A mogroside content controllable momordica grosvenori extract and a preparation method thereof

Abstract

The present application provides a mogroside content controllable momordica grosvenori extract, which is obtained by cyclic supersaturation adsorption of macroporous adsorption resin in the momordica grosvenori extraction process, concentration and drying of the overflow of the supersaturation column to obtain momordica grosvenori extract product I, and concentration and drying of the alcohol eluent of the macroporous adsorption resin to obtain momordica grosvenori extract product II. The momordica grosvenori extract product I comprises the following components: 10-18 wt% 11-oxymogroside V, 48-52 wt% mogroside V, 0.05-1 wt% mogroside VI, 0.05-1 wt% siamenoside, 0.5-2 wt% mogroside IV, and 0.5-2 wt% mogroside III. The momordica grosvenori extract product II comprises the following components: 0.5-2 wt% 11-oxymogroside V, 48-52 wt% mogroside V, 2-6 wt% mogroside VI, 2-6 wt% siamenoside, 1-6 wt% mogroside IV, and 1-6 wt% mogroside III. The products I and II have different rare mogroside contents from conventional V50 products, the product I has higher sweetness multiple, and the product II has better taste.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of momordica grosvenori extract, in particular to a momordica grosvenori extract with improved taste and a preparation method thereof. BACKGROUND

[0002] Momordica grosvenori is the fruit of a perennial vine of the family cucurbitaceae, which is produced in the mountainous areas of Guilin, Guangxi, Shaoyang, Huaihua, Yongzhou, Guizhou, and other places, and is a rare local specialty in China and one of the first "food and medicine" materials approved by the state. Momordica grosvenori has high nutritional value and contains a large amount of vitamin C, momordica grosvenori glycosides, fructose, glucose, protein, pectin, and lipids. According to the Chinese Materia Medica, momordica grosvenori has a sweet and cool taste, and is related to the lung and large intestine channels, and has the effects of moistening the lung to stop coughing, producing saliva to stop thirst, and is suitable for treating lung heat or lung dryness cough, whooping cough, and thirst due to summer heat, and has the effect of moistening the intestine to relieve constipation. Modern medical research has confirmed that momordica grosvenori glycosides, a natural sweetener 400 times sweeter than sucrose, are a sweetener substitute for people with diabetes, obesity, and other conditions that should not eat sugar. Momordica grosvenori glycosides are safe and non-toxic as food additives, and are allowed to be used in various foods without limitation in the national mandatory standard GB2760 Food Additive Usage Standard. Due to its many excellent properties, momordica grosvenori glycosides can completely or partially replace sucrose, and therefore have been widely used in the food industry. In addition, momordica grosvenori glycosides have a very broad application prospect and market potential in the fields of pharmaceuticals, cosmetics, and health foods.

[0003] Momordica grosvenori glycosides are not a single natural compound, but a general term for a variety of saponins with common cucurbitane-type tetracyclic triterpenes. So far, more than 20 momordica grosvenori glycosides have been isolated and identified from momordica grosvenori by Chinese researchers. Among them, the highest content is momordica grosvenori glycoside V (accounting for about 80% of the total momordica grosvenori glycosides), and the momordica grosvenori glycosides other than momordica grosvenori glycoside V are usually referred to as rare momordica grosvenori glycosides; among the rare momordica grosvenori glycosides, 11-oxo-momordica grosvenori glycoside V has the highest content. Commercial momordica grosvenori extract products are usually differentiated by the content of momordica grosvenori glycoside V and priced accordingly, and there is no clear requirement for the content and proportion of various rare momordica grosvenori glycosides.

[0004] The research found that during the growth and maturation of momordica grosvenori, under the action of a series of unique biological enzymes, a common mother nucleus structure of various momordica grosvenori glycosides, momordica grosvenori alcohol, was gradually formed; then, under the action of related glycosyltransferases, one or more glucose groups were transferred to several specific C atoms of the momordica grosvenori alcohol molecule, thereby completing the biosynthesis of momordica grosvenori glycosides. Due to the different positions and quantities of the transferred glucose groups on the momordica grosvenori alcohol molecule, the momordica grosvenori glycosides are diverse. Therefore, the content of various momordica grosvenori glycosides is mainly determined by the expression of the innate genetic genes, except for the influence of postnatal planting and cultivation.

[0005] Although the contents of various momordica grosvenori glycosides in natural momordica grosvenori are different, the content proportions of various momordica grosvenori glycosides are relatively stable under the same variety and the same maturity. Therefore, if not subjected to special process treatment, the content proportions of various momordica grosvenori glycosides in the traditional momordica grosvenori extract V50 commonly seen on the market are basically consistent with the content proportions of various momordica grosvenori glycosides in momordica grosvenori raw materials.

