CN103980335A - Mogroside V preparation method - Google Patents
Mogroside V preparation method Download PDFInfo
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- GHBNZZJYBXQAHG-KUVSNLSMSA-N (2r,3r,4s,5s,6r)-2-[[(2r,3s,4s,5r,6r)-6-[[(3s,8s,9r,10r,11r,13r,14s,17r)-17-[(2r,5r)-5-[(2s,3r,4s,5s,6r)-4,5-dihydroxy-3-[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-6-[[(2r,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@H](CC[C@@H](C)[C@@H]1[C@]2(C[C@@H](O)[C@@]3(C)[C@H]4C(C([C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]6[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O6)O)O5)O)CC4)(C)C)=CC[C@H]3[C@]2(C)CC1)C)C(C)(C)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GHBNZZJYBXQAHG-KUVSNLSMSA-N 0.000 title claims abstract description 29
- TVJXHJAWHUMLLG-UHFFFAOYSA-N mogroside V Natural products CC(CCC(OC1OC(COC2OC(CO)C(O)C(O)C2OC3OC(CO)C(O)C(O)C3O)C(O)C(O)C1O)C(C)(C)O)C4CCC5(C)C6CC=C7C(CCC(OC8OC(COC9OC(CO)C(O)C(O)C9O)C(O)C(O)C8O)C7(C)C)C6(C)C(O)CC45C TVJXHJAWHUMLLG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 91
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000012535 impurity Substances 0.000 claims abstract description 40
- 238000001035 drying Methods 0.000 claims abstract description 38
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 235000009815 Momordica Nutrition 0.000 claims abstract description 29
- 241000218984 Momordica Species 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 238000007670 refining Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical group C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 11
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 99
- 235000016068 Berberis vulgaris Nutrition 0.000 claims description 41
- 241000335053 Beta vulgaris Species 0.000 claims description 41
- 239000012141 concentrate Substances 0.000 claims description 38
- 238000010521 absorption reaction Methods 0.000 claims description 35
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- 241001409321 Siraitia grosvenorii Species 0.000 claims description 26
- 235000011171 Thladiantha grosvenorii Nutrition 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 18
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- -1 carbon chain ester Chemical class 0.000 description 3
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- 229930182478 glucoside Natural products 0.000 description 3
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Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the Corsvenor Momordica Fruit processing field, and concretely relates to a mogroside V preparation method. The preparation method comprises the following steps: crushing an initial raw material manure Corsvenor Momordica Fruit, extracting, clarifying to remove impurities, filtering, carrying out macro-porous adsorption resin adsorption, eluting, carrying out secondary ion exchange resin adsorption, concentrating, drying, and carrying out ethanol refining to obtain mogroside V. Nontoxic ethanol is adopted in the extraction step to substitute traditional methanol, a novel natural traditional Chinese medicinal clarificant is introduced in the extraction process to remove impurities comprising pectin, fibers, proteins and the like, and two different adsorption resins are adopted in the eluting process to carry out adsorption. Ethanol is utilized to substitute traditional methanol, so the degree of the harms of a solvent to the health of human bodies is reduced; and the purity of a product obtained after impurity removal using the clarificant and two-time column adsorption purification increases to above 97%.
Description
Technical field
The invention belongs to Grosvenor Momordica manufacture field, specifically a kind of preparation method of Momordica grosvenori mogroside V.
Background technology
Grosvenor Momordica is perennial climing plant, and Main Cultivation is at Chinese In Northern Guangxi.Its dry fruit is oval or circular, and shell brown or smoking color also have a large amount of tiny black fine, soft furs.Utilize its sweet taste and have the history of counting century as Chinese medicine Chinese people.After processing, Grosvenor Momordica can be used as the medicine for the treatment of flu and moistening lung.Modern Grosvenor Momordica is generally used or is made into good to eat beverage by the low-calorie sweetener as in nectar or beverage.Mainly concentrate on sweet glucoside for the research and development of Grosvenor Momordica at present, wherein Momordica grosvenori mogroside V is main sweet ingredient in sweet glucoside.The sugariness of sweet glucoside be sugar 300 times and thermal content low.That diabetic subject is stable and without fermentable perfect additive.As a kind of general natural sweeteners be replace artificial sweetening agent as aspartame etc. desirable substitute.At beverage, bake, nutritive food, low-heat food or other need low or sweet maybe needs of carbohydrate taste can give full play to its effect in low or empty calory edible food.Culinary art or baking can't affect its local flavor or sugariness.
