar, and is an excellent sweetening agent for common people and patients with obesity, hypertension and diabetes. Clinical tests prove that the mogroside also has various health-care functions of eliminating phlegm, relieving cough, enhancing immunity, eliminating free radicals, preventing cancer and the like. With the improvement of living standard and the improvement of people's attention to health, the domestic demand of mogroside V as an excellent sweetener is increasing.
At present, in the prior art, many methods for extracting mogroside V exist, but the methods have the defects of complex process, low yield, low product purity, large water consumption and the like (for example, Chinese patent application CN 201410190403.7).
Therefore, the industrial production method of mogroside V, which has the advantages of simple process, high yield, high product purity and small water consumption, is a technical problem which needs to be solved by technical personnel in the field urgently.
Disclosure of Invention
Through long-term tests, the applicant develops a production method of high-content mogroside V, and the method has the advantages of low cost, high yield, high product purity, small water consumption, simple process, large-scale continuous industrial production and the like.
Specifically, the invention provides a production method of high-content mogroside V, which comprises a pretreatment step of immediately carrying out instantaneous high-temperature heating on raw material momordica grosvenori after freezing.
More specifically, the invention provides a production method of high-content mogroside V, which comprises the following steps:
1) pretreatment: freezing raw material fructus momordicae and then immediately heating at high temperature;
2) extraction: peeling the preprocessed fructus momordicae, crushing the pulp, adding water for countercurrent circulation extraction to obtain an extracting solution;
3) and (3) filtering: centrifuging the extracting solution, and filtering the supernatant obtained by centrifuging by using a ceramic membrane to obtain filtrate;
4) adsorption and desorption: adsorbing the filtrate with macroporous resin column, and resolving with ethanol solution to obtain resolving solution;
5) and (3) decoloring: sequentially passing the desorption solution through cation exchange resin and anion exchange resin, and collecting column passing solution;
6) concentration and drying: concentrating the column-passing solution, and drying to obtain mogroside V.
Wherein the content of mogroside V is more than or equal to 50%.
The further improvement of the invention is that the column-passing liquid is treated by a continuous chromatographic separation system to obtain refined liquid; concentrating the refined solution, and drying to obtain mogroside V; wherein the content of mogroside V is more than or equal to 98 percent. Wherein the packing material of the continuous chromatographic separation system is selected from one of C30, C18, C8, C4 or silica gel, and the eluent is water, an organic solvent selected from one of ethanol, acetonitrile, methanol or a mixture thereof or an aqueous solution thereof.
The pretreatment steps are as follows: freezing raw material fructus momordicae at-25 to-10 ℃ for 1 to 2 hours, and immediately heating at 105 to 120 ℃ for 5 to 50 seconds, preferably 10 to 40 seconds, and more preferably 20 to 30 seconds.
Wherein, the raw material of the momordica grosvenori in the step 1) is preferably fresh momordica grosvenori.
Wherein, when the pulp of the step 2) is broken, the seeds are not damaged, and preferably the seeds are kept in an intact state; during countercurrent circulation extraction, the mass ratio of the pulp to the water is 1: 2.5-6, and the extraction temperature is 50-90 ℃.
Wherein, the step 3) adopts a horizontal screw centrifuge or a disc centrifuge connected with the horizontal screw centrifuge in series to carry out centrifugal operation, the separation factor of the horizontal screw centrifuge is 2500-6000, and the separation factor of the disc centrifuge is 8000-30000; the aperture of the membrane tube of the ceramic membrane is 50-200 nm.
Wherein the type of the macroporous resin in the step 4) is selected from one of T-28, HDP-100 or DA 201-H; wherein the mass concentration of the ethanol solution is 55-70%, and the volume is 1.5-2.5 BV; the ethanol solution is pre-washed before analysis, 1-3 BV of aqueous alkali with the mass concentration of 2-6 per mill is used for pre-washing, 1-3 BV of acid solution with the mass concentration of 2-6 per mill is used for pre-washing, and finally 2-4 BV of pure water is used for washing until the column-passing liquid is neutral. Wherein the alkali solution is sodium hydroxide solution or potassium hydroxide solution, and the acid solution is hydrochloric acid solution or sulfuric acid solution.
Wherein the cation exchange resin of the step 5) has a model of 001 × 16 or 001 × 7, and the anion exchange resin has a model selected from one of 700B, D941, T-5 or D900.
The method effectively improves the content and yield of mogroside V in the target product by the pretreatment step of immediately carrying out instantaneous high-temperature heating treatment on the frozen raw material of the momordica grosvenori.
