CN113861260A - Preparation method of momordica grosvenori sweet glycoside compounds - Google Patents
Preparation method of momordica grosvenori sweet glycoside compounds Download PDFInfo
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
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- C07J—STEROIDS
- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
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Abstract
The invention discloses a preparation method of a momordica grosvenori sweet glycoside compound, which comprises the following steps: cleaning and crushing fresh momordica grosvenori, and then carrying out water extraction and endophytic enzyme hydrolysis to obtain momordica grosvenori extract; finely filtering and concentrating the momordica grosvenori extract to obtain momordica grosvenori concentrated solution; taking the concentrated momordica grosvenori solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain a momordica grosvenori glycoside enrichment solution; carrying out decoloration, deodorization and pesticide residue removal treatment on the mogroside enrichment solution to obtain a mogroside solution; and concentrating the mogroside solution, and drying to be powdery to obtain the mogroside compound. The method provided by the invention has simple process, can realize large-scale production, reduces the production cost of the mogroside product, and can meet the market demand on the product quality.
Description
Technical Field
The invention relates to the technical field of momordica grosvenori processing, and in particular relates to a preparation method of momordica grosvenori sweet glycoside compounds.
Background
The momordica grosvenori, which is called as the hirsute fruit, the false balsam pear, the momordica glabra, the stephania japonica and the like, is the fruit of Siraitia grosvenorii (swing) C.Jeffrey ex A.M.Lu et Z.Y.Zhang which is a cucurbitaceous plant, is mainly produced in Guilin Yongfu county, has sweet and cool taste, enters lung and large intestine channels, clears heat and moistens lung, relieves sore throat and makes sound, and relieves constipation, and is used for lung heat and dry cough, sore throat and aphonia, and intestinal dryness and constipation.
The momordica grosvenori contains momordica grosvenori triterpenoid saponin, and also contains a large amount of fructose, more than ten kinds of essential amino acids for human bodies, fatty acid, flavonoid compounds, vitamin C, trace elements and the like. The mogroside is used as main component of fructus Siraitiae Grosvenorii sweetener, and is triterpene glucoside with sweet taste, and its glycoside is triterpene alcohol. The mogroside V is a main sweet component, has no toxicity, low calorie, high sweetness and good heat stability, is one of the substances developed by natural sweeteners, is the best substitute of cane sugar, and is increasingly valued by food industries at home and abroad.
Mogroside has been produced for many years, and related technologies are more, but the problems of high production cost and complex process exist.
Disclosure of Invention
The invention mainly aims to provide a preparation method of mogroside compounds, and aims to provide a method for preparing mogroside with low production cost and simple process.
In order to realize the purpose, the invention provides a preparation method of a momordica grosvenori sweet glycoside compound, which comprises the following steps:
cleaning and crushing fresh momordica grosvenori, and then carrying out water extraction and endophytic enzyme hydrolysis to obtain momordica grosvenori extract;
finely filtering and concentrating the momordica grosvenori extract to obtain momordica grosvenori concentrated solution;
taking the concentrated momordica grosvenori solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain a momordica grosvenori glycoside enrichment solution;
carrying out decoloration, deodorization and pesticide residue removal treatment on the mogroside enrichment solution to obtain a mogroside solution;
and concentrating the mogroside solution, and drying to be powdery to obtain the mogroside compound.
Optionally, the steps of washing and crushing fresh momordica grosvenori, and then carrying out water extraction and endophytic enzyme hydrolysis to obtain momordica grosvenori extract comprise:
cleaning and crushing fresh momordica grosvenori, placing the fresh momordica grosvenori in a countercurrent extraction system, extracting the momordica grosvenori for 30-60 min at 45-55 ℃, then extracting the momordica grosvenori for 30-60 min at 70-80 ℃, and then carrying out solid-liquid separation to obtain a momordica grosvenori extracting solution.
Optionally, in the step of fine filtering and concentrating the momordica grosvenori extract to obtain the momordica grosvenori concentrated solution, the fine filtering step includes:
firstly, a ceramic membrane filter element with the thickness of 200nm is used, primary fine filtration is carried out under the conditions that the temperature is 40-50 ℃ and the pressure is 10-20 bar, and then an ultrafiltration membrane with the molecular weight of 1500-2000 is used, and secondary fine filtration is carried out under the conditions that the temperature is 30-40 ℃ and the pressure is 20-30 bar.