At present, the method and the report that extract Momordica grosvenori mogroside V are a lot, but are all taking new fresh Fructus Momordicae as raw material, produce by the technique such as column purification, the extraction of water extraction thin film concentration on water extraction enzymolysis.Preparation method's research of Momordica grosvenori mogroside V, as patent CN200710050255.9, discloses a kind of preparation method of high-purity Momordica grosvenori mogroside V, and its step is as follows: 1) get Momordica-Glycosides and be dissolved in methyl alcohol, filter, obtain filtrate; 2) in gained filtrate, add acetone to make it produce precipitation, filter, obtain throw out; 3) taking precipitate adsorbs with normal phase silicagel column; 4) normal phase silicagel column having adsorbed, is that eluent carries out wash-out with the mixing solutions of low carbon chain ester and ethanol, collects elutriant; 5) reclaim the eluent in elutriant, crystallization, obtains high-purity Momordica grosvenori mogroside V, and this invention need to adopt expensive normal phase silicagel column, and the wash-out of beet aglucone V need to rely on low carbon chain ester, makes this explained hereafter cost high.As patent CN201010223923.5, a kind of method of extracting high-content Momordica grosvenori mogroside V from dried fructus momordicae is disclosed, extraction process comprises the steps: to extract, concentrated, filtration, absorption, decolouring, concentrate drying must contain Momordica grosvenori mogroside V product, it adopts ethanol in extraction step is solvent, but this invention is not to carrying out removal of impurities in leaching process, the impurity that has fiber, albumen, pectin one class in the product obtaining, product purity is not high.
Summary of the invention
The object of the invention is to overcome the problems such as removal of impurities difficulty is extracted in existing Momordica grosvenori mogroside V extraction process existence, leaching organic solution methyl alcohol is poisonous, and plant factor is low, product purity is low, production cost is high, a kind of preparation method of Momordica grosvenori mogroside V is provided.
The solution of the present invention is by such realization: a kind of preparation method of Momordica grosvenori mogroside V, choose the ripe Grosvenor Momordica that fresh nothing is gone rotten, and the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, with the Grosvenor Momordica extracting after solvent countercurrent extraction or refluxing extraction fragmentation, the ratio=2 ~ 8L:1kg of extraction agent and Grosvenor Momordica, extraction time is 3 ~ 8 hours, obtains extracting solution.
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.05 ~ 0.1kg:1L of finings and extracting solution, after stirring, standing 25 ~ 40min, removes by filter precipitation, obtains the solution after removal of impurities.
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 1.5 ~ 2 meters of resin loading heights, extract solution absorbs flow velocity 1-4BV/hr, adsorb the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.3 ~ 0.6L:1L, collect elutriant I.
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.1 ~ 0.4L:1L, collection elutriant II.
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 300 ~ 800rpm, temperature are under the condition of 30 ~ 37 DEG C, concentrate drying is to beet aglucone V product water content≤10%, refining through ethanol again, obtain beet aglucone V product.
As further restriction of the present invention, while adopting refluxing extraction in described extraction step, refluxing extraction is divided and is carried out for 2 ~ 3 times, each 2 hours; Described extraction agent be in 40 ~ 80% aqueous ethanolic solution, pure water any.
As further restriction of the present invention, the finings in described clarification removal step is natural traditional Chinese medicine finings KBT-ZTC; Described step 3) and 4) in the eluent used be any in ethanol or the aqueous solution.
