CN113854533B - A method for preparing mogroside, mogrolic acid, fructus Siraitiae Grosvenorii concentrated juice and fructus Siraitiae Grosvenorii fructose from fresh fructus Siraitiae Grosvenorii - Google Patents

A method for preparing mogroside, mogrolic acid, fructus Siraitiae Grosvenorii concentrated juice and fructus Siraitiae Grosvenorii fructose from fresh fructus Siraitiae Grosvenorii Download PDF

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CN113854533B
CN113854533B CN202111157981.7A CN202111157981A CN113854533B CN 113854533 B CN113854533 B CN 113854533B CN 202111157981 A CN202111157981 A CN 202111157981A CN 113854533 B CN113854533 B CN 113854533B
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momordica grosvenori
mogroside
water
resin
liquid
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CN113854533A (en
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刘庚贵
黄华学
曾润清
何安乐
黄�俊
陈明明
廖智强
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Hunan Huacheng Biotech Inc
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30Artificial sweetening agents
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30Artificial sweetening agents
    • A23L27/33Artificial sweetening agents containing sugars or derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30Artificial sweetening agents
    • A23L27/33Artificial sweetening agents containing sugars or derivatives
    • A23L27/36Terpene glycosides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/30Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The invention relates to a method for preparing mogroside, mogrolic acid, momordica grosvenori concentrated juice and momordica grosvenori fructose from fresh momordica grosvenori. The invention skillfully utilizes the cooperation among the steps, simultaneously obtains the mogroside, the mogroside and the luo han guo concentrated juice by a continuous production mode which is convenient for industrialization and large scale, and can prepare the luo han fructose which has short sweetness duration, excellent taste, is clear and transparent after being dissolved in water by utilizing the obtained mogroside and luo han guo phenolic acid together with erythritol. The invention realizes the comprehensive utilization of the momordica grosvenori, forms a complete set of complete system of the extraction and separation of the bioactive components of the momordica grosvenori and the finish deep processing technology of the terminal application products, covers 2 main extract varieties and 1 type of terminal application varieties of the momordica grosvenori at the present stage, has high product yield and good quality, and has strong industrial practicability.

Description

A method for preparing mogroside, mogrolic acid, fructus Siraitiae Grosvenorii concentrated juice and fructus Siraitiae Grosvenorii fructose from fresh fructus Siraitiae Grosvenorii
Technical Field
The invention relates to the field of plant extraction and separation technology and food additives, in particular to a method for preparing mogrosides, mogrolic acid, momordica grosvenori concentrated juice and momordica grosvenori fructose from fresh momordica grosvenori.
Background
Fructus Siraitiae GrosvenoriiSiraitia grosvenorii(Swingle)C.Jeffrey) English name: fructus momordicae Cucurbitaceae (Cucurbitaceae)Fruits of perennial vine are praised as 'immortal fruits' by people, and are mainly produced in Guangxi Zhuang nationality Gui Linshi Yongfu county Longjiang county, baishou town, longsheng nationality, hunan province, huaihe, yongzhou, heng yang, shaoyang and other places. Momordica grosvenori is one of the first approved materials for both medicine and food, and has the main effects of moistening lung, relieving cough, promoting fluid production and resolving phlegm.
The seed-free fructus momordicae is obtained by planting triploid female plants and diploid male plants of fructus momordicae, artificial pollination of the triploid female plants with the diploid male plants during flowering, and fruiting of the female plants.
Lo Han Guo and seedless Lo Han Guo contain rich flavor and nutrients and triterpene saponin non-sugar sweet components.
Volatile oil component.
The fructus momordicae fruit contains 0.2% -0.3% of volatile oil, the volatile oil content is more than 20, 13 main components are identified from the volatile oil, and the total volatile oil content is 94.96%. Wherein n-hexadecanoic acid (45.609%) and 9, 12-octadecadienoic acid (36.151%) are main components, which account for 81.76% of the total amount of the volatile oil.
The volatile oil composition of the seedless fructus momordicae is similar to that of the fructus momordicae, but the content of the volatile oil is changed, and 24 components in the volatile oil are identified. Wherein, ethylene glycol isopropyl ether (27.21%), 1, 2-phthalic acid butyl-2-ethylhexyl ester (13.51%), diisobutyl phthalate (10.85%), geranial (10.22%), 3-decanoic acid (6.52%), butyl butyrate (4.99%), acetic acid-2-tridecyl ester (4.86%), which account for 78.16% of the total volatile oil.
(II) chemical composition.
Both the momordica grosvenori and the seedless momordica grosvenori contain cucurbitacin alkane type triterpene saponin, mainly comprising mogroside V, IV, 11-O-mogroside V, siamenoside and the like, and the fresh fruit content is 0.3-0.5%, wherein the mogroside V is a main sweet component, and has the advantages of no toxicity, low calorie, high sweetness and good thermal stability; reducing sugar such as glucose, fructose and sucrose, and the fresh fruit content is 9-14%; amino compounds such as protein, amino acid and the like, and the dry fruit content is 7.1% -7.8%; fatty acid, flavonoid compounds, vitamin C, 26 inorganic elements such as manganese, iron, nickel, selenium, tin, iodine, molybdenum and the like, trace elements and the like.
(III) non-sugar sweet components such as mogroside.
The fructus Siraitiae Grosvenorii fruit contains non-sugar sweet component, mainly triterpene saponin with mogrol as aglycone, and is represented by Mogroside (Mogroside) V, IV. Wherein the sweetness of the mogroside V is 256-344 times of that of the sucrose, and the sweetness of the mogroside IV is 126 times of that of the sucrose.
Further comprises D-mannitol (D-mannitol) with sweetness of 0.55-0.65 times that of sucrose.
Chinese name: mogroside V
English name: mogroside V CAS No.:88901-36-4 molecular formula: c (C) 60 H 102 O 29
The research on the momordica grosvenori in China is very much, and relates to germ plasm resources, seedling, planting, management and protection of the momordica grosvenori, chemical composition research, extraction and separation of main bioactive components such as triterpene saponin such as momordica grosvenori sweet glycoside, pharmacology and toxicology of the momordica grosvenori and the momordica grosvenori sweet glycoside, terminal application and the like; the comprehensive utilization of the momordica grosvenori is also studied to a certain extent, such as the production of momordica grosvenori concentrated juice (syrup) from the waste liquid discharged from the momordica grosvenori sweet glycoside adsorption resin, the production of momordica grosvenori flavone from the waste liquid discharged from the momordica grosvenori sweet glycoside decoloration resin, and the like, but the comprehensive utilization is determined according to the extraction and separation process of the momordica grosvenori sweet glycoside, and the comprehensive utilization is only reported to a certain extent as the recycling of the waste, and a complete extraction, separation and deep processing system is not formed yet. Because of different pretreatment of different extraction and separation process technologies, various process technologies such as flocculation, pH adjustment, membrane separation, adsorption resin refining, decoloration resin decoloration and the like are involved, the comprehensive utilization has a certain limitation, flocculation has larger loss on mogroside, the mogroside in flocculation precipitation is difficult to recycle in practice, and the technology needs to be further perfected. The prior art of extraction, separation and preparation technology of mogroside, momordica grosvenori concentrated juice (syrup), momordica grosvenori phenolic acid and momordica grosvenori fructose mainly relates to saccharification after-ripening, crushing, extraction, enzymolysis, flocculation, macroporous adsorption resin refining, ion resin decolorization, ultrafiltration and nanofiltration, organic solvent extraction, alumina chromatography, polyamide chromatography, silica gel chromatography, active carbon chromatography and other technologies of the momordica grosvenori, and the crushed momordica grosvenori is generally extracted at a higher temperature or percolating for a longer time.
The high-temperature extraction increases the dissolution of various components in the fructus momordicae, promotes the overcuring of pulp to form fine viscous sediment, promotes the dissolution of polysaccharide substances and the denaturation of protein substances which cause the hardening of adsorption resin and decoloration resin, and obviously causes the hardening, thereby leading the extracting solution to have a certain viscosity and viscous sediment, being difficult to remove by centrifugation, and being extremely easy to block ceramic membrane holes and difficult to clarify, thereby influencing the adsorption separation and decoloration effect of the resin; the high-temperature extraction also remarkably promotes Maillard reaction of reducing sugar and proteins in the fructus momordicae, thereby causing deepening of color and improving the decoloring difficulty. If the viscous substances are to be removed, enzymolysis, flocculation and other treatments are needed to promote the decomposition or coprecipitation of the components; to achieve good decolorizing results, a combination of decolorizing techniques such as decolorizing resins, polyamides, activated carbon, membrane separation, etc. are required. As previously described, such operations result in some loss of mogrosides, thereby directly increasing production costs.
At present, the aim of researching mogroside is to high-purity mogroside, and the high-purity technological process is accompanied with high-cost operations such as silica gel chromatography, high-speed countercurrent chromatography and the like, so that the product price is high, and the market acceptance is not facilitated; and the high purity product still has a more or less slightly bitter taste on entry for various reasons. The concentrated juice (syrup) of fructus momordicae mainly relates to the preparation from fresh fructus momordicae, or is prepared by recycling waste liquid, mainly uses decolorized concentrated juice, mainly focuses on indexes such as color, various component contents, light transmittance and the like, and has little research on removing pesticide residues in the concentrated juice (syrup) of fructus momordicae, plasticizers and other harmful substances in the preparation process. The study on the momordica grosvenori phenolic acid is less, mainly relates to momordica grosvenori flavone, momordica grosvenori flavine and the like, and the attention is lack to the momordica grosvenori phenolic acid substances which can be exchanged and adsorbed by the ion exchange resin. The momordica grosvenori fructose is simply prepared by using sweet fillers such as the momordica grosvenori glycoside and erythritol which are commercial finished products, and the preparation of the momordica grosvenori glycoside, particularly the preparation of the momordica grosvenori glycoside and the momordica grosvenori phenolic acid, and a series of comprehensive effects generated by the preparation of the momordica grosvenori glycoside and the momordica grosvenori phenolic acid are not involved.