Optionally, the fine filtration and concentration of the momordica grosvenori extract are performed to obtain a momordica grosvenori concentrated solution, wherein the momordica grosvenori concentrated solution comprises the following steps:
the brix of the momordica grosvenori concentrated solution is 5-10%.
Optionally, taking the momordica grosvenori concentrated solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain the momordica grosvenori glycoside enriched solution, wherein the steps comprise:
and the pH value is adjusted to 9.0-10.5.
Optionally, taking the momordica grosvenori concentrated solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain the momordica grosvenori glycoside enriched solution, wherein the steps comprise:
the flow rate of the bubbling gas is as follows: the gas flow rate per min is 1/30-1/20 of the tower volume of the foam separation tower.
Optionally, taking the momordica grosvenori concentrated solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain the momordica grosvenori glycoside enriched solution, wherein the steps comprise:
the multistage foam separation is 1-3 grades.
Optionally, taking the momordica grosvenori concentrated solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain the momordica grosvenori glycoside enriched solution, wherein the defoaming comprises the following steps:
and spraying an ethanol solution with the volume concentration of 90-95% into the foam solution.
Optionally, the step of performing decolorization, deodorization and pesticide residue removal treatment on the mogroside enrichment solution to obtain a mogroside solution comprises the following steps:
decolorizing the mogroside enrichment solution with ion exchange resin, collecting effluent, eluting with purified water until no sweet taste exists, and mixing the effluent and the eluate;
and passing the combined effluent and eluent through an active carbon column, deodorizing and removing pesticide residues, collecting the effluent, eluting by using purified water until no sweet taste exists, and combining the effluent and the eluent again to obtain the mogroside solution.
Optionally, the step of concentrating the mogroside solution and then drying the solution to be powder to obtain the mogroside compound comprises:
and adjusting the pH value of the mogroside solution to 4.0-6.0, then concentrating until the brix is 50-60%, and then carrying out spray drying to obtain the mogroside compound.
According to the technical scheme provided by the invention, the preparation method of the momordica grosvenori sweet glycoside compound firstly carries out endophytic enzyme enzymolysis on momordica grosvenori to obtain momordica grosvenori extract, and then adopts a foam separation technology to purify the momordica grosvenori extract to obtain the momordica grosvenori sweet glycoside compound. The process breaks the limitation of the prior art, does not need exogenous enzyme, fully utilizes the endogenous enzyme of the momordica grosvenori to carry out enzymolysis on protein and pectin, reduces the production cost, and simultaneously eliminates the interference of substances easy to foam, such as protein and the like in the momordica grosvenori; then, the characteristic that mogroside in the momordica grosvenori can generate foam in a large amount and durably under a proper pH value is further utilized, and a foam separation technology is used for purification, so that a large amount of waste water is avoided during generation, and the sewage treatment cost is reduced; in sum, the method provided by the invention has the advantages of simple process, large-scale production, reduction of production cost and capability of meeting the market demand for product quality.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of an embodiment of the method for preparing mogroside compounds provided by the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to reduce the production cost of mogroside and simplify the process, the invention provides a preparation method of a mogroside compound, and fig. 1 shows an embodiment of the preparation method of the mogroside compound provided by the invention. Referring to fig. 1, in this embodiment, the method for preparing mogroside compounds includes the following steps:
step S10, cleaning and crushing fresh fructus Siraitiae Grosvenorii, extracting with water and performing enzymolysis with endogenetic enzyme to obtain fructus Siraitiae Grosvenorii extractive solution;
cleaning and crushing fresh fructus Siraitiae Grosvenorii, placing into countercurrent extraction equipment, performing water extraction and endophytic enzyme enzymolysis by means of segmented temperature control, and performing solid-liquid separation to obtain fructus Siraitiae Grosvenorii extractive solution. The segmented temperature control refers to performing water extraction and endophytic enzyme enzymolysis at two different temperatures, and specifically, in this embodiment, step S10 includes: cleaning and crushing fresh momordica grosvenori, placing the fresh momordica grosvenori in a countercurrent extraction system, extracting for 30-60 min at 45-55 ℃, performing enzymolysis on protein and pectin by using momordica grosvenori endoprotease, and simultaneously preventing the momordica grosvenori from being subjected to protein foaming in the subsequent foam separation step to influence purification of momordica grosvenori glycoside; then extracting at 70-80 ℃ for 30-60 min, and inactivating active protein kinase in the momordica grosvenori, so that the finally prepared momordica grosvenori sweet glycoside compound product has no tongue numbness; and finally, performing solid-liquid separation by using a horizontal screw centrifuge to obtain a momordica grosvenori extract.