As further restriction of the present invention, described step 5) in ethanol refine as utilizing ethanol to dissolve the beet aglucone V obtaining after dry completely, remove by filter throw out, concentrate drying is to beet aglucone V product water content≤10% again.
As complete scheme of the present invention, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, the Grosvenor Momordica after the 60% aqueous ethanolic solution refluxing extraction fragmentation of use extraction solvent 3 times, the ratio=6L:1kg of extraction agent and Grosvenor Momordica, each extraction time is 2.5 hours, obtains extracting solution.
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.05 ~ 0.1kg:1L of finings and extracting solution, after stirring, standing 25 ~ 40min, removes by filter precipitation, obtains the solution after removal of impurities.
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 2 meters of resin loading heights, extract solution absorbs flow velocity 2.5BV/hr, have adsorbed the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.5L:1L, collect elutriant I.
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.2L:1L, collection elutriant II.
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 500rpm, temperature are under the condition of 37 DEG C, concentrate drying is to beet aglucone V product water content≤10%, after dissolving beet aglucone V completely with 60% aqueous ethanolic solution again, remove by filter precipitation, reconcentration is dried to beet aglucone V product water content≤10%, obtains beet aglucone V product.
The know-why that the present invention realizes is: utilizing ripe Grosvenor Momordica fresh fruit is starting raw material, through fragmentation, extract, clarification removal of impurities, filter, absorption with macroporous adsorbent resin, wash-out, the absorption of secondary ions exchange resin, concentrated, dry, the refining Momordica grosvenori mogroside V that obtains of ethanol, in extraction, adopt nontoxic ethanol to replace traditional methyl alcohol, reduce the injury of organic solvent to workman, and in leaching process, introduce new type natural Chinese medicine finings, effectively remove pectin, fiber, the impurity such as protein, in elution process, adopt two kinds of different polymeric adsorbent absorption, improve the purity of product.
The present invention possesses following good result:
(1) the present invention adds new type natural Chinese medicine finings in extracting solution, flocculation sediment has been removed the impurity such as the pectin in extracting solution, fiber, protein, make to extract purifying and obtained purifying, solve a difficult problem for this product extracting liquid filtering technology, improve plant factor, reduced equipment use cost, shortened filtration time and make the most of impurity in extracting solution effectively be removed simultaneously.
(2) by the absorption of different polymeric adsorbents and twice different adsorpting column chromatography wash-out of different elutriants, the purity of product is greatly improved, purity reaches more than 97%.
(3) the present invention adopts ethanol to replace methyl alcohol to refine, and has reduced the hazard rating of organic solvent to HUMAN HEALTH.
Brief description of the drawings
Fig. 1 is preparation method's schema of the present invention.
Embodiment
The preparation method who describes a kind of Momordica grosvenori mogroside V of the present invention below in conjunction with embodiment and accompanying drawing, these descriptions are not that content of the present invention is further limited.
Embodiment 1
A preparation method for Momordica grosvenori mogroside V, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, with the Grosvenor Momordica extracting after solvent countercurrent extraction or refluxing extraction fragmentation, the ratio=8L:1kg of extraction agent and Grosvenor Momordica, extraction time is 5 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.1kg:1L of finings and extracting solution, after stirring, standing 40min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 1.8 meters of resin loading heights, extract solution absorbs flow velocity 4BV/hr, have adsorbed the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.5L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.3L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 600rpm, temperature are under the condition of 37 DEG C, concentrate drying is to beet aglucone V product water content≤10%, refining through ethanol again, obtain beet aglucone V product.
While adopting refluxing extraction in extraction step, refluxing extraction is divided and is carried out for 3 times, each 2 hours; Described extraction agent is 80% aqueous ethanolic solution.
Finings in clarification removal step is natural traditional Chinese medicine finings KBT-ZTC; Described step 3) and 4) in the eluent used be ethanol.
Step 5) in ethanol refine as utilizing ethanol to dissolve the beet aglucone V obtaining after dry completely, remove by filter throw out, concentrate drying is to beet aglucone V product water content≤10% again.