For the reasons, the extraction, separation, fine and deep processing and high-value utilization of the momordica grosvenori are carried out, and the momordica grosvenori sweet glycoside, the momordica grosvenori concentrated juice (syrup), the momordica grosvenori phenolic acid and the momordica grosvenori fructose are considered as a whole to build a complete industrial chain system, so that a technical scheme is formed, and the mass production is realized, thereby promoting the development of the momordica grosvenori industry.
Pulsed Electric Field (PEF) is applied as a non-thermal processing technique for extraction, infusion, sterilization, etc. The pulsed electric field generates a magnetic field, and the pulsed electric field and the pulsed magnetic field alternately act to increase the permeability of the cell membrane, intensify oscillation and weaken the membrane strength, so that the membrane is destroyed, substances in the membrane easily flow out, substances outside the membrane easily permeate, and the protective effect of the cell membrane weakens or even disappears; the anions and cations generated by ionization of the substances near the electrodes act on the substances in the membrane, so that normal biochemical reactions and metabolic processes in the membrane are blocked, and meanwhile, the ionization of the liquid medium generates strong oxidization and can generate a series of chemical reactions with the substances in the cell to sterilize.
At present, no report of performing pretreatment on the momordica grosvenori crushed aggregates by utilizing a pulse electric field so as to realize short-time and high-efficiency extraction of the bioactive components of the momordica grosvenori at low temperature to normal temperature and obviously reduce Maillard reaction exists at home; no report of simultaneously extracting V50 pure flavor mogroside, luo han guo concentrated juice (syrup) and luo han guo phenolic acid from fresh luo han guo and preparing luo han fructose by using luo han guo glycoside and luo han guo phenolic acid is provided; the method is characterized in that the method does not comprise low-temperature or normal-temperature extraction firstly, does not adopt the technical means of enzymolysis, flocculation, pH adjustment and the like, uses the conditions of decoloring ion resin and forming alkaline solution, and the decolored solution is subjected to secondary adsorption and weak alkaline separation by adsorption resin, MCI resin selectively removes bitter saponins and adjusts the proportion of phenolic acid to prepare mogroside, and vegetable oil is used for extracting and removing plasticizer in the mogroside, and low-temperature microfiltration is used for removing sediment, so that the preparation of the mogroside with harmful substance residues meeting national standard, pure taste, white milk color, no sediment in 10% aqueous solution and mogroside V content of 49-62% is reported; the method has the advantages that no special resin for removing pesticide residues is adopted, the pesticide residues in the momordica grosvenori concentrated juice (syrup) are removed by combining the extraction of the vegetable oil, the plasticizer in the momordica grosvenori concentrated juice (syrup) is removed by combining the extraction of the vegetable oil and an ultrafiltration membrane with a certain cut-off molecular weight, and the normal-temperature sterilization of the momordica grosvenori concentrated juice (syrup) is realized by using a pulse electric field instead of the heat sterilization; the method has no report of extracting high-purity momordica phenolic acid from momordica grosvenori by using the combination of ion resin and adsorption resin and removing plasticizer by adopting vegetable oil extraction.
The prior art discloses the comprehensive utilization of momordica grosvenori, and the technical contents of extracting momordica grosvenori sweet glycoside, momordica grosvenori concentrated juice (syrup) and momordica grosvenori phenolic acid from momordica grosvenori, or extracting momordica grosvenori concentrated juice (syrup) and flavone from production waste liquid, and preparing momordica grosvenori fructose are as follows:
1. and (5) comprehensively utilizing the fructus momordicae.
CN201910089371.4 discloses an extraction and purification method for comprehensive utilization of dry fructus momordicae. The method comprises the following steps: s1, extracting the shell-broken dry momordica grosvenori with an ethanol water solution to obtain an extracting solution and pomace, and concentrating the extracting solution to an aqueous phase solution; s2, clarifying the aqueous phase solution to obtain a first filtrate and a first filter residue; s3, adding a precipitant into the first filtrate to obtain second filtrate, and passing the second filtrate through ceramic membrane equipment to obtain third filtrate; s4, injecting the third filtrate into a resin column, and allowing the effluent to pass through cation exchange resin and anion exchange resin to obtain the fructus momordicae high fructose syrup; s5, eluting the resin column with low-concentration ethanol, collecting eluent, and drying to obtain the momordica grosvenori brown pigment; s6, desorbing the eluted resin column by using high-concentration ethanol, concentrating the desorbed solution, and drying to obtain the mogroside V. The method realizes the comprehensive extraction and purification of the high fructose syrup, the brown pigment and the mogroside V from the dried momordica grosvenori.
The method is characterized in that the dried momordica grosvenori is comprehensively utilized, and the momordica grosvenori high fructose syrup, the momordica grosvenori brown pigment and the momordica grosvenori glycoside V are prepared at the same time, but no enterprise at home and abroad is available to prepare the momordica grosvenori high fructose syrup, the momordica grosvenori glycoside V and the momordica grosvenori brown pigment by taking the dried momordica grosvenori as raw materials, no transformation of the dried momordica grosvenori in the enterprise is seen, and the momordica grosvenori production enterprises all take fresh momordica grosvenori as raw materials. The dried momordica grosvenori is easy to store and transport, but the cost is at least more than 2 times of that of the fresh momordica grosvenori, and after long-time baking, serious Maillard reaction occurs, obvious medicinal taste and extremely dark color are generated, the taste is difficult to remove, and decolorization is not realized; the mogroside, the momordica grosvenori brown pigment and the momordica grosvenori concentrated juice (syrup) are water-soluble components, and the production cost is obviously increased by using aqueous alcohol, so that the production operation complexity is increased; the dried momordica grosvenori is extremely difficult to decolorize through full Maillard reaction, and the light-colored momordica grosvenori concentrated juice (syrup) can not be obtained through simple decolorization by using the adsorption resin and the anion-cation resin, so that the original juice and flavor of the momordica grosvenori concentrated juice (syrup) are lost; the adsorption resin adsorbs part of pigments which are only subjected to Maillard reaction, the pigments are obtained by the Maillard reaction, and most phenolic acid pigments of the fructus momordicae per se flow out together with part of the fructus momordicae glycoside V to cause the loss of the fructus momordicae glycoside V when the pigments are eluted by low-alcohol, so that the pigments are impure; the simple adsorption resin and gradient elution mode can not obtain more than 25% of mogroside V, only can obtain low-content and brown mogroside V, and is not a kind of mogroside on the market.
2. Extracting mogroside.
CN201811250821.5 discloses a method for producing high-content mogroside V, which takes momordica grosvenori subjected to instantaneous high-temperature heating treatment immediately after freezing as a raw material, and 1) pretreatment: immediately heating the raw material momordica grosvenori at a high temperature instantly after freezing, and immediately heating the raw material momordica grosvenori at 105-120 ℃ for 5-50 seconds after freezing the raw material momordica grosvenori at-25-10 ℃ for 1-2 hours; 2) Extracting: peeling pretreated fructus Siraitiae Grosvenorii, crushing pulp, and countercurrent extracting with water to obtain extractive solution; 3) And (3) filtering: centrifuging the extractive solution, filtering the supernatant with ceramic membrane to obtain filtrate; 4) Adsorption and analysis: adsorbing the filtrate with macroporous resin column, and resolving with ethanol solution to obtain resolving solution; 5) Decoloring: sequentially passing the analysis liquid through cation exchange resin and anion exchange resin, and collecting column passing liquid; 6) Concentrating and drying: concentrating and drying the column passing solution to obtain mogroside V; wherein the content of the mogroside V is more than or equal to 50 percent.
CN201510634737.3 discloses a method for improving purity of mogroside V in mogroside, which is prepared from fresh or dried fructus momordicae by 1) extracting, 2) preconcentrating, 3) enzymolysis, 4) primary filtering, 5) resin adsorption, eluting, 6) concentrating, secondary filtering, 7) resin column desalting, 8) resin column decolorizing, 9) further decolorizing with activated carbon, and 10) sterilizing and drying.
CN201410190403.7 discloses a method for extracting mogroside V, which uses fresh momordica grosvenori as raw material, and comprises the steps of cleaning, crushing, and extracting according to the following steps: 1) Saccharifying fresh fructus Siraitiae Grosvenorii; 2) Extracting with water and concentrating; 3) Sedimentation and centrifugation treatment; 4) Macroporous resin adsorption and separation, adopting a multi-resin column group to selectively adsorb, collecting analytic liquid in sections, and combining the analytic liquid in batches according to different contents; 5) Refining ion exchange resin; 6) Concentrating and recovering ethanol; 7) Refining silica gel; 8) Concentrating and spray drying to obtain the final product mogroside V extract.
CN201410192274.5 discloses a process for preparing mogroside V. The preparation method uses mature fresh fructus momordicae as a starting material, and comprises the steps of crushing, extracting, clarifying, removing impurities, filtering, adsorbing by macroporous adsorption resin, eluting, adsorbing by secondary ion exchange resin, concentrating, drying and refining by ethanol to obtain mogroside V.
The invention discloses a preparation method of high-purity mogroside V, which comprises the following steps: (1) Beating fresh fructus Siraitiae Grosvenorii into paste, adding deionized water, heating, high-shear extracting, filtering, extracting the residue again, mixing the filtrates, and concentrating under reduced pressure to obtain A; (2) Separating A with AB-8 type macroporous adsorbent resin column, eluting with alkaline water to colorless, eluting with deionized water to neutrality, eluting with ethanol solution, and concentrating the eluate under reduced pressure to obtain B; (3) Separating B with 001×16 strong acid styrene cation exchange resin column, eluting with acidic water, and concentrating the eluate under reduced pressure to obtain C; (4) Separating C with D941 weak base anion exchange resin column, eluting with water, concentrating the eluate under reduced pressure to obtain D, and spray drying to obtain mogroside V.
CN200910044558.9 discloses a method for producing momordica grosvenori extract with the content of mogroside V being more than 60%. The method comprises the steps of passing fresh fructus momordicae through: crushing, saccharification, water extraction, concentration, sedimentation and centrifugation, ion exchange resin refining, macroporous resin refining, concentration, alumina refining, concentration, spray drying and finished product preparation.