S20, carrying out fine filtration and concentration on the fructus momordicae extract to obtain a fructus momordicae concentrated solution;
after the fructus momordicae extract is prepared, macromolecules such as protein without enzymolysis are removed through fine filtration, and then concentrated into concentrated solution. The fine filtration comprises a two-step fine filtration process, and in this embodiment, the two-step fine filtration process specifically comprises: firstly, a ceramic membrane filter element with the thickness of 200nm is used, and primary fine filtration is carried out under the conditions of the temperature of 40-50 ℃ and the pressure of 10-20 bar to obtain fine filtration liquid; and pumping the refined filtrate into a membrane system by using a pump, performing secondary fine filtration by using an ultrafiltration membrane with the molecular weight of 1500-2000 at the temperature of 30-40 ℃ and under the pressure of 20-30 bar, and filtering macromolecular substances such as pectin, protein and the like in the refined filtrate to obtain the dialysate.
Then, concentrating the obtained dialysate to obtain a concentrated solution, wherein controlling the concentration of the concentrated solution is important for the subsequent foam separation process, and if the concentration is relatively too high, the size of bubbles may be reduced, the liquid content of the bubbles may be increased, the separation efficiency may be low, and the concentration of residual liquid may be increased; if the concentration is relatively low, there may be a problem that the driving force for mogroside to diffuse from the center of the solution to the surface is insufficient. Preferably, in the embodiment of the invention, the fructus momordicae concentrated solution requires that the Brix is 5-10%. Within the concentration range, the subsequent foam separation mode is more favorable for separating and purifying the mogrosides in the concentrated momordica grosvenori liquid.
S30, taking the concentrated momordica grosvenori solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain a mogroside enrichment solution;
after the momordica grosvenori concentrated solution is prepared, the momordica grosvenori concentrated solution is used as bubbling initial feed liquid to carry out multistage foam separation and purification, the foam separation technology is to carry out separation based on the surface activity difference between momordica grosvenori sweet glycoside to be separated and other components in the solution according to the surface adsorption principle, and the foam layer is separated from the main body of the solution by bubbling in the solution and forming the foam layer, so that the purpose of enriching the momordica grosvenori sweet glycoside can be achieved because the momordica grosvenori sweet glycoside is gathered in the foam layer. In addition, the initial mother liquor after foam separation is concentrated and dried, and can also be used for preparing low-content mogroside products rich in amino acid.
Further, in step S30, the pH adjustment is performed to adjust the pH of the luo han guo concentrated solution to be alkaline, so as to avoid the problem that luo han guo glycoside generates few and transient bubbles under acidic conditions. Particularly preferably, the pH value of the fructus momordicae concentrated solution is adjusted to 9.0-10.5. Thus, the method is favorable for generating abundant and stable bubbles in the foam separation process of the mogroside.
Furthermore, in step S30, the bubbling gas flow rate is also an important parameter, and too high a gas flow rate increases the amount of foam, and the residence time in the foam tower decreases, which easily results in a decrease in the concentration of mogroside separated from the foam; too low a gas flow may result in the bubbles not reaching the height of the foam column and not being collected. Preferably, in the embodiment of the present invention, the flow rate of the bubbling gas is: the gas flow rate per min is 1/30-1/20 of the tower volume of the foam separation tower. In this way, it is ensured that the foam layer can be separated from the foam, and the mogroside concentration in the separated foam layer is high.