[0006] CN113461765A discloses a method for separating momordica grosvenori glycoside V and rare momordica grosvenori glycosides. After momordica grosvenori glycosides are dissolved and degassed, a sample solution is obtained. After the sample solution is loaded into a multi-stage cascade chromatographic column in which an imprint polymer chromatographic column and a macroporous adsorption resin chromatographic column are connected in series, the column is sequentially washed with degassed ethanol aqueous solution and degassed water, and then the vacuum is released to normal pressure. The imprint polymer chromatographic column is desorbed with a mixed solution of acetonitrile and ethanol, and the desorption solution containing rare momordica grosvenori glycosides is collected. The macroporous adsorption resin chromatographic column is desorbed with ethanol aqueous solution, and the desorption solution containing momordica grosvenori glycoside V is collected. The method has high yield and high purity of the collected momordica grosvenori glycosides, and the chromatographic column can be recycled. The patent method is used to obtain rare momordica grosvenori glycosides in momordica grosvenori, rather than to obtain an extract with different proportions of momordica grosvenori rare glycosides.

[0007] At present, there is no literature that clearly records a method for redistributing and recombining various momordica grosvenori glycoside components in momordica grosvenori extract V50 products. Unlike momordica grosvenori extract V50 products produced by traditional processes, the method of the present application provides a momordica grosvenori extract with special content of one or two momordica grosvenori glycosides and a preparation method thereof. SUMMARY

[0008] In order to solve the problem that the content of momordica grosvenori glycosides in the extract obtained by the momordica grosvenori extraction process in the prior art is basically consistent with that in momordica grosvenori raw materials, and different specifications of momordica grosvenori extract cannot be obtained, the present application provides a momordica grosvenori extract with controllable content of momordica grosvenori glycosides and a preparation method thereof, which can continuously process a large amount of raw materials, has simple equipment and low production cost.

[0009] The present application provides the following technical solutions:

[0010] The present application provides a mogroside content controllable momordica grosvenori extract, which is obtained by cyclic supersaturation adsorption of macroporous adsorption resin in the momordica grosvenori extraction process, concentration and drying of the overflow of the supersaturation column to obtain momordica grosvenori extract product I, and concentration and drying of the alcohol eluent of the macroporous adsorption resin to obtain momordica grosvenori extract product II.

[0011] The momordica grosvenori extract product I comprises the following components: 10-18wt% 11-oxymogroside V, 48-52wt% mogroside V, 0.05-1wt% mogroside VI, 0.05-1wt% siamenoside, 0.5-2wt% mogroside IV, and 0.5-2wt% mogroside III.

[0012] The momordica grosvenori extract product II comprises the following components: 0.5-2wt% 11-oxymogroside V, 48-52wt% mogroside V, 2-6wt% mogroside VI, 2-6wt% siamenoside, 1-6wt% mogroside IV, and 1-6wt% mogroside III.

[0013] Preferably, the momordica grosvenori extract product I comprises the following components: 9-15wt% 11-oxymogroside V, 49-51wt% mogroside V, 0.06-0.8wt% mogroside VI, 0.06-0.5wt% siamenoside, 0.8-1.8wt% mogroside IV, and 0.8-1.8wt% mogroside III; and the momordica grosvenori extract product II comprises the following components: 0.8-1.8wt% 11-oxymogroside V, 49-52wt% mogroside V, 3-5wt% mogroside VI, 2.5-5wt% siamenoside, 2-5wt% mogroside IV, and 1.5-5wt% mogroside III.

[0014] The present application also provides a momordica grosvenori extract with improved taste and mouthfeel, which is the momordica grosvenori extract product II described above and comprises the following components: 0.5-2wt% 11-oxymogroside V, 48-52wt% mogroside V, 2-6wt% mogroside VI, 2-6wt% siamenoside, 1-6wt% mogroside IV, and 1-6wt% mogroside III.

[0015] Preferably, the momordica grosvenori extract product II comprises the following components: 0.8-1.8wt% 11-oxymogroside V, 49-52wt% mogroside V, 3-5wt% mogroside VI, 2.5-5wt% siamenoside, 2-5wt% mogroside IV, and 1.5-5wt% mogroside III.

[0016] The product II of Momordica grosvenori extract is obtained by the following steps: the product I of Momordica grosvenori extract is obtained by the process of cyclic supersaturation adsorption of macroporous adsorption resin, and the product II of Momordica grosvenori extract is obtained by the process of concentration and drying of the effluent of the supersaturation adsorption, and the alcohol eluent of the macroporous adsorption resin is concentrated and dried to obtain the product II of Momordica grosvenori extract. Compared with the conventional Momordica grosvenori extract V50 (the contents of mogroside V in the three are close to 50%), the contents of rare mogrosides in the product I and the product II are significantly different. In the product I, 11-oxymogroside V is more enriched, and in the product II, mogroside VI, siamenoside, mogroside IV and mogroside III are more enriched. The inventors unexpectedly found that the product II has a more excellent subjective evaluation of taste than V50.