CN200710049737.2 discloses a milk white momordica grosvenori extract with mogroside V more than or equal to 40% and mogroside more than or equal to 98% and a preparation method thereof, which is prepared from fresh momordica grosvenori as a raw material through water extraction, concentration, enzymolysis, macroporous adsorption resin refining, ion exchange resin decolorization, concentration and spray drying.
The process route of extracting mogroside V by the method comprises the main process steps of clarifying the momordica grosvenori extracting solution, carrying out enzymolysis, refining by macroporous adsorption resin, decolorizing by ion resin, decolorizing by active carbon, refining by silica gel and the like to obtain the mogroside V with the purity of about 50 percent, and relates to biological enzymolysis, concentration before filtration, silica gel refining and the like, which is used for separating and purifying the mogroside V, and does not relate to preparation of momordica grosvenori concentrated juice (syrup) and momordica grosvenori phenolic acid, removal of components affecting taste and mouthfeel in the mogroside V, removal of harmful substances such as plasticizers in the mogroside V and post-precipitation treatment of product solution.
3. Extracting fructus Siraitiae Grosvenorii concentrated juice (syrup).
CN201710141754.2 discloses a process for producing a concentrated juice (syrup) of momordica grosvenori from a waste liquid discharged from a momordica grosvenori glycoside adsorption resin column, which comprises the steps of: adsorption resin feeding waste liquid in the production process of fresh momordica grosvenori, ceramic membrane microfiltration clarification, anion resin pH adjustment, reverse osmosis membrane concentration, decolorization resin decolorization, active carbon decolorization, plate and frame filtration, titanium rod fine filtration, reverse osmosis membrane concentration, low-temperature cooling, ceramic membrane microfiltration clarification, vacuum decompression concentration to prepare paste, sterilization, vacuum packaging and momordica grosvenori concentrated juice (syrup).
CN202011089686.8 discloses a preparation method of sugar-rich flavored momordica grosvenori concentrated juice (syrup), which comprises the following steps: the method comprises the steps of taking waste liquid generated in the process of preparing mogroside as a raw material, filtering the waste liquid, carrying out vacuum concentration, carrying out alcohol precipitation, recovering alcohol, decoloring resin, regulating pH value, and carrying out vacuum concentration to obtain the sugar-rich flavored momordica grosvenori concentrated juice (syrup).
CN201910820713.5 discloses a natural siraitia grosvenorii syrup without addition, which is prepared from the raw materials of adsorption resin wastewater in the production process of fresh siraitia grosvenorii, and specifically comprises the following components: 14-24% of glucose, 16-24% of fructose, 1-14% of sucrose, 1-8% of mannitol, 40-50% of water and the balance of less than or equal to 2% of components, wherein the siraitia grosvenorii syrup is obtained by steps of refining, decoloring, deacidifying, removing pesticide residues and heavy metals from waste liquid of adsorption resin in the production process of fresh siraitia grosvenorii, concentrating and the like, and has no other additives except siraitia grosvenorii, seedless siraitia grosvenorii and water.
CN201710277285.7 discloses a process for preparing decolored concentrated juice of fresh momordica grosvenori from fresh and mature momordica grosvenori, which comprises the following steps: fresh fructus Siraitiae Grosvenorii, saccharification, fruit selection and washing, crushing, percolation extraction, disc centrifugation, microfiltration and clarification by a 0.45 mu m ceramic membrane, ultrafiltration and separation of molecular weight, decolorization by polyamide resin, decolorization by decolorizing resin, pH adjustment by cation resin, concentration by reverse osmosis membrane, residue removal by a granular activated carbon column, microfiltration and clarification by a 0.22 mu m ceramic membrane, ointment preparation by vacuum decompression and concentration, sterilization, vacuum packaging and decolorization of fresh fructus Siraitiae Grosvenorii.
The method relates to preparation of the momordica grosvenori concentrated juice (syrup) from fresh momordica grosvenori or momordica grosvenori sweet glycoside production waste liquid, mainly relates to decolorization, clarification, pH, pesticide residue removal, heavy metal removal and the like of the momordica grosvenori concentrated juice (syrup), and mainly aims at preparing the decolorized concentrated juice, not simultaneously preparing the momordica grosvenori sweet glycoside and the momordica grosvenori phenolic acid, and not removing plasticizer residues and the like in the momordica grosvenori concentrated juice (syrup).
4. Preparing the momordica grosvenori fructose.
CN201710035875.9 discloses a method for preparing healthy momordica grosvenori fructose with double or multiple sugar, which comprises the following steps: (1) Respectively weighing mogroside V and erythritol, wherein the weight ratio of the mogroside V to the erythritol is (8-40) (1000-5000); (2) Heating and mixing erythritol to 30-35 ℃ to obtain slightly hot erythritol; (3) Dissolving mogroside V in edible alcohol with the mass concentration of 98% which is 2-3 times of that of the mogroside V to obtain a mogroside V solution, uniformly spraying the mogroside V solution on the slightly hot erythritol obtained in the step (2), and then continuously mixing for 15-25min to obtain a crude product of the mogroside; and (4) drying the crude product of the momordica grosvenori obtained in the step (3).
CN200410022754.3 discloses a low-calorie siraitia grosvenorii fruit, the invention also discloses a method for producing the low-calorie siraitia grosvenorii fruit, which comprises the following steps: selecting fruits, crushing, extracting with water, filtering, adsorbing, eluting, concentrating, drying, mixing, clathrating, recrystallizing and drying to obtain the finished product.
The method relates to the preparation of momordica grosvenori fructose, wherein the momordica grosvenori extract obtained by refining mogroside or momordica grosvenori through adsorption resin is compounded with erythritol, and the preparation of V50 pure-taste mogroside and momordica grosvenori phenolic acid and the compounding of the V50 pure-taste mogroside and the momordica grosvenori phenolic acid with sugar alcohol sweet filling agents are not involved, and the fluidized bed granulation technology is not involved.
5. Application of pulsed electric field in plant extraction.
CN201810373260.1 discloses a method for extracting plant polyphenol by combining pulsed electric field-double water phase-column chromatography, which comprises the following steps: (1) pretreating plants to be extracted to obtain raw material liquid; (2) Ethanol is used as a solvent, and active substances in the raw material liquid are extracted by using a pulse electric field to obtain an extracting solution; (3) Filtering the extracting solution, and extracting active ingredients in the extracting solution by adopting a double aqueous phase to obtain a crude extracting solution of plant polyphenol; (4) Purifying active substances in the extract by column chromatography after removing alcohol by rotary evaporation of the crude extract of plant polyphenol; and (5) concentrating and drying to obtain the plant polyphenol product.
The invention discloses a method for extracting grape skin residue polyphenol by using an ultrasonic synergistic pulse electric field, which comprises the following steps: placing grape skin residue to be treated and an ethanol water solution in a treatment chamber between two electrodes of a pulse electric field, inserting an ultrasonic probe into the grape skin residue ethanol water solution, and simultaneously starting ultrasonic waves and the pulse electric field for extraction; the mass ratio of the grape skin residue to the ethanol water solution is 1:2. The invention adopts ultrasonic cooperated with pulse electric field to extract grape skin residue polyphenol, and utilizes cavitation effect and secondary effect generated by ultrasonic wave, under the same operation condition, the extraction rate is obviously improved compared with the pure pulse electric field or the ultrasonic field. The invention has simple extraction process and easy operation, and can achieve better extraction effect in a short time.
The method uses a single pulse electric field or the cooperation of ultrasonic waves to extract polyphenol, but uses ethanol water solution as an extraction solvent, and ethanol has extremely strong penetrability to plant cells without pulse electric field treatment, and the two contradicts each other, so that resource waste and cost increase are caused; polyphenols are water-soluble substances, and the ethanol extraction method is not suitable for industrial scale production from the comprehensive aspects of production cost and production operation. Therefore, the pulsed electric field is applied to extracting plant polyphenol, practical consideration needs to be combined with production, and no pulsed electric field pretreatment technology is applied to extracting and separating bioactive components of the momordica grosvenori at present.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects, and provides a method for fully utilizing fresh momordica grosvenori, and a method for simultaneously preparing mogroside, momordica grosvenori concentrated juice (syrup) and momordica grosvenori fructose: the method is characterized in that fresh momordica grosvenori is used as a raw material, a traditional high-temperature extraction or long-time percolation extraction mode is changed, and a pulse electric field is used for carrying out pretreatment on momordica grosvenori crushed aggregates, so that short-time and high-efficiency extraction of the bioactive components of the momordica grosvenori from low temperature to normal temperature is realized, the Maillard reaction degree is reduced, the yield of effective components such as mogroside and the like is improved, and the decolorization effect of the mogroside and the momordica grosvenori concentrated juice (syrup) is obviously improved; realizing the comprehensive utilization of fresh fructus momordicae, simultaneously preparing V50 pure flavor mogroside, fructus momordicae concentrated juice (syrup) and mogrolic acid, and preparing the fructus momordicae fructose by using the mogroside, the mogrolic acid and the erythritol; removing harmful substances such as pesticide residues, plasticizers and the like in the 3 products, and solving the problem of post-product precipitation; the high-quality mogroside, the mogroside concentrated juice (syrup) and the mogrolic acid are prepared by using the combined technology of ion resin, adsorption resin, special resin, MCI resin and vegetable oil extraction, and the technology is applied to mass production, so that the bioactive components of the momordica grosvenori are simultaneously extracted, separated and finely processed, and industrialization is realized.
The technical scheme adopted for solving the technical problems is as follows: a method for preparing mogroside, mogrolic acid and fructus Siraitiae Grosvenorii concentrated juice from fresh fructus Siraitiae Grosvenorii comprises the following steps:
(S1) crushing fresh momordica grosvenori, immersing the crushed momordica grosvenori in water, treating the crushed momordica grosvenori under the condition of a pulse electric field, extracting the momordica grosvenori under the condition of low temperature by continuous countercurrent extraction or extraction tank extraction, filtering, loading the obtained product on an alkaline anion resin column, washing the obtained product after the whole raw material is fed, collecting a washing liquid 1, and combining a feeding effluent and the washing liquid 1; desorbing with alcohol solution containing water and acid, eluting with water, collecting water washing solution 2, and mixing the desorption solution and the water washing solution 2;
the water in the step (S1) is added in an amount capable of immersing the surface of crushed aggregates, and in one specific embodiment of the invention, the volume of water is 0.8-1.2 times (L/kg) of the weight of the fresh fructus momordicae.