In addition, the multi-stage foam separation in the step S30 is 1-3 stages, and products with different mogroside V contents can be obtained by performing foam separation in a grading manner, so that different application requirements can be met. When 1-level foam separation is adopted, directly taking the momordica grosvenori concentrated solution as bubbling initial feed liquid to perform foam separation and collecting a foam solution; the initial mother liquor after foam separation is concentrated and dried, and can be used for preparing low-content mogroside products rich in amino acid. When 2-stage foam separation is adopted, the foam solution collected at the 1 st stage is used as the initial feed liquid of the 2 nd-stage foam separation, and the foam solution at the 2 nd stage is collected for defoaming; the initial mother liquor after foam separation can be used for preparing a low-content mogroside product rich in amino acid after concentration and drying, and the 1 st-level mother liquor can be used for preparing a compounded high-content mogroside product after subsequent decolorization, deodorization, pesticide residue removal, concentration, drying and other treatment provided by the invention so as to adapt to different customer requirements. When 3-level foam separation is adopted, the foam solution collected at the 1 st level is used as the initial feed liquid of the 2 nd level foam separation, the foam solution collected at the 2 nd level is used as the initial feed liquid of the 3 rd level foam separation, and finally the foam solution collected at the 3 rd level is defoamed; the initial mother liquor after foam separation is concentrated and dried and can be used for preparing low-content mogroside products rich in amino acid, and the 1 st-level and 2 nd-level mother liquors can be used for preparing compound high-content mogroside products after subsequent decolorization, deodorization, pesticide residue removal, concentration, drying and other treatments provided by the invention so as to adapt to different customer requirements.
In addition, the method for defoaming the foaming solution in step S30 may be a method of standing, vacuum stirring or adding a defoaming agent, and preferably a method of adding a defoaming agent is used. In a preferred embodiment of the present invention, an ethanol solution with a volume concentration of 90-95% is used as a defoaming agent, and the defoaming treatment is performed by spraying the ethanol solution with a volume concentration of 90-95% into the foam solution. Therefore, the defoaming time can be shortened, and the production efficiency can be improved.
Step S40, carrying out decoloration, deodorization and pesticide residue removal treatment on the mogroside enrichment solution to obtain a mogroside solution;
after the foam separation and purification is completed, the obtained mogroside enrichment liquid is required to be subjected to decolorization, deodorization and pesticide residue removal treatment, wherein the decolorization treatment can be realized by using ion exchange resin, and the deodorization and pesticide residue removal treatment can be realized by using an activated carbon column. Specifically, in the embodiment of the present invention, step S40 includes: firstly, decoloring the mogroside enrichment solution by using ion exchange resin, wherein the ion exchange resin is preferably D947 ion exchange resin, so that a product subjected to decoloring treatment is more milky, collecting effluent liquid, eluting by using purified water until no sweet taste exists, and then combining the effluent liquid and the eluate to finish decoloring treatment; and then, passing the combined effluent and eluent through an activated carbon column, removing peculiar smell and pesticide residue, collecting the effluent, eluting by using purified water until no sweet taste exists, combining the effluent and the eluent again, and finishing the treatments of deodorizing and removing pesticide residue to obtain the mogroside solution.
And step S50, concentrating the mogroside solution, and drying to be powdery to obtain the mogroside compound.
And finally, concentrating and drying the prepared mogroside solution to obtain the mogroside compound, wherein the drying can be performed in a spray drying manner, and the method has the advantage of high drying efficiency. Specifically, in the present embodiment, step S50 includes: firstly, the pH value of the mogroside solution is adjusted to 4.0-6.0, which is beneficial to making the finally prepared mogroside compound product have fresh and sweet taste; and then concentrating the mogroside solution until Brix is 50-60%, and finally performing spray drying to obtain a powdery product, namely the mogroside compound.
According to the technical scheme provided by the invention, the preparation method of the momordica grosvenori sweet glycoside compound firstly carries out endophytic enzyme enzymolysis on momordica grosvenori to obtain momordica grosvenori extract, and then adopts a foam separation technology to purify the momordica grosvenori extract to obtain the momordica grosvenori sweet glycoside compound. The process breaks the limitation of the prior art, does not need exogenous enzyme, fully utilizes the endogenous enzyme of the momordica grosvenori to carry out enzymolysis on protein and pectin, reduces the production cost, and simultaneously eliminates the interference of substances easy to foam, such as protein and the like in the momordica grosvenori; then, the characteristic that mogroside in the momordica grosvenori can generate foam in a large amount and durably under a proper pH value is further utilized, and a foam separation technology is used for purification, so that a large amount of waste water is avoided during generation, and the sewage treatment cost is reduced; in general, the method provided by the invention is simple in process, can realize large-scale production, reduces the production cost, can meet the market demand for product quality, and finally obtains the mogroside V content of the finally prepared mogroside compound of 31.7-61.3%, wherein the result is lower than the detection limit through 530 pesticide scans.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) Cleaning 5000kg fresh fructus Siraitiae Grosvenorii, crushing, placing in countercurrent extraction equipment, extracting at 50 deg.C for 60min, extracting at 80 deg.C for 30min, and centrifuging with horizontal screw centrifuge to obtain 15000L fructus Siraitiae Grosvenorii extract;