[0017] The present application also provides a preparation method of the Momordica grosvenori extract with controllable mogroside content, comprising the following steps:

[0018] (1) extraction of total mogrosides of Momordica grosvenori:

[0019] 1a, enzyme inactivation and crushing: taking Momordica grosvenori raw materials, enzyme inactivation is performed before or after crushing;

[0020] 1b, extraction: the enzyme inactivation and crushing treated raw materials are extracted with a solvent, and the solvent is water and / or alcohol;

[0021] 1c, filtration: the extract is filtered to obtain a filtrate;

[0022] (2) enrichment of total mogrosides of Momordica grosvenori:

[0023] 2a, macroporous resin adsorption chromatography: the filtrate is columned on a macroporous adsorption resin column A until the resin is saturated with adsorption;

[0024] 2b, impurity removal and elution of the macroporous resin column: after columning, the resin column A is first eluted with acid and / or base, then washed with water until the pH value of the effluent is neutral, and finally eluted with ethanol, and the ethanol eluent A is collected;

[0025] (3) decolorization of total mogrosides of Momordica grosvenori: the ethanol eluent A is concentrated to be alcohol-free, and then decolorized by a combination of cation and anion exchange resin columns, and the decolorized liquid is collected for use;

[0026] (4) re-enrichment and distribution recombination of various mogroside components:

[0027] 4a, saturated adsorption: the decolorized liquid is columned on a macroporous adsorption resin column B for adsorption until the resin is saturated with adsorption, and the unsaturated column effluent without sweetness is discarded;

[0028] 4b, supersaturation adsorption: after the macroporous adsorption resin column B is saturated with adsorption, the decolorized liquid is continuously columned until all the decolorized liquid is columned, and the supersaturated column effluent with sweetness is collected.

[0029] 4c, circulating supersaturation adsorption: at this time, the material of the macroporous adsorption resin column B is no longer the decolorizing solution, but the supersaturated column effluent with sweetness from the previous step. Similarly, the supersaturated column effluent with sweetness in this step is collected as the material for subsequent column adsorption, and the column adsorption is repeated in this way;

[0030] 4d, collection and elution: after the repeated circulation of the supersaturation adsorption is completed, the collected supersaturated column effluent is concentrated and dried to obtain product I; the macroporous adsorption resin column B is eluted with ethanol, and the eluate B is collected, the ethanol is recovered, concentrated, and dried to obtain product II.

[0031] Preferably, in step (1a), the enzyme inactivation method includes but is not limited to hot water inactivation, steam inactivation, hot air inactivation, acid-base inactivation, radiation inactivation, microwave inactivation, and ray inactivation.

[0032] Preferably, in step (1b), the extraction method includes but is not limited to traditional fraction extraction, reflux extraction, countercurrent extraction, beating extraction, squeezing extraction, microwave-assisted extraction, subcritical extraction, and supercritical extraction.

[0033] Preferably, in step (1b), the alcohol is selected from ethanol, and the solvent usage is 2-10 times the mass of the momordica grosvenori material, such as 3 times, 4 times, 5 times, 6 times, 7 times, or 8 times.

[0034] Preferably, in step (1c), the filtration method includes but is not limited to screen filtration, filter cloth filtration, plate and frame filtration, centrifugal filtration, sedimentation filtration, titanium rod filtration, membrane filtration, ceramic membrane filtration, ultrafiltration, nanofiltration, and combinations of the above filtration methods.

[0035] Preferably, in step (2a), in the macroporous adsorption resin column A, the type of macroporous adsorption resin used is non-polar macroporous adsorption resin, medium-polar macroporous adsorption resin, or weak-polar macroporous adsorption resin, or a combination of two or more of the above resins; the height-diameter ratio of the macroporous adsorption resin column A is 0.5:1-20:1, preferably 2-10:1, such as 4:1; the column flow rate is 0.1-10 BV / hour, preferably 0.5-4 BV / hour, such as 0.8 BV / hour.

[0036] Preferably, in step (2b), the acid solution is selected from at least one of 0.5-5wt% hydrochloric acid and sulfuric acid, and the alkali solution is selected from at least one of 0.5-5wt% NaOH solution and KOH solution; the usage of the acid solution / alkali solution is 1-2 BV.