In the step (S1), the crushing into the broken shell without breaking the seeds breaks the shell of the momordica grosvenori, but maintains the integrity of the seeds, and the taste and the mouthfeel of the mogroside and the momordica grosvenori concentrated juice (syrup) are affected because the seeds have a certain bitter taste and contain oil.
In the step (S1), the strength of the pre-treatment pulse electric field is 0.5-2.0 kv/cm, the times are 10-30, and the treatment degree is that the pulp tissue structure of the crushed momordica grosvenori is loose. The pulsed electric field treatment damages the tissue cell structure of pulp, greatly promotes the dissolution of bioactive substances such as mogroside which is easy to dissolve in water, reduces the dissolution of impurities such as polysaccharide, improves the extraction efficiency and shortens the extraction time.
In the step (S1), the low temperature is 10-20 ℃, and the too low temperature is not beneficial to the concentration diffusion of effective components such as mogroside and the like in the extracting solution, so that the extracting efficiency is reduced; when the temperature is too high, the pulp of the momordica grosvenori can be cured to generate fine viscous precipitate, the filtering clarification and the resin separation effect are affected, and serious Maillard reaction is caused to lead the product to be difficult to decolorize.
In step (S1), the process of continuous countercurrent extraction is well known in the art. In one embodiment of the invention, the continuous countercurrent extraction process results in two sections of extraction tanks; the time is 2.0h to 3.0h; adding 1.5-3.0 times of water (water volume/fresh fructus momordicae, V/W); squeezing and filtering after extraction, and collecting the extract. Extracting in a conventional extracting tank: starting stirring or compressed air recoil; extracting for 3 times; the time is 1-2.0h, 0.5-1.5h and 0.5-1h respectively; the water adding amount of each time is 2-4 times of the fresh fructus momordicae (the water volume/the fresh fructus momordicae mass, V/W); combining the first 2 times of extracting solutions, and carrying out the 3 rd time of extraction.
In the step (S1), the filtering is a combination of disc centrifugation and ceramic membrane clarification, wherein pulp scraps and other sediments are separated by disc centrifugation, and then the ceramic membrane clarification is performed; the ceramic membrane is made of aluminum oxide or zirconium oxide, and the aperture is 100-400 nm.
In the step (S1), the basic anion resin includes gel-type and macroporous acrylic weak base anion resin, acrylic strong base and weak base anion resin, gel-type and macroporous styrene strong base anion resin, macroporous acrylic strong base anion resin, macroporous styrene weak base anion resin, preferably model: d900, D941, D316, D296, D280. The resin has good exchange adsorption effect on phenolic acid substances in the momordica grosvenori, and has no adsorption on reducing sugars such as mogroside, fructose and the like. The amount of the alkaline anionic resin is 7-20wt% of the fresh fructus momordicae. The height-diameter ratio of the alkaline anion resin is 4-8:1, the feeding flow rate is 0.6-1.5BV/h, the water washing flow rate is 1.0-2.0BV/h, and the pH of the water washing effluent is 7.5-8.5.
In the step (S1), the alcohol solution containing water and acid is an alcohol water solution with the alcohol concentration of 50-75wt% and the inorganic acid concentration of 0.3-1wt%, and the alcohol is at least one of methanol, ethanol and propanol, preferably ethanol. The amount of the aqueous and acid alcohol solution is 1.5-3 times of the weight of the anionic resin. The momordica grosvenori phenolic acid which is exchanged and adsorbed on the ion resin can be completely eluted by adjusting the desorption process parameters, and phenolic acid substances are in a free state through dilute acid, so that the stability of the phenolic acid is improved.
(S2) combining alkaline anion resin feed effluent and water washing liquid 1, loading the mixture on a macroporous adsorption resin column, washing until the effluent is clear, transparent and colorless, desorbing the effluent with aqueous alcohol 1, washing the mixture with water, collecting desorption liquid and water washing liquid, concentrating the mixture, loading the mixture on an MCI column, collecting MCI column feed effluent, desorbing the mixture with aqueous alcohol 2, eluting the mixture with water, combining the desorption liquid and the water washing liquid, concentrating the mixture, combining the mixture with MCI column feed effluent to obtain MCI column refined liquid, concentrating the mixture, adding edible vegetable oil, stirring the mixture under heating, carrying out countercurrent extraction, standing and layering, collecting water phase, refrigerating the water phase, filtering the water phase, concentrating the water phase, and spray-drying the water phase to obtain V50 mogroside;
in the step (S2), the macroporous adsorption resin is of a nonpolar D101, LX-100B, LX-T28, LX-T81, a weak polar AB-8 or any combination thereof. The resin has good adsorption effect on saponin substances such as mogroside and the like, and has no adsorption on reducing sugar such as fructose and the like. The dosage of the macroporous adsorption resin is 25-60% of the weight of the fresh fructus momordicae. The volume usage of the aqueous alcohol 1 is 1.5-3 times (V/W) of the mass of the macroporous adsorption resin, and the volume usage of the water washing water after the desorption of the aqueous alcohol 1 is 0.7-1.5 times (V/W) of the mass of the macroporous adsorption resin.
In the step (S2), the MCI column filler is a polystyrene-based reverse phase GEL filler CHP20P 75-150 um series, the specification model is one or any combination of polystyrene-based GEL CHP20 SS, GEL CHP 2MG and methacrylate-based GEL CHP 2MG, and the collecting part is the sum of column inlet effluent, 35-50% aqueous alcoholysis liquid and water washing liquid. Because the bittering saponin in the momordica grosvenori, namely the mogroside IIE and the mogroside III, and the main sweet components in the mogroside, such as mogroside IV, mogroside V, 11-O-mogroside V, siamenoside I molecular structure and coordination glycosyl difference, the resin of the MCI column filler has good adsorption effect on bitter substances in the mogroside, particularly on some saponins with bitter taste, and has smaller adsorption on the mogroside, and bitter and astringent components can be further removed on the basis of refining, desalting and debitterizing of the early-stage adsorption resin, so that the taste and mouthfeel of the mogroside are obviously improved. The mass dosage of the MCI resin is 15-30 times of the mass of solid matters in the macroporous adsorption resin desorption liquid and the water washing liquid. The volume usage of the aqueous alcohol 2 is 1-2.5 times (V/W) of the mass of the MCI resin, and the volume usage of the water washing water after the desorption of the aqueous alcohol 2 is 0.5-1.5 times (V/W) of the mass of the MCI resin.
In the step (S2), the alcohol concentration of the aqueous alcohol 1 is 50-70 wt%, the alcohol concentration of the aqueous alcohol 2 is 35-50wt%, and the alcohol is at least one of methanol, ethanol and propanol. The alcohol concentration of the aqueous alcohol 2 cannot be higher than that of the aqueous alcohol 1 because the adsorption and desorption properties and the use purposes of the macroporous adsorption resin and the MCI resin are different, the MIC column aims at adsorbing bitter substances affecting the mouthfeel of the product, and if the concentration of the aqueous alcohol 2 is higher, part of the bitter substances can be eluted together, so that the mouthfeel and the taste of the product are poor.
In the step (S2), the MCI column refined liquid is concentrated to have the solid content of 8-15%, the consumption of the edible vegetable oil is 0.7-1.5 times of the volume of the concentrated MCI column refined liquid, and the heating temperature is 60-75 ℃. Under the temperature and the operation condition, the vegetable oil has good solubility for pesticide residues and plasticizer oil-soluble components, while the reducing sugar such as mogroside, fructose and the like is insoluble, and the water phase and the oil phase are kept stand for layering, so that the pesticide residues, plasticizers and other harmful substances are obviously removed.
In the step (S2), the refrigeration is carried out at the temperature of 1-5 ℃, and under the refrigeration temperature condition, on one hand, the solid content of the step of extraction and plasticization before direct connection is carried out, and on the other hand, the method is favorable for fully separating out the post-precipitation in the mogroside. The concentration is carried out after filtration until the solid content is 20-30%, and the spray drying process conditions are that the inlet air temperature is 160-190 ℃ and the outlet air temperature is 75-90 ℃.
(S3) collecting the macroporous adsorption resin feed effluent and the initial water washing liquid in the step (S2), loading the macroporous adsorption resin feed effluent and the initial water washing liquid on a cation resin column, collecting the feed effluent, feeding purified water after feeding, washing with water, combining the cation resin column feed effluent and 0-2 BV water washing liquid, concentrating to obtain desalted liquid, loading the desalted liquid into a special resin column for pesticide residue removal, washing with water, combining the effluent and the water washing liquid, concentrating for the first time, adding edible vegetable oil, heating and stirring, countercurrent extracting, standing and layering, collecting water phase, feeding the water phase into an organic film complete equipment with the molecular weight of 2 KD-3 KD, concentrating for the second time, filtering, concentrating for the third time, refrigerating, filtering again, concentrating to a proper sugar degree, and obtaining concentrated liquid;
in the step (S3), after the initial washing liquid is fed, purified water is fed again, and the washing liquid within 1-2BV is collected; the cationic resins include gel-type and macroporous styrene strong acid cationic resins, acrylic gel-type and macroporous weak acid cationic resins, preferably model: 001 x 16, D717. The mass of the cationic resin is 0.4-1.0 times of that of the alkaline anionic resin in the step (S1).
In the step (S3), the special pesticide residue removing resin includes gel-type and macroporous acrylic resin, gel-type and macroporous styrene resin, macroporous acrylic resin, macroporous styrene resin, acrylic gel-type resin, preferably model: LSA-900B, LSA-900D. The resin has remarkable adsorption effect on trace pesticide residues, and has no adsorption on reducing sugars such as fructose. The mass of the special resin for pesticide residue removal is 0.2-1.0 times of that of the cationic resin in the step (S3).