(2) performing primary fine filtration on the fructus momordicae extract obtained in the step (1) by using a 200nm ceramic membrane filter element at the temperature of 45 ℃ and the pressure of 15bar to obtain a fine filtration solution; pumping the fine filtrate into a membrane system by using a pump, performing secondary fine filtration by using an ultrafiltration membrane with the molecular weight of 1800 under the conditions of the temperature of 35 ℃ and the pressure of 25bar, and filtering macromolecular substances such as pectin, protein and the like remained in the fine filtration to obtain dialysate; concentrating the dialysate to Brix of 8% to obtain fructus Siraitiae Grosvenorii concentrate 4800L;
(3) taking the concentrated momordica grosvenori solution obtained in the step (2) as bubbling initial feed liquid, adjusting the pH value to 9.51 by using a 10% sodium hydroxide solution, then putting the raw material into a foam separation tower with the volume of 1000L, continuously feeding, adjusting the flow of bubbling gas to 35L/min, heating the solution to 65 ℃, performing 1-level foam separation and purification, collecting a foam solution, and spraying and defoaming a small amount of ethanol solution with the volume concentration of 90% to obtain the mogroside enrichment solution;
(4) decoloring the mogroside enrichment solution obtained in the step (3) by using D947 ion exchange resin at the flow rate of 1.5BV/h, collecting effluent liquid, eluting by using purified water until no sweet taste exists, and then combining the effluent liquid and the eluate; then, passing the combined effluent and eluent through an active carbon column, removing peculiar smell and pesticide residue at the flow rate of 1.5BV/h, collecting the effluent and eluting by using purified water until no sweet taste exists, and combining the effluent and the eluent again to obtain a mogroside solution;
(5) and (4) regulating the pH value of the mogroside solution obtained in the step (4) to 4.73 by using citric acid, then concentrating until the Brix is 50%, and performing spray drying to obtain 53.4kg of the mogroside compound.
Through detection, the mogroside compound prepared by the embodiment contains 31.7% of mogroside V, and the result is lower than the detection limit through 530 pesticide scans.
Example 2
(1) Cleaning 7000kg fresh fructus Siraitiae Grosvenorii, crushing, placing in countercurrent extraction equipment, extracting at 55 deg.C for 45min, extracting at 75 deg.C for 50min, and centrifuging with horizontal screw centrifuge to obtain 20500L fructus Siraitiae Grosvenorii extract;
(2) performing primary fine filtration on the fructus momordicae extract obtained in the step (1) by using a 200nm ceramic membrane filter element at the temperature of 45 ℃ and the pressure of 15bar to obtain a fine filtration solution; pumping the fine filtrate into a membrane system by using a pump, performing secondary fine filtration by using an ultrafiltration membrane with the molecular weight of 1800 under the conditions of the temperature of 35 ℃ and the pressure of 30bar, and filtering macromolecular substances such as pectin, protein and the like remained in the fine filtration to obtain dialysate; concentrating the dialysate to Brix of 10% to obtain fructus Siraitiae Grosvenorii concentrated solution 5400L;
(3) taking the concentrated momordica grosvenori solution obtained in the step (2) as a bubbling initial feed liquid, adjusting the pH value to 9.06 by using a 10% sodium hydroxide solution, then putting the obtained material into a foam separation tower with the volume of 1000L, continuously feeding the material, adjusting the flow rate of bubbling gas to 33L/min, heating the solution to 65 ℃, performing 2-level foam separation and purification, taking the foam solution collected at the 1 st level as the initial feed liquid for 2 nd-level foam separation, collecting the foam solution at the 2 nd level, and spraying and defoaming a small amount of ethanol solution with the volume concentration of 95% to obtain the mogroside-enriched liquid;
(4) decoloring the mogroside enrichment solution obtained in the step (3) by using D947 ion exchange resin at the flow rate of 1.5BV/h, collecting effluent liquid, eluting by using purified water until no sweet taste exists, and then combining the effluent liquid and the eluate; then, passing the combined effluent and eluent through an active carbon column, removing peculiar smell and pesticide residue at the flow rate of 1.0BV/h, collecting the effluent and eluting by using purified water until no sweet taste exists, and combining the effluent and the eluent again to obtain a mogroside solution;
(5) and (4) regulating the pH value of the mogroside solution obtained in the step (4) to 5.40 by using citric acid, then concentrating until the Brix is 57%, and performing spray drying to obtain 44.1kg of the mogroside compound.