[0037] Preferably, in step (3), the combination mode and sequence of the anion and cation exchange resin columns include, but are not limited to, "anion first and then cation", "cation first and then anion", "cation + anion + cation", "anion + cation + anion", "cation + anion + anion", "anion + cation + cation", "cation + cation + anion", "anion + anion + cation", "anion + cation + anion + cation", "cation + anion + cation + anion", "cation + anion + anion + cation", "anion + cation + cation + anion".

[0038] Preferably, in step (3), the anion exchange resin is selected from at least one of LX-T5 and D941; the cation exchange resin is selected from at least one of 001x16 and 732. The height-diameter ratio of the anion and cation exchange resins is 2-4:1, such as 3.5:1, and the column loading flow rate is 1-2 BV / hour.

[0039] Preferably, in step (4), the macroporous adsorption resin used in the macroporous adsorption resin column B is a non-polar macroporous adsorption resin, a medium-polar macroporous adsorption resin, or a weak-polar macroporous adsorption resin, or a combination of two or more of the above resins.

[0040] Preferably, in step (4), the height-diameter ratio of the macroporous adsorption resin column B is 0.5:1-20:1, preferably 2-10:1, such as 5:1, and the column loading flow rate is 0.1-10 BV / hour, preferably 0.3-3 BV / hour, such as 0.5 BV / hour.

[0041] 10:1, such as 5:1, and the column loading flow rate is 0.1-10 BV / hour, preferably 0.3-3 BV / hour, such as 0.5 BV / hour.

[0042] Preferably, in step (4), the amount of macroporous adsorption resin used in the macroporous adsorption resin column B is 0.5-20 times (V / m, L / Kg) the weight of the solids in the decoloring solution.

[0043] Preferably, in step (4), the number of times of cyclic supersaturation adsorption is 1-50 times, preferably 5-10 times.

[0044] In the cyclic supersaturation adsorption, all the decoloring solution is passed through the macroporous adsorption resin column B, the unsaturated column effluent without sweetness is discarded (i.e., step 4a is completed), and all the supersaturated effluent is collected (i.e., step 4b is completed). The supersaturated effluent is again loaded onto the macroporous adsorption resin column B, which is referred to as the first cyclic supersaturation adsorption. After the first cyclic supersaturation adsorption is completed, the supersaturated effluent of the first cyclic supersaturation adsorption is collected, and the supersaturated effluent is again repeatedly loaded onto the macroporous adsorption resin column B, which is referred to as the second cyclic supersaturation adsorption. The number of times of cyclic supersaturation adsorption is counted in this way.

[0045] In the present application, 1 BV = 1 resin column volume.

[0046] The method of the present application controls the number of times of cyclic supersaturation adsorption, thereby regulating the content of rare mogrosides in products I and II. The more the number of times of cyclic supersaturation adsorption, the less the enrichment degree of 11-oxymogroside V in product I, and the more the enrichment degree of mogroside VI, siamenoside, mogroside IV and mogroside III in product II. With the increase of the enrichment degree of mogroside VI, siamenoside, mogroside IV and mogroside III, the flavor and taste of product II are better than those of conventional V50.

[0047] Compared with other prior arts, the present application has the following characteristics:

[0048] (1) The method of the present application can continuously process a large amount of raw materials, has simple equipment, low production cost and strong operability, and is suitable for industrialized continuous production. The process of the present application is different from that for preparing conventional V50% product of momordica grosvenori, and the present method can simultaneously obtain two kinds of momordica grosvenori extract products with special contents of mogrosides, and the contents of rare mogrosides have a large difference.

[0049] (2) The two kinds of momordica grosvenori extract products with special contents of mogrosides prepared by the method of the present application have the following advantages compared with conventional V50% product, because the contents and proportions of various mogrosides (especially rare mogrosides other than mogroside V) are different: in product I, the contents of two rare mogrosides (mogroside VI and siamenoside) with the best sweetness and flavor are significantly higher than those of conventional V50% product, so product II has better flavor and taste than conventional mogroside product V50; in product II, the total content of mogrosides (especially the content of 11-oxymogroside V + the content of mogroside V) is significantly higher than that of conventional V50% product, so the sweetness multiple of product II exceeds that of conventional V50% product. The characteristics of the two products are different, and can meet different application scenarios and market demands. BRIEF DESCRIPTION OF DRAWINGS

[0050] Figure 1 The figure is a schematic diagram of the process of the present application.

[0051] Figure 2 The figure is a schematic diagram of the process of the present application. DETAILED DESCRIPTION

[0052] The present application will be described below through specific examples, but the present application is not limited thereto.

[0053] The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents, materials, etc. used in the following examples can be obtained from commercial channels unless otherwise specified.