The present embodiment obtains product purity and reaches 97.5%.
Embodiment 2
A preparation method for Momordica grosvenori mogroside V, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, with the Grosvenor Momordica extracting after solvent countercurrent extraction or refluxing extraction fragmentation, the ratio=2L:1kg of extraction agent and Grosvenor Momordica, extraction time is 8 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.05kg:1L of finings and extracting solution, after stirring, standing 25min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 2 meters of resin loading heights, extract solution absorbs flow velocity 3BV/hr, have adsorbed the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.3L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.1L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 300rpm, temperature are under the condition of 30 DEG C, concentrate drying is to beet aglucone V product water content≤10%, refining through ethanol again, obtain beet aglucone V product.
While adopting refluxing extraction in extraction step, refluxing extraction is divided and is carried out for 2 times, each 2 hours; Described extraction agent is 40% aqueous ethanolic solution.
Finings in clarification removal step is natural traditional Chinese medicine finings KBT-ZTC; Described step 3) and 4) in the eluent used be ethanol.
Step 5) in ethanol refine as utilizing ethanol to dissolve the beet aglucone V obtaining after dry completely, remove by filter throw out, concentrate drying is to beet aglucone V product water content≤10% again.
The present embodiment obtains product purity and reaches 98.5%.
Embodiment 3
A preparation method for Momordica grosvenori mogroside V, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, with the Grosvenor Momordica extracting after solvent countercurrent extraction or refluxing extraction fragmentation, the ratio=6L:1kg of extraction agent and Grosvenor Momordica, extraction time is 3 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.08kg:1L of finings and extracting solution, after stirring, standing 25min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 1.5 meters of resin loading heights, extract solution absorbs flow velocity 1BV/hr, have adsorbed the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.3L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.1L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 300rpm, temperature are under the condition of 35 DEG C, concentrate drying is to beet aglucone V product water content≤10%, refining through ethanol again, obtain beet aglucone V product.
While adopting refluxing extraction in extraction step, refluxing extraction is divided and is carried out for 3 times, each 2 hours; Described extraction agent is 60% aqueous ethanolic solution.
Finings in clarification removal step is natural traditional Chinese medicine finings KBT-ZTC; Described step 3) and 4) in the eluent used be the aqueous solution.
Step 5) in ethanol refine as utilizing ethanol to dissolve the beet aglucone V obtaining after dry completely, remove by filter throw out, concentrate drying is to beet aglucone V product water content≤10% again.
The present embodiment obtains product purity and reaches 98.2%.
Embodiment 4
A preparation method for Momordica grosvenori mogroside V, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, with the Grosvenor Momordica extracting after solvent countercurrent extraction or refluxing extraction fragmentation, the ratio=4L:1kg of extraction agent and Grosvenor Momordica, extraction time is 5 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.05kg:1L of finings and extracting solution, after stirring, standing 25 ~ 40min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 1.6 meters of resin loading heights, extract solution absorbs flow velocity 2.5BV/hr, adsorb the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.45L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.25L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 600rpm, temperature are under the condition of 30 DEG C, concentrate drying is to beet aglucone V product water content≤10%, refining through ethanol again, obtain beet aglucone V product.
While adopting refluxing extraction in extraction step, refluxing extraction is divided and is carried out for 3 times, each 2 hours; Described extraction agent is pure water.
Finings in clarification removal step is natural traditional Chinese medicine finings KBT-ZTC; Described step 3) and 4) in the eluent used be ethanol.
Step 5) in ethanol refine as utilizing ethanol to dissolve the beet aglucone V obtaining after dry completely, remove by filter throw out, concentrate drying is to beet aglucone V product water content≤10% again.
The present embodiment obtains product purity and reaches 97.8%.