Through detection, the mogroside compound prepared by the embodiment contains 48.6% of mogroside V, and the result is lower than the detection limit through 530 pesticide scans.
Example 3
(1) Cleaning 6000kg of fresh fructus Siraitiae Grosvenorii, crushing, placing in countercurrent extraction equipment, extracting at 52 deg.C for 50min, then at 77 deg.C for 60min, and centrifuging with horizontal screw centrifuge to obtain 18600L fructus Siraitiae Grosvenorii extract;
(2) performing primary fine filtration on the fructus momordicae extract obtained in the step (1) by using a ceramic membrane filter element with the thickness of 200nm at the temperature of 45 ℃ and the pressure of 20bar to obtain fine filtration liquid; pumping the fine filtrate into a membrane system by using a pump, performing secondary fine filtration by using an ultrafiltration membrane with the molecular weight of 1800 under the conditions of the temperature of 35 ℃ and the pressure of 20bar, and filtering macromolecular substances such as pectin, protein and the like remained in the fine filtration to obtain dialysate; concentrating the dialysate to Brix of 5% to obtain fructus Siraitiae Grosvenorii concentrated solution 8700L;
(3) taking the concentrated momordica grosvenori solution obtained in the step (2) as a bubbling initial feed liquid, adjusting the pH value to 10.48 by using a 10% sodium hydroxide solution, then putting the concentrated momordica grosvenori solution into a foam separation tower with the volume of 1000L, continuously feeding, adjusting the flow rate of bubbling gas to be 45L/min, heating the solution to 75 ℃, performing 3-level foam separation and purification, taking a foam solution collected at the 1 st level as the initial feed liquid of 2 nd level foam separation, taking a foam solution collected at the 2 nd level as the initial feed liquid of 3 rd level foam separation, collecting a foam solution at the 3 rd level, and spraying and defoaming a small amount of ethanol solution with the volume concentration of 90% to obtain a mogroside enriched liquid;
(4) decoloring the mogroside enrichment solution obtained in the step (3) by using D947 ion exchange resin at the flow rate of 1.0BV/h, collecting effluent liquid, eluting by using purified water until no sweet taste exists, and then combining the effluent liquid and the eluate; then, passing the combined effluent and eluent through an active carbon column, removing peculiar smell and pesticide residue at the flow rate of 1.0BV/h, collecting the effluent and eluting by using purified water until no sweet taste exists, and combining the effluent and the eluent again to obtain a mogroside solution;
(5) and (4) regulating the pH value of the mogroside solution obtained in the step (4) to 4.85 by using citric acid, then concentrating until the Brix is 54%, and performing spray drying to obtain 27.6kg of the mogroside compound.
Through detection, the mogroside compound prepared by the embodiment contains 61.3% of mogroside V, and the result is lower than the detection limit through 530 pesticide scans.
Example 4
(1) Cleaning 10000kg of fresh fructus Siraitiae Grosvenorii, crushing, placing in countercurrent extraction equipment, extracting at 45 deg.C for 30min, then at 70 deg.C for 40min, and centrifuging with horizontal screw centrifuge to obtain 25800L fructus Siraitiae Grosvenorii extract;
(2) performing primary fine filtration on the fructus momordicae extract obtained in the step (1) by using a ceramic membrane filter element with the thickness of 200nm at the temperature of 40 ℃ and the pressure of 10bar to obtain fine filtration liquid; pumping the fine filtrate into a membrane system by using a pump, performing secondary fine filtration by using an ultrafiltration membrane with the molecular weight of 1500 at the temperature of 30 ℃ and under the pressure of 25bar, and filtering macromolecular substances such as pectin, protein and the like remained in the fine filtration to obtain dialysate; concentrating the dialysate to Brix of 7% to obtain concentrated solution 11300L of fructus Siraitiae Grosvenorii;
(3) taking the concentrated momordica grosvenori solution obtained in the step (2) as a bubbling initial feed liquid, adjusting the pH value to 9.86 by using a 10% sodium hydroxide solution, then putting the concentrated momordica grosvenori solution into a foam separation tower with the volume of 1000L, continuously feeding, adjusting the flow rate of bubbling gas to be 50L/min, heating the solution to 50 ℃, performing 3-level foam separation and purification, taking a foam solution collected at the 1 st level as the initial feed liquid of 2 nd level foam separation, taking a foam solution collected at the 2 nd level as the initial feed liquid of 3 rd level foam separation, collecting a foam solution at the 3 rd level, and spraying and defoaming a small amount of ethanol solution with the volume concentration of 95% to obtain the mogroside enriched liquid;
(4) decoloring the mogroside enrichment solution obtained in the step (3) by using D947 ion exchange resin at the flow rate of 1.0BV/h, collecting effluent liquid, eluting by using purified water until no sweet taste exists, and then combining the effluent liquid and the eluate; then, passing the combined effluent and eluent through an active carbon column, removing peculiar smell and pesticide residue at the flow rate of 1.0BV/h, collecting the effluent and eluting by using purified water until no sweet taste exists, and combining the effluent and the eluent again to obtain a mogroside solution;
(5) and (4) regulating the pH value of the mogroside solution obtained in the step (4) to 4.08 by using citric acid, then concentrating until the Brix is 52%, and performing spray drying to obtain 53.7kg of the mogroside compound.