[0054] Example 1

[0055] (1) Extraction of total mogrosides from Momordica grosvenori Swingle:

[0056] 1a, Enzyme inactivation and crushing: 10 tons of fresh Momordica grosvenori Swingle fruits were put into hot water at a temperature of 100°C so that the fresh fruits were completely immersed in the hot water, and then soaked for 30 minutes to inactivate the enzymes. Then the fresh fruits were taken out of the hot water and crushed by a pulper.

[0057] 1b, Extraction: The crushed and enzyme-inactivated material was extracted by a countercurrent extractor, and the amount of water used for extraction was 3 times the weight of the material. The extraction temperature was 95°C, and an extract was obtained.

[0058] 1c, Filtration: The extract was filtered by a horizontal screw centrifuge and a disc centrifuge in sequence, and then filtered by a ceramic membrane, and a filtrate was obtained.

[0059] (2) Enrichment of total mogrosides from Momordica grosvenori Swingle:

[0060] 2a, Macroporous resin adsorption chromatography: The filtrate was loaded onto a macroporous adsorption resin column A (in which, the macroporous adsorption resin was labeled as D101, the amount of resin used was 2500L, and the height-diameter ratio of the resin column was 4:1), and the flow rate of loading was 0.8BV / hour, until the resin was saturated.

[0061] 2b, Removal of impurities and elution from the macroporous resin column: After loading, the resin column A was first eluted with 2BV of a 0.5% sodium hydroxide aqueous solution at a flow rate of 1BV / hour to remove impurities, and then washed with water until the pH value of the effluent was neutral. Finally, the column was eluted with 2BV of ethanol with a volume fraction of 70%, and the ethanol eluate A was collected.

[0062] (3) Decolorization of total mogrosides from Momordica grosvenori Swingle: The ethanol eluate A was concentrated to remove alcohol, and then decolorized by a combination of cation and anion exchange resin columns in the order of "cation + anion + cation" (in which, the cation exchange resin in the first resin column was labeled as 732, the amount of resin used was 500L, and the height-diameter ratio of the resin column was 4:1; the anion exchange resin in the second resin column was labeled as D941, the amount of resin used was 500L, and the height-diameter ratio of the resin column was 4:1; the cation exchange resin in the third resin column was labeled as 732, the amount of resin used was 500L, and the height-diameter ratio of the resin column was 4:1), and the flow rate of loading was 1BV / hour. The decolorized liquid was collected for use. The weight of the solid in the decolorized liquid was about 85kg as measured by sampling.

[0063] (4) Re-enrichment and distribution recombination of various mogrosides:

[0064] 4a, saturated adsorption: take the decoloring liquid to column, and adsorb with macroporous adsorption resin column B (in which, the macroporous adsorption resin is LX-T28, the resin amount is 400L, and the height-diameter ratio of the resin column is 5:1), the flow rate of column is 0.5BV / hour, until the resin is saturated, and the unsaturated column effluent without sweet taste is discarded;

[0065] 4b, supersaturated adsorption: after the macroporous adsorption resin column B is saturated, take the decoloring liquid to continue column, the flow rate of column is kept 0.5BV / hour, until all the decoloring liquid is columned, and the supersaturated column effluent with sweet taste is collected;

[0066] 4c, cyclic supersaturated adsorption: at this time, the material columned in the macroporous adsorption resin column B is not the decoloring liquid, but the supersaturated column effluent with sweet taste in the last step, and the supersaturated column effluent with sweet taste in this step is also collected as the material for subsequent column, and the column is repeated for 5 times.

[0067] 4d, collection and elution: after the cyclic supersaturated adsorption is completed, the collected supersaturated column effluent is concentrated and dried to obtain 49.68kg product I; the macroporous adsorption resin column B is eluted with 2BV of 70% ethanol, the eluate B is collected, the ethanol is recovered, concentrated, and the concentrated liquid is dried to obtain 35.19kg product II.

[0068] The contents of the mogrosides in the product I and the product II are shown in the following table by HPLC external standard method:

[0069]

[0070] Example 2

[0071] (1) Extraction of total mogrosides of momordica grosvenori:

[0072] 1a, crushing: take 10 tons of fresh momordica grosvenori as raw material, and crush with a beater.

[0073] 1b, extraction and enzyme inactivation: extract the crushed momordica grosvenori raw material with a countercurrent extractor, the water amount for extraction is 3 times the weight of the raw material, and the extraction temperature is 95℃, to obtain an extraction liquid; pass the extraction liquid through a continuous enzyme inactivator with a maximum temperature of 120℃, to obtain an extraction liquid after enzyme inactivation.

[0074] 1c, filtration: filter the extraction liquid after enzyme inactivation with a horizontal screw centrifuge and a disc centrifuge in turn, and then filter with a ceramic membrane, to obtain a filtrate.