Embodiment 5
A preparation method for Momordica grosvenori mogroside V, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, the Grosvenor Momordica after the 60% aqueous ethanolic solution refluxing extraction fragmentation of use extraction solvent 3 times, the ratio=6L:1kg of extraction agent and Grosvenor Momordica, each extraction time is 2.5 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.05kg:1L of finings and extracting solution, after stirring, standing 25min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 2 meters of resin loading heights, extract solution absorbs flow velocity 2.5BV/hr, have adsorbed the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.5L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.2L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 500rpm, temperature are under the condition of 37 DEG C, concentrate drying is to beet aglucone V product water content≤10%, after dissolving beet aglucone V completely with 60% aqueous ethanolic solution again, remove by filter precipitation, reconcentration is dried to beet aglucone V product water content≤10%, obtains beet aglucone V product.
The present embodiment obtains product purity and reaches 98.9%.
Embodiment 6
A preparation method for Momordica grosvenori mogroside V, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, the Grosvenor Momordica after the 60% aqueous ethanolic solution refluxing extraction fragmentation of use extraction solvent 3 times, the ratio=6L:1kg of extraction agent and Grosvenor Momordica, each extraction time is 2.5 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.1kg:1L of finings and extracting solution, after stirring, standing 40min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 2 meters of resin loading heights, extract solution absorbs flow velocity 2.5BV/hr, have adsorbed the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.5L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.2L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 500rpm, temperature are under the condition of 37 DEG C, concentrate drying is to beet aglucone V product water content≤10%, after dissolving beet aglucone V completely with 60% aqueous ethanolic solution again, remove by filter precipitation, reconcentration is dried to beet aglucone V product water content≤10%, obtains beet aglucone V product.
The above embodiment of the present invention scheme is only can not limit the present invention to explanation of the present invention, in claim, point out the scope of product moiety of the present invention, component proportions, preparation method's parameter, and the scope of parameter of the present invention is not pointed out in above-mentioned explanation, therefore, any change in implication and the scope suitable with claims of the present invention, is all considered to be in the scope that is included in claims.
The present invention is the researchist's long term operation experience accumulation through the preparation method of multidigit Momordica grosvenori mogroside V, and creates by creative work, and product purity reaches more than 97%.
Claims (5)
1. a preparation method for Momordica grosvenori mogroside V, is characterized in that, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, with the Grosvenor Momordica extracting after solvent countercurrent extraction or refluxing extraction fragmentation, the ratio=2 ~ 8L:1kg of extraction agent and Grosvenor Momordica, extraction time is 3 ~ 8 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.05 ~ 0.1kg:1L of finings and extracting solution, after stirring, standing 25 ~ 40min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 1.5 ~ 2 meters of resin loading heights, extract solution absorbs flow velocity 1-4BV/hr, adsorb the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.3 ~ 0.6L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.1 ~ 0.4L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 300 ~ 800rpm, temperature are under the condition of 30 ~ 37 DEG C, concentrate drying is to beet aglucone V product water content≤10%, refining through ethanol again, obtain beet aglucone V product.
2. the preparation method of Momordica grosvenori mogroside V according to claim 1, is characterized in that, while adopting refluxing extraction in described extraction step, refluxing extraction is divided and carried out for 2 ~ 3 times, each 2 hours; Described extraction agent be in 40 ~ 80% aqueous ethanolic solution, pure water any.
3. according to the preparation method of the Momordica grosvenori mogroside V described in right 1 ~ 2 any one, it is characterized in that, the finings in described clarification removal step is natural traditional Chinese medicine finings KBT-ZTC; Described step 3) and 4) in the eluent used be any in ethanol or the aqueous solution.
4. the preparation method of Momordica grosvenori mogroside V according to claim 3, it is characterized in that, described step 5) in ethanol refine as utilizing ethanol to dissolve the beet aglucone V obtaining after dry completely, remove by filter throw out, concentrate drying is to beet aglucone V product water content≤10% again.