In the step (S3), the first concentration is to concentrate until the solid content is 9-12%; the second concentration is concentration until the solid content is 4-10%; and the third concentration is to concentrate to the solid content of 12-20%. The substances which generate turbidity and post-precipitation in the momordica grosvenori concentrated juice (syrup) can be completely removed by two-step filtration and clarification, the operation of reducing the yield of the momordica grosvenori sweet glycoside, such as enzymolysis, flocculation and the like, is not needed in the whole process, and the problem of post-precipitation of the momordica grosvenori concentrated juice (syrup) is completely solved by only physical separation.
In the step (S3), the addition amount of the edible vegetable oil is 0.4-1.5 times of the volume of the pesticide-removed residual liquid obtained by the first concentration, and the heating temperature is 60-75 ℃ after the edible vegetable oil is added.
In the step (S3), the temperature is 1-5 ℃ to fully separate out the precipitate.
In the step (S3), the concentration is performed to a proper sugar degree, that is, to 50-70 brix, and the concentrated solution may be sterilized after the concentration, for example, by pulsed electric field sterilization or high temperature sterilization. Preferably, the sterilization is performed by a pulsed electric field, the strength of the pulsed electric field is 30-50 kv/cm, and the times are 400-600. The process realizes normal temperature high-efficiency sterilization of the fructus momordicae concentrated juice (syrup) in a non-heat treatment mode, and avoids Maillard reaction of the concentrated juice due to heating and influence on color.
The sugar degree of the fructus momordicae concentrated juice (syrup) obtained in the step (S3) is 60-70 Brix, and the fructus momordicae concentrated juice mainly comprises the following components: 15-25% of fructose, 15-25% of glucose, 5-12% of sucrose and 38-52% of total amount of monosaccharide and disaccharide. Main officer experience index: 1. taste and mouthfeel: the honey has mellow taste similar to honey, is extremely sweet and is pleasant to enter; 2. smell: has honey fragrance and characteristic fruit fragrance of fructus Siraitiae Grosvenorii; 3. color: pale yellow to yellow, clear, transparent, and free of turbidity and precipitation.
(S4) combining the anion resin desorption liquid and the water washing liquid 2 in the step (S1), concentrating, adding a phenolic acid special-purpose adsorption resin, washing with water, desorbing with aqueous alcohol 3, concentrating the desorption liquid, adding edible vegetable oil, heating and stirring, countercurrent extracting, standing for layering, collecting a water phase, filtering, concentrating, and spray-drying to obtain the momordica grosvenori phenolic acid;
in the step (S4), the special resin is phenolic acid adsorption special resin, has specific and selective adsorption on momordica grosvenori phenolic acid, and has a specification type of one or any combination of nonpolar styrene material LXD-200, polar polyamide material LX-8, acrylic acid material LX-17 and styrene brominated resin LX-207. The resin special for preparing high-purity phenolic acid has strong selective adsorptivity, and compared with broad-spectrum resin, the phenolic acid content is improved by more than 30%.
In the step (S4), the combined solution of the anion resin desorption liquid and the water washing liquid 2 is concentrated until no alcohol smell exists, the concentration of the desorption liquid is concentrated until the solid content is 9-12%, and the concentration before spray drying is concentrated until the solid content is 20-30%.
In the step (S4), the volume addition amount of the edible vegetable oil is 0.4-1.5 times of the desorption liquid after concentration, the heating temperature is 60-75 ℃,
in the steps (S2) to (S4), the filtering is carried out by arranging ceramic membranes in a whole set, wherein the ceramic membranes are made of alumina or zirconia, and the pore diameter is 100-400nm.
In a preferred technical scheme of the invention, the method further comprises the step of preparing the momordica grosvenori fructose (S5):
(S5A) preparing original momordica grosvenori fructose:
taking mogroside V50 in the step (S2) and mogroside acid in the step (S4) according to a proportion, adding water for dissolution, taking erythritol as an adhesive, putting the erythritol into a fluidized bed, uniformly spraying the adhesive, and drying to obtain the original momordica grosvenori fructose;
and/or (S5B) preparing momordica grosvenori zero-calorie sugar:
taking the mogroside V50 in the step (S2) according to a proportion, adding water for dissolution, taking the mogroside V as an adhesive, putting erythritol into a fluidized bed, uniformly spraying the adhesive, and drying to obtain the momordica grosvenori zero-calorie sugar.
Preferably, in the step (S5A), the mass ratio of mogroside V50 to mogroside V phenolic acid is 1: 0.5-15. Preferably 1:6-12.
Preferably, in the step (S5), the momordica grosvenori is prepared by a fluidized bed granulation method, and the solid content of the binder is 5-20%; the addition amount of erythritol is 2-250 times of the total weight of V50 mogroside or V50 mogroside and mogroside.
The sweetness of the erythritol is 60-70% of that of sucrose, and the adding amount of the erythritol depends on the sweetness of the required obtained momordica grosvenori sweetener. When high-intensity sweetener is desired, erythritol is added in a low amount, such as 2 times that of V50 mogrosides; if it is desired to obtain Lo Han Guo sugar substitutes having sweetness close to that of sucrose, the erythritol is added in a high amount, such as 250 times that of V50 mogroside.
The inventor discovers that the original flavor momordica grosvenori fructose prepared from the momordica grosvenori glycoside V50 and the momordica grosvenori phenolic acid, which are obtained by the method, has improved taste, no bitter and astringent taste in the mouth, shortened post-sweetness time, and sweetness duration of about 15 seconds, and is more similar to that of sucrose.
The invention provides a method for preparing mogroside, momordica grosvenori concentrated juice (syrup) and momordica grosvenori fructose from fresh momordica grosvenori, which takes fresh and mature momordica grosvenori as a raw material, breaks the shell of the raw material under the condition of keeping the seeds intact, and avoids dissolving out bitter substances and grease which have influence on the taste and the mouthfeel of the momordica grosvenori glucoside and the momordica grosvenori concentrated juice (syrup). Proper amount of water is added to fully spread the crushed fruit, the permeability of the pulp cell membrane is increased, the vibration is aggravated, the membrane strength is weakened, the reducing sugar such as mogroside, fructose and the like in the membrane easily flows out, the phenolic acid substances outside the membrane easily permeate, and the protective effect of the cell membrane is weakened or even disappears. After pretreatment is completed, the dynamic extraction mode is adopted from low temperature to normal temperature, so that the transfer of mogroside, fructose and other reducing sugar and mogrolic acid in the cell membrane of the Siraitia grosvenorii pulp to a solution system is further promoted, and the maximum concentration gradient difference is formed, thereby realizing short-time and high-efficiency extraction, greatly reducing the dissolution of substances such as polysaccharide and the like, avoiding viscous precipitation caused by overcuring the pulp, obviously reducing the Maillard reaction degree, and being beneficial to product refining and decolorization. The low-temperature extracted momordica grosvenori extracting solution is not sticky and has no obvious sticky sediment, clear and transparent feed liquid can be obtained through disc centrifugation and simple operation of a ceramic membrane, and the resin separation and purification effect is obviously improved.
The anion exchange resin with a certain specification and model has larger exchange capacity, has selective exchange adsorption effect on the mogroside, and has no adsorption effect on the mogroside, fructose, glucose, sucrose and other reducing sugars, so that substances which are not adsorbed by the resin are washed out of the resin column through the anion exchange resin by purification and water washing, thereby realizing the separation of the mogroside from the luo han guo sweet glycoside and the luo han guo concentrated juice (syrup) rich in fructose and other reducing sugars.
The effluent of the ion resin column contains the mogroside, glucose, fructose, sucrose and other reducing sugar, and the macroporous adsorption resin with certain specification has good adsorption to the mogroside and no adsorption to the fructose and other reducing sugar, so that substances which are not adsorbed by the resin are washed out of the resin column through the macroporous adsorption resin by purification and water washing, and the separation of the mogroside and the luo han guo concentrated juice (syrup) rich in the fructose and other reducing sugar is realized. Because the ion resin effluent is alkaline, when the ion resin effluent is separated by macroporous adsorption resin, triterpene saponin neutral substance-mogroside is fully adsorbed, and partial pigment and other impurities which permeate the ion resin are not adsorbed in an ion form and flow out under alkaline conditions, thereby realizing the refining and full decolorization of the mogroside by combining anion exchange resin and macroporous adsorption resin. The macroporous adsorption resin is fully washed until effluent liquid is clear and transparent, and substances which are not adsorbed by the resin can be basically and completely washed out, so that the desalting of mogroside is realized, and the taste and mouthfeel of the mogroside are obviously improved. The MCI resin has specific and selective adsorption to bitter components in the mogrosides, has smaller adsorption to the mogrosides, and can obtain the mogrosides with pure taste by collecting effluent liquid and alcohol hydrolysis liquid absorption with certain concentration. Pesticide is applied to the momordica grosvenori in the planting process, pesticide residues and plasticizer residues exist in the process of extracting and separating mogroside by using ion exchange resin and macroporous adsorption resin, and the two harmful substance residues are fat-soluble, namely oil-soluble, can be completely dissolved by hot vegetable oil, are not mutually soluble, and can be removed by layering. Although the mogroside is purified by resin, trace impurities sometimes exist to cause post-precipitation of high-concentration aqueous solution, so that the high-quality V50 pure-taste mogroside can be prepared by concentrating the mogroside to a certain concentration and then clarifying the concentrated product by a ceramic membrane.