[0075] (2) Enrichment of total mogrosides of momordica grosvenori:

[0076] 2a, macroporous resin adsorption chromatography: the filtrate is loaded onto a macroporous adsorption resin column A (wherein the macroporous adsorption resin is AB-8, the resin amount is 2800L, and the height-diameter ratio of the resin column is 5:1), the loading flow rate is 1 BV / hour, and the loading is continued until the resin is saturated.

[0077] 2b, impurity removal and elution of the macroporous resin column: after the loading, the resin column A is first eluted with 2 BV of 0.5% sodium hydroxide aqueous solution at a flow rate of 1 BV / hour to remove impurities, then washed with water until the effluent is neutral, and finally eluted with 2 BV of 70% ethanol, and the ethanol eluate A is collected.

[0078] (3) decolorization of total mogrosides: the ethanol eluate A is concentrated to remove ethanol, and then subjected to decolorization by a combination of cation and anion exchange resin columns in the order of "cation + anion + anion + cation" (wherein the cation exchange resin in the first resin column is 001*16, the resin amount is 450L, and the height-diameter ratio of the resin column is 3.5:1; the anion exchange resin in the second resin column is LX-T5, the resin amount is 450L, and the height-diameter ratio of the resin column is 3.5:1; the anion exchange resin in the third resin column is LX-T5, the resin amount is 450L, and the height-diameter ratio of the resin column is 3.5:1; and the cation exchange resin in the fourth resin column is 001*16, the resin amount is 450L, and the height-diameter ratio of the resin column is 3.5:1), the loading flow rate is 1 BV / hour, and the decolorized liquid is collected for use. The weight of the solid in the decolorized liquid is about 83 kg as determined by sampling.

[0079] (4) re-enrichment and distribution recombination of various mogroside components:

[0080] 4a, saturated adsorption: the decolorized liquid is loaded onto a macroporous adsorption resin column B (wherein the macroporous adsorption resin is D101c, the resin amount is 300L, and the height-diameter ratio of the resin column is 4:1), the loading flow rate is 2 BV / hour, and the loading is continued until the resin is saturated, and the unsaturated loading effluent without sweetness is discarded;

[0081] 4b, supersaturated adsorption: after the saturated adsorption of the macroporous adsorption resin column B, the decolorized liquid is continuously loaded, the loading flow rate is maintained at 2 BV / hour, and the loading is continued until all the decolorized liquid is loaded, and the supersaturated loading effluent with sweetness is collected;

[0082] 4c, cyclic supersaturated adsorption: at this time, the material loaded onto the macroporous adsorption resin column B is not the decolorized liquid, but the supersaturated loading effluent with sweetness from the previous step, and the supersaturated loading effluent with sweetness in this step is also collected as the material for subsequent loading, and the loading is repeated for 10 times.

[0083] 4d, collection and elution: after the repeated over-saturation adsorption was completed, the collected over-saturation column effluent was concentrated and dried to obtain 53.75 kg of product I; the macroporous adsorption resin column B was eluted with 2 BV of 70% ethanol, the eluate B was collected, the ethanol was recovered, concentrated, and the concentrated solution was dried to obtain 28.75 kg of product II.

[0084] The contents of the mogrosides in the products I and II were detected by high performance liquid chromatography (HPLC) external standard method as shown in the following table:

[0085]

[0086] Comparative Example 1

[0087] Steps (1), (2) and (3) were completely consistent with Example 1, but step (4) was not performed.

[0088] The decolorized solution obtained in step (3) was concentrated and spray dried to obtain 84.67 kg of traditional V50 product with normal content of mogrosides.

[0089] The content of the mogrosides in the product was detected by high performance liquid chromatography (HPLC) external standard method as shown in the following table:

[0090]

[0091] Application Example 1

[0092] The products of the above examples and comparative examples were tested for the following performances:

[0093] 1. Flavor and taste test:

[0094] According to the provisions of GB / T 16291.2-2010, sensory evaluation personnel were screened, and after taste sensitivity training, 20 subjects (half male and half female) were finally selected to form a sensory evaluation team.

[0095] The subjects were restricted in diet within 1 h before the experiment, and 10 most suitable sensory evaluation personnel were selected from the 20 subjects for different taste experiments to set up samples for sensory test. The monk fruit extracts of the examples and comparative examples were diluted with water to the same sweetness as a 5% sucrose aqueous solution, and the subjects were asked to taste each sample. After the evaluation of each sample was completed, the subjects rinsed their mouths with 20±2℃ water, and after an interval of 30 min, the next sensory test was performed. The scoring was evaluated according to a full score of 5 points and a minimum score of 1 point. The higher the score, the better the taste.