According to the requirement of the purity of the target product, the invention can produce mogroside V products with the content of more than or equal to 50 percent and more than or equal to 98 percent and different specifications. Namely, if the content of mogroside V in the target product is more than or equal to 50 percent, the column passing liquid is directly concentrated and dried, and the yield is as high as more than 95 percent; if the content of mogroside V in the target product is more than or equal to 98 percent, the column passing liquid is subjected to continuous chromatographic separation and then concentrated and dried, and the yield is up to more than 90 percent.
Detailed Description
The specific embodiments of the present invention are merely to further explain and illustrate the present invention, and the raw materials, auxiliary materials, equipment, etc. used in the examples are all commercially available.
Example 1
1) Pretreatment: placing fresh fructus Siraitiae Grosvenorii in a low-temperature freezer at-25 deg.C, freezing for 1 hr, and immediately heating with 105 deg.C steam for 20 s;
2) extraction: peeling the preprocessed fructus Siraitiae Grosvenorii, crushing the pulp (the seeds are kept intact), adding water with the mass 2.5 times of the pulp, and performing countercurrent circulation extraction at 50 deg.C to obtain extractive solution;
3) and (3) filtering: centrifuging the extractive solution with a horizontal screw centrifuge with a separation factor of 3000, and filtering the supernatant with a ceramic membrane with a membrane tube pore diameter of 50nm to obtain filtrate;
4) adsorption and desorption: adsorbing the filtrate by a DA201-H macroporous resin column, pre-washing with 1BV sodium hydroxide solution with the mass concentration of 2 per thousand, pre-washing with 1BV hydrochloric acid solution with the mass concentration of 2 per thousand, washing with 2BV pure water until the column-passing liquid is neutral, and finally resolving with 1.5BV ethanol solution with the mass concentration of 55% to obtain resolving liquid;
5) and (3) decoloring: the analytic solution is treated by 001X 16 cation exchange resin and T-5 anion exchange resin, and the solution passing through the column is collected;
6) concentration and drying: concentrating the column-passing solution to a solid content of 35%, and performing spray drying to obtain mogroside V.
Example 2
1) Pretreatment: placing fresh fructus Siraitiae Grosvenorii in a low-temperature freezer at-10 deg.C, freezing for 1.5 hr, and immediately heating with 120 deg.C steam for 30 s;
2) extraction: peeling the preprocessed fructus momordicae, crushing the pulp (seeds are kept complete), adding water with the mass 6 times of the pulp for countercurrent circulation extraction at the extraction temperature of 90 ℃ to obtain an extracting solution;
3) and (3) filtering: centrifuging the extractive solution with horizontal screw centrifuge with separation factor of 3500, centrifuging with disc centrifuge with separation factor of 8500, filtering the supernatant with ceramic membrane with membrane tube aperture of 200nm to obtain filtrate;
4) adsorption and desorption: adsorbing the filtrate by a T-28 macroporous resin column, pre-washing with 3BV sodium hydroxide solution with the mass concentration of 6 per thousand, pre-washing with 3BV hydrochloric acid solution with the mass concentration of 6 per thousand, washing with 4BV pure water until the column filtrate is neutral, and finally resolving with 1.5BV ethanol solution with the mass concentration of 60% to obtain resolving solution;
5) and (3) decoloring: the analytic solution is treated by 001 multiplied by 7 cation exchange resin and D900 anion exchange resin, and the column passing solution is collected;
6) refining: passing the column-passing liquid through a continuous chromatographic separation system with a separation column packed with C18, and eluting with 70% ethanol water solution to obtain refined liquid;
7) concentration and drying: concentrating the refined solution to solid content of 20%, and spray drying to obtain mogroside V.
Examples 3 to 4
The preparation methods of examples 3-4 are similar to example 2, except that the specific process parameters are different (see the following table, wherein the "water addition amount" is a multiple of the mass of the raw material fructus momordicae pulp).
Comparative examples 1 to 4
The preparation methods of comparative examples 1 to 4 were similar to those of examples 1 to 4, respectively, except that: comparative examples 1 and 2 did not employ a pretreatment step of immediately performing instantaneous high-temperature heating after freezing; the freezing temperature of the comparative example 3 was-30 ℃, the freezing time was 1 hour, the high-temperature heating temperature was 130 ℃, and the heating time was 30 seconds; the comparative example 4 had a freezing temperature of-5 ℃ and a freezing time of 3 hours, a high-temperature heating temperature of 110 ℃ and a heating time of 60 seconds.