Through detection, the mogroside compound prepared by the embodiment contains 51.4% of mogroside V, and the result is lower than the detection limit through 530 pesticide scans.
Example 5
(1) Cleaning 8000kg fresh fructus Siraitiae Grosvenorii, crushing, placing in countercurrent extraction equipment, extracting at 48 deg.C for 40min, extracting at 73 deg.C for 45min, and centrifuging with horizontal screw centrifuge to obtain 22800L fructus Siraitiae Grosvenorii extract;
(2) performing primary fine filtration on the fructus momordicae extract obtained in the step (1) by using a ceramic membrane filter element with the thickness of 200nm at the temperature of 50 ℃ and the pressure of 15bar to obtain fine filtration liquid; pumping the fine filtrate into a membrane system by using a pump, performing secondary fine filtration by using an ultrafiltration membrane with the molecular weight of 2000 at the temperature of 40 ℃ and under the pressure of 25bar, and filtering macromolecular substances such as pectin, protein and the like remained in the fine filtration to obtain dialysate; concentrating the dialysate to Brix of 6% to obtain fructus Siraitiae Grosvenorii concentrated solution 10600L;
(3) taking the concentrated momordica grosvenori solution obtained in the step (2) as a bubbling initial feed liquid, adjusting the pH value to 10.14 by using a 10% sodium hydroxide solution, then putting the concentrated momordica grosvenori solution into a foam separation tower with the volume of 1000L, continuously feeding, adjusting the flow rate of bubbling gas to 47L/min, heating the solution to 80 ℃, performing 3-level foam separation and purification, taking a foam solution collected at the 1 st level as the initial feed liquid of 2 nd level foam separation, taking a foam solution collected at the 2 nd level as the initial feed liquid of 3 rd level foam separation, collecting a foam solution at the 3 rd level, and spraying and defoaming a small amount of ethanol solution with the volume concentration of 92% to obtain a mogroside enriched liquid;
(4) decoloring the mogroside enrichment solution obtained in the step (3) by using D947 ion exchange resin at the flow rate of 1.0BV/h, collecting effluent liquid, eluting by using purified water until no sweet taste exists, and then combining the effluent liquid and the eluate; then, passing the combined effluent and eluent through an active carbon column, removing peculiar smell and pesticide residue at the flow rate of 1.0BV/h, collecting the effluent and eluting by using purified water until no sweet taste exists, and combining the effluent and the eluent again to obtain a mogroside solution;
(5) and (4) regulating the pH value of the mogroside solution obtained in the step (4) to 5.96 by using citric acid, then concentrating until the Brix is 60%, and performing spray drying to obtain 41.4kg of the mogroside compound.
Through detection, the mogroside compound prepared by the embodiment contains 55.8% of mogroside V, and the result is lower than the detection limit through 530 pesticide scans.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (10)
1. A preparation method of a momordica grosvenori sweet glycoside compound is characterized by comprising the following steps:
cleaning and crushing fresh momordica grosvenori, and then carrying out water extraction and endophytic enzyme hydrolysis to obtain momordica grosvenori extract;
finely filtering and concentrating the momordica grosvenori extract to obtain momordica grosvenori concentrated solution;
taking the concentrated momordica grosvenori solution as a bubbling initial feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multistage foam separation and purification in a foam separation tower, collecting a foam solution, and then defoaming to obtain a momordica grosvenori glycoside enrichment solution;
carrying out decoloration, deodorization and pesticide residue removal treatment on the mogroside enrichment solution to obtain a mogroside solution;
and concentrating the mogroside solution, and drying to be powdery to obtain the mogroside compound.