[0096] 2. Sweetness multiple

[0097] 1), reagents and containers: sucrose, monk fruit extract sample, distilled water, 100 ml volumetric flask, 10 ml graduated pipette

[0098] 2) Operation steps:

[0099] Preparation of control sample (5% sucrose solution): weigh 5g sucrose solution, dilute with distilled water to 100ml.

[0100] 3) Preparation of series concentration sample: weigh 1.0g sample, dilute with distilled water to 100ml to form 1.0% sample solution. Respectively take 10ml, 7ml, 5.0ml, 4ml, 3.3ml, 2.5ml, 2ml, 1.66ml, 1.25ml of 1.0% sample solution to 100ml volumetric flask, dilute to 100ml, the solution concentration is 0.1%, 0.07%, 0.05%, 0.04%, 0.033%, 0.025%, 0.02%, 0.015%, 0.0125% respectively.

[0101] 4) Sample taste comparison: at least 10 people constitute the evaluation group to taste the sample, judge which one of the series concentration sample is the same or similar to the sweetness of 5% sucrose solution, so as to calculate the sweetness of the sample.

[0102] The formula is as follows: sweetness = 5% / diluted sample concentration

[0103] The relationship between the sweetness of the sample and the concentration is shown in Table 1 below:

[0104] Table 1

[0105] Amount of sample solution taken up Concentration of solution after dilution Sweetness equivalent to sucrose 10.0 0.1％ 50 7.0 0.07％ 70 5.0 0.05％ 100 4.0 0.04％ 125 3.3 0.033％ 150 2.5 0.025％ 200 2.0 0.02％ 250 1.66 0.0166％ 300 1.25 0.0125％ 400

[0106] The results are shown in Table 2 below.

[0107] Table 2

[0108]

[0109]

[0110] The inventor also tried other conditions and operations same as example 1, the only difference is that in step 4c, the number of repeated column cycles is changed to 2 and 30 respectively, but the flavor and taste of product II are worse than example 1, which shows that by controlling the number of repeated column cycles, the content of rare sweet glycosides can be adjusted, and when the content of specific rare sweet glycosides is adjusted, the product II will have significantly improved taste and flavor.

[0111] Application example 2

[0112] The evaluation is carried out by using TS-5000Z intelligent taste analysis system (electronic tongue), which is similar to the working principle of human tongue taste cells and can evaluate the basic taste sensory indexes of food or medicine samples such as bitter taste, astringent taste, sour taste, salty taste, umami taste, sweet taste, raw material taste and the like in a digital manner. Meanwhile, the aftertaste of bitterness, the aftertaste of astringency and the aftertaste of umami (richness) can also be analyzed. The traditional momordica grosvenori V50 product obtained in the comparative example, the product I and the product II obtained in example 1, and the V50 product prepared in comparative example 1 are all prepared into aqueous solutions with a mass percentage concentration of 0.05wt%, and the data obtained by electronic tongue evaluation is plotted as shown in Figure 2

[0113] As shown in Figure 2 Amount of sample solution taken up Concentration of solution after dilution Sweetness equivalent to sucrose Figure 2 Figure 2 Amount of sample solution taken up Concentration of solution after dilution Sweet the above three products have relatively small differences in sweet time, and have relatively obvious differences in sweetness multiple, fruit flavor, pureness of taste, softness and freshness. Although the sweetness multiple of the product II is slightly low, the fruit flavor, the pureness of taste, the softness and the freshness of the product II are obviously better than those of the product I and the traditional momordica grosvenori V50 product. Therefore, the taste of the product II obtained in example 1 is obviously improved.​