Test examples
Taking the mogroside V prepared in the examples 1-4 and the comparative examples 1-4, detecting the content of the mogroside V according to the national standard (GB1886.77-2016), and calculating the yield according to the following formula: (the mass of mogroside V in the product/the mass of mogroside V in Lo Han Guo) × 100%, the results were as follows:
| content (wt.) | Yield of | |
| Example 1 | 55.0％ | 96％ |
| Example 2 | 98.5％ | 91％ |
| Example 3 | 98.0％ | 90％ |
| Example 4 | 98.2％ | 91％ |
| Comparative example 1 | 47.2％ | 76％ |
| Comparative example 2 | 92.3％ | 85％ |
| Comparative example 3 | 94.3％ | 87％ |
| Comparative example 4 | 93.5％ | 84％ |
Therefore, the content and yield of the mogroside V (as in examples 1-2) with two specifications prepared by the method are obviously superior to those of the corresponding control examples 1-2 which do not adopt the pretreatment step; particularly, the content and yield of the mogroside V prepared by the invention (as in examples 3-4) are obviously better than those of the corresponding control examples 3-4 with the freezing and heating process parameter values outside the claimed protection range.
Claims (7)
1. A production method of mogroside V comprises the following steps:
1) pretreatment: freezing raw material momordica grosvenori, immediately heating at high temperature, freezing the raw material momordica grosvenori at-25 to-10 ℃ for 1 to 2 hours, and immediately heating at 105 to 120 ℃ for 5 to 50 seconds;
2) extraction: peeling the preprocessed fructus momordicae, crushing the pulp, adding water for countercurrent circulation extraction to obtain an extracting solution;
3) and (3) filtering: centrifuging the extracting solution, and filtering the supernatant obtained by centrifuging by using a ceramic membrane to obtain filtrate;
4) adsorption and desorption: adsorbing the filtrate with macroporous resin column, and resolving with ethanol solution to obtain resolving solution, wherein the type of macroporous resin is selected from one of T-28, HDP-100 or DA 201-H; wherein the mass concentration of the ethanol solution is 55-70%, and the volume is 1.5-2.5 BV; pre-washing the ethanol solution before analysis, namely pre-washing the ethanol solution by using 1-3 BV of aqueous alkali with the mass concentration of 2-6 per mill, pre-washing the ethanol solution by using 1-3 BV of acid solution with the mass concentration of 2-6 per mill, and finally washing the ethanol solution by using 2-4 BV of pure water until the column solution is neutral;
5) and (3) decoloring: sequentially passing the desorption solution through cation exchange resin and anion exchange resin, and collecting column passing solution;
6) concentration and drying: concentrating and drying the column passing liquid to obtain mogroside V;
wherein the content of mogroside V is more than or equal to 50%.
2. A method for producing mogroside V according to claim 1, wherein the column-passing liquid is treated by a continuous chromatographic separation system to obtain a refined liquid; concentrating the refined solution, and drying to obtain mogroside V; wherein the content of mogroside V is more than or equal to 98 percent.
3. A mogroside V production method according to claim 2, wherein the packing material of the continuous chromatographic separation system is selected from one of C30, C18, C8, C4 or silica gel, and the eluent is water, an organic solvent selected from one of ethanol, acetonitrile, methanol or a mixture thereof or an aqueous solution thereof.
4. A method for producing mogroside V according to any one of claims 1-3, wherein the seeds remain intact when the pulp of step 2) is broken; during countercurrent circulation extraction, the mass ratio of the pulp to the water is 1: 2.5-6, and the extraction temperature is 50-90 ℃.
5. A mogroside V production method according to any one of claims 1-3, wherein step 3) is performed by a horizontal screw centrifuge or a horizontal screw centrifuge in series with a disk centrifuge, the separation factor of the horizontal screw centrifuge is 2500-6000, and the separation factor of the disk centrifuge is 8000-30000; the aperture of the membrane tube of the ceramic membrane is 50-200 nm.
6. A production method of mogroside V according to claim 1, wherein the alkali solution is sodium hydroxide solution or potassium hydroxide solution, and the acid solution is hydrochloric acid solution or sulfuric acid solution.
7. A mogroside V production method according to any one of claims 1-3, wherein the cation exchange resin of step 5) is 001 x 16 or 001 x 7, and the anion exchange resin is selected from one of 700B, D941, T-5 or D900.
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| CN111978365B (en) * | 2020-09-10 | 2022-04-12 | 上海诺德生物实业有限公司 | Preparation method of mogroside V-containing mogroside |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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 |
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