2. The method of claim 1, wherein the steps of washing and crushing fresh luo han guo, extracting with water and performing enzymolysis with endophytic enzymes to obtain luo han guo extract comprise:
cleaning and crushing fresh momordica grosvenori, placing the fresh momordica grosvenori in a countercurrent extraction system, extracting the momordica grosvenori for 30-60 min at 45-55 ℃, then extracting the momordica grosvenori for 30-60 min at 70-80 ℃, and then carrying out solid-liquid separation to obtain a momordica grosvenori extracting solution.
3. The method of claim 1, wherein the step of fine filtering and concentrating the Luo Han Guo extract to obtain the Luo Han Guo concentrated solution comprises the steps of:
firstly, a ceramic membrane filter element with the thickness of 200nm is used, primary fine filtration is carried out under the conditions that the temperature is 40-50 ℃ and the pressure is 10-20 bar, and then an ultrafiltration membrane with the molecular weight of 1500-2000 is used, and secondary fine filtration is carried out under the conditions that the temperature is 30-40 ℃ and the pressure is 20-30 bar.
4. The method of claim 1, wherein the momordica grosvenori glycosides are obtained by fine-filtering and concentrating the momordica grosvenori extract, wherein the step of obtaining the momordica grosvenori glycosides concentrate comprises:
the brix of the momordica grosvenori concentrated solution is 5-10%.
5. The method for preparing mogroside compounds as claimed in claim 1, wherein the mogroside concentrate is used as initial bubbling feed liquid, the pH value and the bubbling gas flow are adjusted, the solution is heated to 50-80 ℃, multi-stage foam separation and purification are performed in a foam separation tower, the foam solution is collected, and then defoaming is performed to obtain the mogroside enriched liquid:
and the pH value is adjusted to 9.0-10.5.
6. The method for preparing mogroside compounds as claimed in claim 1, wherein the mogroside concentrate is used as initial bubbling feed liquid, the pH value and the bubbling gas flow are adjusted, the solution is heated to 50-80 ℃, multi-stage foam separation and purification are performed in a foam separation tower, the foam solution is collected, and then defoaming is performed to obtain the mogroside enriched liquid:
the flow rate of the bubbling gas is as follows: the gas flow rate per min is 1/30-1/20 of the tower volume of the foam separation tower.
7. The method for preparing mogroside compounds as claimed in claim 1, wherein the mogroside concentrate is used as initial bubbling feed liquid, the pH value and the bubbling gas flow are adjusted, the solution is heated to 50-80 ℃, multi-stage foam separation and purification are performed in a foam separation tower, the foam solution is collected, and then defoaming is performed to obtain the mogroside enriched liquid:
the multistage foam separation is 1-3 grades.
8. The method for preparing mogroside compounds as claimed in claim 1, wherein the step of taking the concentrated momordica grosvenori solution as initial bubbling feed liquid, adjusting the pH value and the bubbling gas flow rate, heating the solution to 50-80 ℃, performing multi-stage foam separation and purification in a foam separation tower, collecting the foam solution, and then defoaming to obtain the mogroside enriched solution comprises:
and spraying an ethanol solution with the volume concentration of 90-95% into the foam solution.
9. The method of claim 1, wherein the step of decolorizing, deodorizing and pesticide residue removing the mogroside enriched solution to obtain a mogroside solution comprises:
decolorizing the mogroside enrichment solution with ion exchange resin, collecting effluent, eluting with purified water until no sweet taste exists, and mixing the effluent and the eluate;
and passing the combined effluent and eluent through an active carbon column, deodorizing and removing pesticide residues, collecting the effluent, eluting by using purified water until no sweet taste exists, and combining the effluent and the eluent again to obtain the mogroside solution.
10. The method of claim 1, wherein the step of concentrating the mogroside solution and drying the mogroside solution to a powder form to obtain the mogroside comprises:
and adjusting the pH value of the mogroside solution to 4.0-6.0, then concentrating until the brix is 50-60%, and then carrying out spray drying to obtain the mogroside compound.
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Application publication date: 20211231 |