The two-stage separation and purification of the ion exchange resin and the macroporous adsorption resin lead the reducing sugar such as glucose, fructose, sucrose and the like to flow out along with the feeding effluent liquid of the macroporous adsorption resin and the water washing column liquid, and as mentioned before, the effluent liquid after the ion exchange resin is used for separating the momordica grosvenori phenolic acid is alkalescent and contains impurities such as ionic salt and the like, thereby not only affecting the taste and the taste of the momordica grosvenori concentrated juice (syrup), but also affecting the stability and the clarity of the solution. The cation exchange resin can exchange and adsorb ionic salts generated by the anion exchange resin, and can adjust the pH of effluent liquid to restore the original balance of the solution, so that the solution can be reduced by the cation exchange resin. The concentrated juice (syrup) of fructus momordicae still has pesticide residue, plasticizer and other residues, and has certain viscosity due to higher sugar degree of the concentrated juice, so the concentrated juice can be extracted and combined with vegetable oil to remove pesticide residue through special resin for removing pesticide residue at a certain concentration. The plasticizer is a substance with benzene ring, has larger steric hindrance and is intercepted by an ultrafiltration membrane with certain molecular weight, and reducing sugar such as fructose can pass through, so that plasticizer residue is further removed by membrane separation on the basis of extracting pesticide residue and plasticizer from vegetable oil. Since some substances which are accompanied by reducing sugars such as fructose and which are precipitated and post-precipitated are not likely to be precipitated at normal temperature and low concentration, the post-precipitated substances can be completely removed by clarifying the ceramic membrane at different solid contents and temperatures by fractional precipitation. In the past, the sterilization of the momordica grosvenori concentrated juice (syrup) is mainly heat sterilization, and the color of the concentrated juice is deepened due to Maillard reaction, so that deep decolorization is needed before sterilization and protein and amino acid substances are removed as much as possible, but the pulse electric field sterilization is used as a non-heat treatment technology, so that the high-efficiency sterilization at normal temperature can be realized, and the color of the momordica grosvenori concentrated juice (syrup) is hardly changed, and therefore, the high-quality momordica grosvenori concentrated juice (syrup) with extremely light color can be obtained by combining the prior decolorization of ion exchange resin through the pulse electric field sterilization technology.
The momordica grosvenori phenolic acid is subjected to exchange adsorption in the anion exchange resin step to be separated from reducing sugar such as mogroside, fructose and the like, the enrichment of the momordica grosvenori phenolic acid can be realized by washing an ion resin column and desorbing the ion resin column by using aqueous alcohol, and a proper amount of acid is added into the aqueous alcohol before the desorption, so that the momordica grosvenori phenolic acid is favorably converted into a free state in time, and the stability is improved. The phenolic acid special adsorption resin has specific and selective adsorption to the momordica grosvenori phenolic acid, and little adsorption to other substances, and the high-purity momordica grosvenori phenolic acid can be prepared by combining the anion exchange resin and the phenolic acid special resin. Harmful substances such as pesticide residues, plasticizers and the like are removed through hot extraction of vegetable oil, and high-quality mogrolic acid can be prepared through clarifying and removing solution after precipitation of ceramic membranes with certain concentration.
The sweetness of the mogroside is 256-344 times that of the sucrose, and the mogroside is too high to be directly used; the momordica grosvenori phenolic acid has various biological activities and is a main substance of the biological activity of the momordica grosvenori; erythritol is an excellent sweetener filler that can dilute the sweetness of mogrosides. The mogroside prepared by the application can be used as the representation of the sweetness and the bioactivity of the momordica grosvenori together with the momordica grosvenori phenolic acid, and can be compounded with erythritol to prepare the original momordica grosvenori fructose which has the taste, the sweetness multiple and the sweetness duration equivalent to those of sucrose and has the bioactivity of the momordica grosvenori; the mogroside prepared by the application can be compounded with erythritol, and can be used for preparing the momordica grosvenori zero-calorie candy with taste and multiple sweetness and the sweetness duration being equivalent to that of sucrose.
The application has the beneficial effects that:
(1) The application provides a method for preparing mogroside, momordica grosvenori concentrated juice (syrup), momordica grosvenori phenolic acid and momordica grosvenori fructose from fresh momordica grosvenori. Fresh mature fructus momordicae is taken as a raw material, and V50 pure flavor mogroside is prepared through the steps of pulse electric field pretreatment, low-temperature extraction, filtration clarification, anion resin separation, ion resin effluent liquid purification by adsorption resin, MCI column chromatography, vegetable oil extraction and plasticizer removal, low-temperature clarification and the like; desalting the effluent of the adsorption resin, removing pesticide residues by the resin, extracting, separating the plasticizer by a membrane, clarifying step by step, sterilizing by a pulse electric field and the like to prepare the fructus momordicae concentrated juice (syrup); refining the ion resin desorption liquid by using phenolic acid special resin, extracting to remove plasticizer, clarifying and the like to prepare the momordica grosvenori phenolic acid. And finally, respectively compounding mogroside and mogroside or mogroside and erythritol to prepare the momordica grosvenori fructose. The application realizes the comprehensive utilization of the momordica grosvenori, forms a complete set of complete momordica grosvenori bioactive component extraction and separation and finish deep processing technology system of terminal application products, covers 2 main extract varieties and 1 type of terminal application varieties of the momordica grosvenori at the present stage, and has industrial practicability.
(2) The application provides a momordica grosvenori sweet glycoside, a momordica grosvenori concentrated juice (syrup), momordica grosvenori phenolic acid and momordica grosvenori fructose. The mogroside is pure-taste mogroside, wherein the content of mogroside V is 45-62%, the content of white powder is similar to that of white powder, pesticide residues and plasticizer residues meet national standards, and the 10% aqueous solution is clear, transparent, free of turbidity and precipitation, and free of slight bitter taste. The sugar degree of the fructus momordicae concentrated juice (syrup) is 60-70 Brix, the fructose is 15-25%, the glucose is 15-25%, the sucrose is 5-12%, and the total amount of monosaccharide and disaccharide is 38-52%. The content of phenolic acid in the momordica grosvenori phenolic acid is 80-90%. The momordica grosvenori comprises primary momordica grosvenori and momordica grosvenori zero calorie sugar, the sweet duration is less than or equal to 15 seconds, the content of mogroside V is 0.1-3.0%, and the content of erythritol is 70.0-99.9%.
(3) The application applies the pulsed electric field technology to the extraction, separation and deep processing of the momordica grosvenori. The method for efficiently extracting the bioactive components of the momordica grosvenori at normal temperature to low temperature is provided, namely, the crushed momordica grosvenori is subjected to pretreatment by a pulse electric field, the cell structure is destroyed, the dissolution of bioactive components such as the mogroside and the like is promoted, the Maillard reaction of reducing sugar such as fructose and the like in the momordica grosvenori and amino substances such as protein and the like is obviously reduced, the mogroside and the momordica grosvenori concentrated juice (syrup) are easy to decolorize, complex decolorization steps and procedures are not needed, and the product yield is further improved. The method uses the pulse electric field to sterilize the momordica grosvenori concentrated juice (syrup), avoids Maillard reaction of the concentrated juice under the heated condition, maintains the flavor and the nutrition components of the concentrated juice on the premise of keeping light color, and combines the decoloring technology of the application to obtain the high-quality momordica grosvenori decolored concentrated juice by a simple method.
(4) The invention provides a new momordica grosvenori extract variety-momordica grosvenori phenolic acid. The momordica grosvenori phenolic acid is used as a representative of the bioactive components of the momordica grosvenori, has the original bioactivity of the momordica grosvenori, can be matched with mogroside to prepare the original momordica grosvenori fructose, and therefore the sweet taste and the bioactivity of the momordica grosvenori are fully exerted.
Detailed Description
The invention is further illustrated below with reference to examples.
The fresh momordica grosvenori used in the embodiment of the invention is purchased from Jingzhou county in Huai of Hunan province, and the content of mogroside V is 0.47%.
The purified water is prepared by a secondary pure water device for production workshops, and the used anion exchange resin, macroporous adsorption resin, MCI column filler, cation exchange resin, pesticide residue removing special resin, polyphenol adsorption special macroporous resin, edible vegetable oil and other raw and auxiliary materials are all obtained through conventional commercial approaches if no special description exists.
Unless otherwise specified, "%" in the examples of the present invention means mass percent.
In the embodiment of the invention, the content of mogroside V is determined by High Performance Liquid Chromatography (HPLC); detecting glucose, fructose and sucrose with high performance liquid chromatography with differential refraction detector according to "Mel" of 2020 edition of Chinese pharmacopoeia; the mogrolic acid is determined by ultraviolet-visible spectrophotometry (UV) with a wavelength of 770nm (Fulin method); the taste, sweetness multiplier and sweetness duration of the luo han fructose were determined by sensory perception.
Example 1
(1) Crushing and pulsed electric field pretreatment. Taking 5000kg of fresh and mature fructus Siraitiae Grosvenorii, crushing with a fresh fruit crusher, maintaining the state of broken shell but no broken seed, soaking the surface of crushed material with 4500L tap water, and treating with 0.15kv/cm pulse electric field for 25 times until the pulp tissue structure is loose.
(2) Extracting at low temperature. Continuous countercurrent extraction of pretreated Siraitia grosvenorii crushed material at 13 ℃: the extraction tank is divided into 2 sections, water 9000L is added, wherein the first section 4500L and the second section 4500L; extraction was run for 2.5h. After extraction, the residue is squeezed and filtered, and effluent liquid is collected to obtain 13000L of extract.
(3) Filtering and clarifying. The extracting solution is firstly passed through a disk centrifuge, and the centrifugate is further passed through a ceramic membrane complete equipment with the material of zirconia and the aperture of 500nm, and after the feeding is finished, 500L purified water is added to wash the upstream liquid of the ceramic membrane, and the permeate liquid is collected, so that 13000 clear transparent clear liquid of the ceramic membrane is obtained.
(4) And (5) separating the ion resin. The chromatography column is filled with 750kg of macroporous weak alkaline anion exchange resin of model D900 in advance and treated with acid and alkali for standby, 13000L of ceramic membrane clear liquid is fed into the resin column, 3000L of purification water washing resin column is used after feeding is finished, and ion resin effluent and desorption liquid are treated according to IA and IB respectively:
And IA. Ion resin effluent to prepare mogroside.
(1) Refining the adsorption resin. The method comprises the steps of arranging 1200kg of large adsorption resin of AB-8 type in a chromatographic column in advance, treating the adsorption resin with aqueous alcohol and acid and alkali for standby, sequentially and continuously feeding 16000L of feed effluent and water washing liquid of an ion resin column into the resin column, purifying the water washing resin column with 4000L of purified water until the effluent is clear and transparent and nearly colorless after feeding, desorbing with 2400L of ethanol with 65% concentration, eluting ethanol in the chromatographic column with 1000L of purified water after the ethanol is desorbed, and collecting ethanol desorption liquid and water washing alcohol liquid to obtain 3300L of desorption liquid.