5. the preparation method of Momordica grosvenori mogroside V according to claim 1, is characterized in that, the method step comprises:
Step 1) extract: get ripe arhat fresh fruit and carry out fragmentation, the Grosvenor Momordica after the 60% aqueous ethanolic solution refluxing extraction fragmentation of use extraction solvent 3 times, the ratio=6L:1kg of extraction agent and Grosvenor Momordica, each extraction time is 2.5 hours, obtains extracting solution;
Step 2) clarification removal of impurities: in step 1) and add finings in the extracting solution that obtains, the ratio=0.05 ~ 0.1kg:1L of finings and extracting solution, after stirring, standing 25 ~ 40min, removes by filter precipitation, obtains the solution after removal of impurities;
Step 3) upper prop absorption: by step 2) solution that obtains after removal of impurities passes through absorption with macroporous adsorbent resin, 2 meters of resin loading heights, extract solution absorbs flow velocity 2.5BV/hr, have adsorbed the rear eluting solvent wash-out of using, eluent and extraction solution proportion=0.5L:1L, collect elutriant I;
Step 4) secondary upper prop absorption: by step 3) the elutriant I that obtains adsorbs by ion exchange resin, adsorb the rear eluting solvent wash-out of use, eluent and extraction solution proportion=0.2L:1L, collection elutriant II;
Step 5) concentrate drying is refining: by step 4) the elutriant II that obtains adopts traditional vacuum concentrate drying, in the situation that vacuumizing, centrifugal speed is that 500rpm, temperature are under the condition of 37 DEG C, concentrate drying is to beet aglucone V product water content≤10%, after dissolving beet aglucone V completely with 60% aqueous ethanolic solution again, remove by filter precipitation, reconcentration is dried to beet aglucone V product water content≤10%, obtains beet aglucone V product.
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Cited By (5)
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| CN106943447A (en) * | 2017-04-01 | 2017-07-14 | 成都普睿法药物研发有限公司 | A kind of preparation method of Fructus Monordicae extract |
| WO2018166029A1 (en) * | 2017-03-14 | 2018-09-20 | 桂林莱茵生物科技股份有限公司 | Method for separating and purifying mogroside v by means of subcritical hydrolytic adsorption technology |
| WO2020048049A1 (en) * | 2018-09-06 | 2020-03-12 | 湖南绿蔓生物科技股份有限公司 | Method for preparing luo han guo sweetener composition from siraitia grosvenorii and use thereof |
| CN114539330A (en) * | 2022-02-16 | 2022-05-27 | 广西扶南东亚糖业有限公司 | Extraction method and application of mogroside |
| CN115873059A (en) * | 2023-01-05 | 2023-03-31 | 湖南华康生物资源有限公司 | Method for separating mogroside V from waste liquid of fructus momordicae extraction |
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| WO2018166029A1 (en) * | 2017-03-14 | 2018-09-20 | 桂林莱茵生物科技股份有限公司 | Method for separating and purifying mogroside v by means of subcritical hydrolytic adsorption technology |
| US10759827B2 (en) | 2017-03-14 | 2020-09-01 | Guilin Layn Natural Ingredients Corp. | Method for separating and purifying mogroside V by subcritical water desorption technology |
| CN106943447A (en) * | 2017-04-01 | 2017-07-14 | 成都普睿法药物研发有限公司 | A kind of preparation method of Fructus Monordicae extract |
| WO2020048049A1 (en) * | 2018-09-06 | 2020-03-12 | 湖南绿蔓生物科技股份有限公司 | Method for preparing luo han guo sweetener composition from siraitia grosvenorii and use thereof |
| CN114539330A (en) * | 2022-02-16 | 2022-05-27 | 广西扶南东亚糖业有限公司 | Extraction method and application of mogroside |
| CN115873059A (en) * | 2023-01-05 | 2023-03-31 | 湖南华康生物资源有限公司 | Method for separating mogroside V from waste liquid of fructus momordicae extraction |
| CN115873059B (en) * | 2023-01-05 | 2024-03-26 | 湖南华康生物资源有限公司 | Method for separating mogroside V from fructus Siraitiae Grosvenorii extraction waste liquid |
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