Claims

1. A method for preparing a mogroside content controllable monk fruit extract, characterized in that, The method comprises the following steps: (1) extraction of total mogrosides from Siraitia grosvenorii: (1a) enzyme inactivation and crushing: taking Siraitia grosvenorii raw materials, enzyme inactivation is performed before or after crushing; (1b) extraction: extracting the enzyme-inactivated and crushed raw materials with a solvent, the solvent being water and / or alcohol; (1c) filtration: filtering the extract to obtain a filtrate; (2) enrichment of total mogrosides from Siraitia grosvenorii: (2a) macroporous resin adsorption chromatography: loading the filtrate onto a macroporous adsorption resin column A until the resin is saturated; the type of macroporous adsorption resin used in the macroporous adsorption resin column A is nonpolar macroporous adsorption resin or weakly polar macroporous adsorption resin, or a combination of the two; the height-diameter ratio of the macroporous adsorption resin column A is 0.5:1-20:1, and the loading speed is 0.1-10 BV / hour; (2b) impurity removal and elution of the macroporous resin column: after loading, the macroporous adsorption resin column A is first eluted with a lye, then washed with water until the pH value of the effluent is neutral, and finally eluted with ethanol with a volume fraction of 70%, and the ethanol eluate A is collected; the lye is selected from at least one of 0.5-5wt% NaOH solution and KOH solution; the amount of lye is 1-2 BV; (3) decolorization of total mogrosides from Siraitia grosvenorii: concentrating the ethanol eluate A to remove alcohol, and then decolorizing it with a combination of cation and anion exchange resin columns, and collecting the decolorized liquid for later use; (4) re-enrichment and distribution recombination of various mogrosides: (4a) saturated adsorption: loading the decolorized liquid onto a macroporous adsorption resin column B for adsorption until the resin is saturated, and discarding the unsaturated effluent without sweetness; (4b) supersaturated adsorption: after the macroporous adsorption resin column B is saturated, the decolorized liquid is continuously loaded until all the decolorized liquid is loaded, and the supersaturated effluent with sweetness is collected; (4c) cyclic supersaturated adsorption: at this time, the material loaded onto the macroporous adsorption resin column B is not the decolorized liquid, but the supersaturated effluent with sweetness from the previous step, and the supersaturated effluent with sweetness from this step is also collected as the material for subsequent loading, and the process is repeated; (4d) collection and elution: after the repeated cyclic supersaturated adsorption is completed, the collected supersaturated effluent is concentrated and dried to obtain product I; the macroporous adsorption resin column B is eluted with ethanol, and the eluate B is collected, the ethanol is recovered, and the concentrated liquid is dried to obtain product II; the type of macroporous adsorption resin used in the macroporous adsorption resin column B is nonpolar macroporous adsorption resin, moderately polar macroporous adsorption resin, or weakly polar macroporous adsorption resin, or a combination of two or more of the above resins; the height-diameter ratio of the macroporous adsorption resin column B is 0.5:1-20:1, and the loading speed is 0.1-10 BV / hour; the amount of macroporous adsorption resin is 0.5-20 times the weight of the solid in the decolorized liquid, unit L / Kg. The mogroside extract product I includes the following components: 10-18 wt% 11-oxymogroside V, 48-52 wt% mogroside V, 0.05-1 wt% mogroside VI, 0.05-1 wt% siamenoside, 0.5-2 wt% mogroside IV, 0.5-2 wt% mogroside III; The mogroside extract product II includes the following components: 0.5-2 wt% 11-oxymogroside V, 48-52 wt% mogroside V, 2-6 wt% mogroside VI, 2-6 wt% siamenoside, 1-6 wt% mogroside IV, 1-6 wt% mogroside III.

2. The production method according to claim 1, characterized by, The mogroside extract product I includes the following components: 10-15 wt% 11-oxymogroside V, 49-51 wt% mogroside V, 0.06-0.8 wt% mogroside VI, 0.06-0.5 wt% siamenoside, 0.8-1.8 wt% mogroside IV, 0.8-1.8 wt% mogroside III; the mogroside extract product II includes the following components: 0.8-1.8 wt% 11-oxymogroside V, 49-52 wt% mogroside V, 3-5 wt% mogroside VI, 2.5-5 wt% siamenoside, 2-5 wt% mogroside IV, 1.5-5 wt% mogroside III.

3. The preparation method according to claim 1, characterized in that, In step (1a), the enzyme inactivation method includes hot water inactivation, steam inactivation, acid or alkali inactivation, radiation inactivation, microwave inactivation, high-energy electron beam inactivation, or high-voltage pulse electric field inactivation; In step (1b), the extraction method includes fraction extraction, reflux extraction, pulping extraction, squeezing extraction, microwave-assisted extraction, subcritical extraction, or supercritical extraction; In step (1b), the alcohol is selected from ethanol, and the solvent usage is 2-10 times the mass of the original momordica grosvenori material; In step (1c), the filtration method includes screen filtration, filter cloth filtration, plate and frame filtration, centrifugal filtration, sedimentation filtration, titanium rod filtration, ultrafiltration, or nanofiltration, and combinations of the above filtration methods.

4. The production method according to claim 1, characterized by, In step (2a), the height-diameter ratio of the macroporous adsorption resin column A is 2-10:1, and the column loading flow rate is 0.5-4 BV / hour.

5. The preparation method according to claim 1, characterized in that, In step (3), the combination mode and sequence of the cation and anion exchange resin columns include "first cation then anion", "first anion then cation", "cation + anion + cation", "anion + cation + anion", "cation + anion + anion", "anion + cation + cation", "cation + cation + anion", "anion + anion + cation", "anion + cation + anion + cation", "cation + anion + cation + anion", "cation + anion + anion + cation", or "anion + cation + cation + anion".

6. The method of claim 1, wherein, In step (4), the number of cycles of supersaturation adsorption is 1-50 times.

7. The production method according to claim 6, wherein In step (4), the number of cycles of supersaturation adsorption is 5-10 times.

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