(2) MCI column chromatography. Concentrating 3300L of adsorption resin desorption liquid to recover ethanol until no ethanol smell exists, and concentrating to 800L, wherein the solid content is 5.1%. 800kg of GEL CHP20SS resin is filled in a resin column in advance and treated with aqueous alcohol for standby, the concentrated solution is passed through an MCI column, and the feed effluent is collected; and then 1200L of 42% ethanol is used for desorption, after the ethanol is desorbed, 500L of purified water is used for eluting the ethanol in the chromatographic column, and 1700L of desorption liquid is obtained after the desorption liquid is collected. Concentrating the desorption solution to recover ethanol, and combining the ethanol with the effluent to obtain 1800L of MCI column refined solution.
(3) Extracting to remove the plasticizer. Concentrating MCI column refined solution to 370L with solid content of 10.72%, adding 300L edible vegetable oil, stirring, heating to 69 deg.C, maintaining temperature, countercurrent extracting, standing for layering, and collecting water phase.
(4) And (5) clarifying at a low temperature. Refrigerating the water phase to the system temperature of 1 ℃, filtering by using ceramic membrane complete equipment with the material of zirconia and the pore diameter of 200nm, collecting membrane permeation liquid, adding 100L of purified water to wash upstream liquid after feeding, and obtaining clear and transparent ceramic membrane clear liquid.
(5) And (5) drying. Concentrating the clear ceramic membrane liquid until the solid content is 24.6%, and spray-drying at the inlet air temperature of 180 ℃ and the outlet air temperature of 85 ℃ to obtain 38.9kg of V50 pure mogroside.
II, preparing the momordica grosvenori concentrated juice (syrup) by adsorbing the resin effluent.
Desalting. 600kg of macroporous strong acid cation exchange resin with the model of 001 multiplied by 16 is filled in a chromatographic column in advance and treated by acid and alkali for standby, the feed effluent (16000L) and the initial water washing liquid (the initial water washing liquid is 1800L of macroporous adsorption resin 1.5BV in the step IA) of the adsorption resin column are collected, 8000L of concentrated solution is obtained by concentration through a reverse osmosis membrane, the cation resin column is fed, 1800L of purified water is further washed until the pH of the effluent is 5.8 after the feed is finished, and the concentrated solution and the water washing liquid are combined to obtain the desalted solution.
(2) And (5) removing pesticide residues from the resin. 500kg of LSA-900B resin is filled in a chromatographic column in advance, the chromatographic column is treated by aqueous alcohol and acid and alkali for standby, 9800L of desalting solution is fed into the resin column, 1500L of purified water is used for washing the column after feeding, and feeding effluent and water washing liquid are collected to obtain 11200L of pesticide-removing residual liquid.
(3) And (5) extracting. Concentrating the pesticide-removed residual liquid to 3500L under vacuum at 62 ℃ with solid content of 11.4%, adding 2000L edible vegetable oil, continuously stirring, heating to 65 ℃, maintaining the temperature, countercurrent extracting, standing for layering, and collecting water phase.
(4) And (3) membrane separation of the plasticizer. 3500L of water phase is put into organic membrane complete equipment with the molecular weight cut-off of 2KD, and membrane permeate is collected; when the volume of the upstream liquid reaches about 1000L, adding 1000L of purified water into the upstream liquid, continuing to pass through the membrane, and collecting membrane permeation liquid; when the upstream liquid volume reaches about 400L, 400L of purified water is added into the upstream liquid, the membrane is continuously passed through, the upstream liquid volume is 200L, the water-washed permeate is collected and combined with the previous membrane permeate, and the plasticizer removing liquid 4700L is obtained.
(5) Clarifying step by step. Through detection, the solid content of the de-plasticizer liquid is 8.1%, the solution is cooled to room temperature, and the solution is subjected to ceramic membrane complete equipment with zirconium oxide and 500nm pore diameter, and membrane permeate liquid is collected; concentrating the ceramic membrane permeation solution to 2500L, refrigerating to a system temperature of 2 ℃ until the solid content is 15.1%, fully precipitating the precipitate, passing through ceramic membrane complete equipment with zirconium oxide and pore diameter of 200nm, and collecting the membrane permeation solution to obtain clear and transparent ceramic membrane clear liquid.
(6) Concentrating. The clear solution of the ceramic membrane is concentrated to have a sugar degree of 67Brix under reduced pressure at 62 ℃ and a vacuum degree of-0.085 MPa, and 557.8kg of concentrated solution is obtained.
(7) And (5) sterilizing by a pulsed electric field. Treating with 45kv/cm pulse electric field for 500 times, and sterilizing the concentrated solution to obtain 557.8kg of fructus Siraitiae Grosvenorii concentrated juice (syrup).
IB preparing the momordica grosvenori phenolic acid by using the ion resin desorption solution.
(1) And (5) desorption. After 750kg of the macroporous weak-base anion resin column of model D900 is fed, the column is washed by 3000L of purified water until the pH of effluent liquid is 8.2, then the effluent liquid is desorbed by 1500L of aqueous acid-alcohol with hydrochloric acid concentration of 0.4% and ethanol concentration of 65%, and desorption liquid is collected; after the desorption solvent is fed, 600L of purified acid washing alcohol is fed, and the column washing liquid is collected. And combining the desorption liquid and the column washing liquid to obtain 2000L of desorption liquid.
(2) Refining special resin. Recovering ethanol in the desorption liquid under vacuum at 65 ℃ and vacuum degree of-0.085 MPa until no ethanol smell exists, and adding purified water to adjust the solid content to 5.4% to obtain 860L. Pre-filling 1000kg of macroporous adsorption resin special for LX-8 phenolic acid in a chromatographic column, treating with aqueous alcohol and acid and alkali for later use, feeding 860L of desorption concentrate into the resin column, washing the column with 3000L of purified water after feeding until effluent is clear and transparent and nearly colorless, desorbing with 2000L of 65% ethanol, and collecting desorption liquid; and then 600L of purified water is added to wash the ethanol in the column, and effluent liquid is collected. And combining the desorption liquid and the effluent liquid to obtain 2500L of desorption liquid.
(3) Extracting to remove the plasticizer. Concentrating the desorption solution to 360L, adding 200L edible vegetable oil, continuously stirring, heating to 70deg.C, maintaining the temperature, countercurrent extracting, standing for layering, and collecting water phase.
(4) Clarifying. Cooling the water phase to room temperature, adopting ceramic membrane complete equipment with the pore diameter of 500nm and zirconia as the material, and collecting membrane permeate to obtain clear and transparent ceramic membrane clear liquid.
(5) And (5) drying. Concentrating the ceramic membrane clear liquid until the solid content is 22.6%, and spray-drying at 185 ℃ and 82 ℃ to obtain 38.7kg of momordica phenolic acid.
(5) Preparing the momordica grosvenori fructose.
I, original taste momordica grosvenori.
Taking 0.95kg of V50 pure-taste mogroside of the IA in the step (4) and 10.2kg of mogroside of the IB in the step, adding 110kg of purified water for dissolution, and taking the solid content of 9.2% as an adhesive. 88.85kg of erythritol is put into a fluidized bed, the temperature is 75 ℃, the vacuum degree is-0.085 MPa, the adhesive is evenly sprayed at the speed of 45kg/h, and 98.5kg of original momordica grosvenori is obtained after drying.
II, momordica grosvenori zero calorie sugar.
Taking 0.48kg of V50 pure mogroside of the IA of the step (4), adding 8kg of purified water for dissolution, and taking the solid content of 5.66% as an adhesive. 99.52kg of erythritol is put into a fluidized bed, the temperature is 75 ℃, the vacuum degree is-0.085 MPa, the adhesive is evenly sprayed at the speed of 3kg/h, and the raw taste momordica grosvenori 99.3kg is obtained after drying.
Through the detection, the detection results show that,
the mogroside V50 is pure-taste mogroside, wherein the mogroside V content is 52.93wt%, white milk powder is free from pesticide residues and plasticizers, and the 10% aqueous solution is clear, transparent, free from turbidity and precipitation, and free from slight bitter taste.
The sugar degree of the fructus momordicae concentrated juice (syrup) is 67Brix, fructose is 20.1%, glucose is 18.4%, sucrose is 8.27%, and the total amount of monosaccharide and disaccharide is 46.77%.
The phenolic acid content of the momordica grosvenori phenolic acid is 86.31wt%.
The original taste of the momordica grosvenori is about 2 times of that of sucrose, the sweetness duration is 15.3 seconds, the content of the mogroside V is 0.50 weight percent, and the content of the erythritol is 88.85 weight percent.
Lo Han Guo has no calorie sugar, sweetness about 1 time of sucrose, sweetness duration of 12.5 seconds, mogroside V content of 0.25wt% and erythritol content of 99.52wt%.
Example 2
Other operations and conditions were the same as in example 1, except that in step (2), the pretreated crushed grosvenor momordica fruit was subjected to continuous countercurrent extraction at 10 ℃. 33.2kg of V50 pure-taste mogroside is finally obtained, wherein the content of the mogroside V is 51.33wt%, the color is milky white, no pesticide residues and plasticizers are detected, and the 10% aqueous solution is clear, transparent, free of turbidity and precipitation, and free of slight bitter taste in the mouth.
The V50 mogroside and the mogroside acid powder obtained in example 2 are prepared into the original flavor of momordica grosvenori and momordica grosvenori zero-calorie sugar according to the same conditions and raw material ratio in example 1.
Example 3
Other operations and conditions were the same as in example 1, except that in step (2), the pretreated crushed grosvenor momordica fruit was subjected to continuous countercurrent extraction at 20 ℃. And finally obtaining 35.1kg of V50 pure-taste mogroside, wherein the content of the mogroside V is 52.16wt%, the color is slightly yellow, no pesticide residues and plasticizers are detected, and the 10% aqueous solution is slightly yellow and has no slight bitter taste in the mouth.
The V50 mogroside and the mogroside acid powder obtained in example 3 are prepared into the original flavor of momordica grosvenori fructose and momordica grosvenori zero-calorie sugar according to the same conditions and raw material ratio in example 1.
Example 4
Other operations and conditions were the same as in example 1, except that in step (2), the pretreated crushed grosvenor momordica fruit was subjected to continuous countercurrent extraction at 30 ℃. 34.7kg of V50 pure-taste mogroside is finally obtained, wherein the mogroside V content is 50.58wt%, the color is yellowish white, no pesticide residues and plasticizers are detected, and the 10% aqueous solution is light yellow, and has no slight bitter taste when being imported.
The V50 mogroside and the mogroside acid powder obtained in example 4 are prepared into the original flavor of momordica grosvenori and momordica grosvenori zero-calorie sugar according to the same conditions and raw material ratio in example 1.
Example 5
Other operations and conditions were the same as in example 1 except that in step IA (2) MCI column chromatography, 1200L concentration 50% ethanol was used for desorption. 39.0kg of V50 pure mogroside is finally obtained, wherein the content of the mogroside V is 52.70wt%.
The V50 mogroside and the mogroside acid powder obtained in example 5 are prepared into the original flavor of momordica grosvenori and momordica grosvenori zero-calorie sugar according to the same conditions and raw material ratio in example 1.
Example 6
Other operations and conditions were the same as in example 1 except that in step IA (2) MCI column chromatography, 1200L concentration 60% ethanol was used for desorption. 39.4kg of V50 pure mogroside is finally obtained, wherein the content of the mogroside V is 50.61wt%.
The V50 mogroside and the mogroside acid powder obtained in example 6 are prepared into the original flavor of momordica grosvenori fructose and momordica grosvenori zero calorie sugar according to the same conditions and raw material ratio in example 1.
Example 7
Other operations and conditions were the same as in example 1 except that 1200L of 65% ethanol was used for desorption in the (2) MCI column chromatography of step IA. 39.4kg of V50 pure mogroside is finally obtained, wherein the content of the mogroside V is 50.61wt%.
The V50 mogroside and the mogroside acid powder obtained in example 6 are prepared into the original flavor of momordica grosvenori fructose and momordica grosvenori zero calorie sugar according to the same conditions and raw material ratio in example 1.
Example 8
Other operations and conditions are the same as in example 1, except that in the step (1) of preparing mogrolic acid from the ion resin desorption solution in step IB. The desorption liquid is 1500L of alcohol water solution with 65% of ethanol concentration, namely, the solution does not contain 0.4% hydrochloric acid. 29.5kg of momordica grosvenori phenolic acid is finally obtained, and the phenolic acid content is 85.29wt%.
The original momordica grosvenori fructose and momordica grosvenori zero-calorie sugar obtained in the above example were subjected to sensory testing according to the following method:
1. screening and training of sensory analysts
Sensory panelists were screened according to the rules of GB/T16291.2-2010, and after the odor and taste sensitivity training, sensory panelists were screened to make up a sensory panel.
2. Subjective evaluation of taste:
sensory analysts restricted their diets, especially food consumption, within 1h before the start of the assessment experiment, which could severely affect smell and taste. 12 sensory analysts (halves of men and women) were selected from 20 subjects to perform sensory evaluation of the reduced-sugar sweetener of the present invention. The odor and taste of the sweetener solution were scored comprehensively, with scores ranging from 1 to 10.
The taste test is specifically to prepare the momordica grosvenori and water in the embodiment into a solution with the same sweetness as that of a 3wt% sucrose solution, test, take 10mL of the solution to be evaluated in a disposable paper cup, make the solution stay in the mouth for a few seconds and spit out, make the solution be classified into full score of 5, make the taste best, make the evaluation time interval be 20min, and remove the evaluation result to evaluate the highest score and the lowest score, and take the average value of scores of the rest 10 evaluation staff.
The odor test asks the panelists to directly evaluate the odor about 3-5cm from the nose, the evaluation time interval is 20min, the 5 points are full points, the odor test senses the best, the highest point and the lowest point are removed from the evaluation result, and the average value of scores of the rest 10 panelists is taken. The results are shown in table 1 below:
TABLE 1
Therefore, after the mogroside V50 and the mogrol are prepared by the method, the taste of the prepared momordica grosvenori fructose is obviously improved. The possible reasons are 1, removing the known substances affecting the taste and flavor of mogrosides, such as mogroside IIE, which is a bitter saponin component; 2. unknown impurities possibly introduced due to ion exchange during decolorization of the ion resin are removed; 3. the advantages of mogroside and mogrolic acid in taste are complementary, and the taste is synergistically improved.

Claims (6)

1. A method for preparing mogroside, mogrolic acid and fructus Siraitiae Grosvenorii concentrated juice from fresh fructus Siraitiae Grosvenorii comprises the following steps:
(S1) crushing fresh momordica grosvenori, immersing the crushed momordica grosvenori in water, treating the crushed momordica grosvenori under the condition of a pulse electric field, continuously countercurrent extracting the momordica grosvenori under the condition of low temperature, filtering the momordica grosvenori, loading the momordica grosvenori on an alkaline anion resin column, washing the momordica grosvenori after full feeding, collecting a washing liquid 1, and combining a feeding effluent and the washing liquid 1; desorbing with alcohol solution containing water and acid, eluting with water, collecting water washing solution 2, and mixing the desorption solution and the water washing solution 2; the strength of the pretreatment pulse electric field is 0.5-2.0 kv/cm, and the times are 10-30; the low temperature is 10-20 ℃; the alcohol solution containing water and acid is an alcohol water solution with the alcohol concentration of 50-75wt% and the inorganic acid concentration of 0.3-1wt%; the dosage of the alkaline anion resin is 7-20wt% of the fresh fructus momordicae, the height-diameter ratio of the alkaline anion resin is 4-8:1, the feeding flow rate is 0.6-1.5BV/h, the water washing flow rate is 1.0-2.0BV/h, and the pH of the effluent liquid is washed until the pH is 7.5-8.5;
(S2) combining alkaline anion resin feed effluent and water washing liquid 1, loading the mixture on a macroporous adsorption resin column, washing until the effluent is clear, transparent and colorless, desorbing the effluent with aqueous alcohol 1, washing the mixture with water, collecting desorption liquid and water washing liquid, concentrating the mixture, loading the mixture on an MCI column, collecting MCI column feed effluent, desorbing the mixture with aqueous alcohol 2, eluting the mixture with water, combining the desorption liquid and the water washing liquid, concentrating the mixture, combining the mixture with MCI column feed effluent to obtain MCI column refined liquid, concentrating the mixture, adding edible vegetable oil, stirring the mixture under heating, carrying out countercurrent extraction, standing and layering, collecting water phase, refrigerating the water phase, filtering the water phase, concentrating the water phase, and spray-drying the water phase to obtain V50 mogroside; the alcohol concentration of the aqueous alcohol 1 is 50-70 wt%, and the alcohol concentration of the aqueous alcohol 2 is 35-50wt%; the volume consumption of the aqueous alcohol 1 is 1.5-3 times of the mass of the macroporous adsorption resin, the unit L/kg, and the volume consumption of the aqueous alcohol 2 is 1-2.5 times of the mass of the MCI resin, the unit L/kg;
(S3) collecting the macroporous adsorption resin feed effluent and the initial washing liquid in the step (S2), loading the macroporous adsorption resin feed effluent and the initial washing liquid on a cation resin column, collecting the feed effluent, feeding purified water after feeding, washing the purified water, combining the cation resin column feed effluent and 0-2 BV washing liquid, concentrating to obtain desalted liquid, loading the desalted liquid into a special pesticide residue removing resin column, washing the desalted liquid, combining the effluent and the washing liquid, concentrating for the first time, adding edible vegetable oil, heating and stirring, countercurrent extracting, standing and layering, collecting water phase, feeding the water phase into an organic film complete equipment with the molecular weight of 2 KD-3 KD, concentrating for the second time, filtering, concentrating for the third time, refrigerating, filtering again, concentrating to proper sugar degree, and obtaining the fructus momordicae concentrated juice;
(S4) combining the anion resin desorption liquid and the water washing liquid 2 in the step (S1), concentrating, adding a phenolic acid special-purpose adsorption resin, washing with water, desorbing with aqueous alcohol 3, concentrating the desorption liquid, adding edible vegetable oil, heating and stirring, countercurrent extracting, standing for layering, collecting a water phase, filtering, concentrating, and spray-drying to obtain the momordica grosvenori phenolic acid;
in the steps (S2), (S3) and (S4), the addition amount of the edible vegetable oil is 0.4-1.5 times of the volume of the concentrated solution, and the heating temperature is 60-75 ℃ after the edible vegetable oil is added.
2. The method according to claim 1, further comprising the step of preparing momordica grosvenori fructose of step (S5):
(S5A) preparing original momordica grosvenori fructose:
taking mogroside V50 in the step (S2) and mogroside acid in the step (S4) according to a proportion, adding water for dissolution, taking erythritol as an adhesive, putting the erythritol into a fluidized bed, uniformly spraying the adhesive, and drying to obtain the original momordica grosvenori fructose;
and/or
(S5B) preparing momordica grosvenori zero-calorie sugar:
dissolving mogroside V50 in the step (S2) in water, adding erythritol into a fluidized bed as an adhesive, uniformly spraying the adhesive, and drying to obtain the momordica grosvenori zero-calorie sugar.
3. The method according to claim 1, wherein in step (S2), the refrigeration is at 1-5 ℃.
4. The method according to claim 1, wherein in the step (S3), the first concentration is to a solids content of 9 to 12%; the second concentration is concentration until the solid content is 4-10%; and the third concentration is to concentrate to the solid content of 12-20%.
5. The method of claim 2, wherein the mass ratio of mogroside V50 to mogroside acid in step (S5A) is 1: 0.5-15.
6. The method of claim 5, wherein the mass ratio of mogroside V50 to mogroside acid in step (S5A) is 1:6-12.
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CN114410411A (en) * 2022-01-11 2022-04-29 刘庚贵 Momordica grosvenori wine and preparation method thereof
CN115581266B (en) * 2022-09-02 2024-03-12 湖南华诚生物资源股份有限公司 Clean production method of momordica grosvenori dry powder and momordica grosvenori concentrated juice
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