CN112244185A - Preparation method of sugar-rich flavor fructus momordicae concentrated juice - Google Patents
Preparation method of sugar-rich flavor fructus momordicae concentrated juice Download PDFInfo
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- CN112244185A CN112244185A CN202011089686.8A CN202011089686A CN112244185A CN 112244185 A CN112244185 A CN 112244185A CN 202011089686 A CN202011089686 A CN 202011089686A CN 112244185 A CN112244185 A CN 112244185A
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- 235000000346 sugar Nutrition 0.000 title claims abstract description 39
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 72
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- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
- 101001097860 Lithospermum erythrorhizon Phenylalanine ammonia-lyase 1 Proteins 0.000 description 1
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- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 1
- MUPFEKGTMRGPLJ-RMMQSMQOSA-N Raffinose Natural products O(C[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@@H](O[C@@]2(CO)[C@H](O)[C@@H](O)[C@@H](CO)O2)O1)[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 MUPFEKGTMRGPLJ-RMMQSMQOSA-N 0.000 description 1
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- 241001409305 Siraitia Species 0.000 description 1
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- IAJILQKETJEXLJ-RSJOWCBRSA-N aldehydo-D-galacturonic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-RSJOWCBRSA-N 0.000 description 1
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- 235000003599 food sweetener Nutrition 0.000 description 1
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- PFOARMALXZGCHY-UHFFFAOYSA-N homoegonol Natural products C1=C(OC)C(OC)=CC=C1C1=CC2=CC(CCCO)=CC(OC)=C2O1 PFOARMALXZGCHY-UHFFFAOYSA-N 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
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- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
- A23L2/02—Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof containing fruit or vegetable juices
- A23L2/08—Concentrating or drying of juices
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
- A23L2/72—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration
- A23L2/74—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration using membranes, e.g. osmosis, ultrafiltration
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/49—Removing colour by chemical reaction, e.g. bleaching
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Seasonings (AREA)
- Non-Alcoholic Beverages (AREA)
Abstract
A preparation method of a sugar-rich flavor fructus momordicae concentrated juice comprises the following steps: taking waste liquid generated in the process of preparing the mogroside as a raw material, filtering the waste liquid, carrying out vacuum concentration, carrying out alcohol precipitation, recovering alcohol, carrying out resin decoloration, adjusting the pH value, and carrying out vacuum concentration to obtain the sugar-rich flavor concentrated momordica grosvenori juice. The method has simple process flow and easy control of process parameters, and the used equipment is common and necessary equipment in the industry; the used raw material is waste liquid generated in the production process of the momordica grosvenori glycoside, so that excessive sewage discharge is avoided, the sewage treatment pressure is reduced, and the comprehensive utilization rate of momordica grosvenori resources is improved; harmful solvents, enzyme preparations or other non-natural auxiliary materials or processing aids are not introduced, so that the pure natural characteristic of the product is ensured; the obtained concentrated juice has uniform texture, light yellow to yellowish color, clear and bright color after brewing, fragrant and sweet taste, rich flavor, and unique fresh and fragrant quality of fructus Siraitiae Grosvenorii.
Description
Technical Field
The invention relates to a preparation method of a beverage fructus momordicae juice, in particular to a preparation method of fructus momordicae concentrated juice.
Background
The fructus Siraitiae Grosvenorii is a plant of genus Siraitia of CucurbitaceaeSiraitia grosvenorii(Swingle) C.Jeffery]The mature fruit of (1). The theory of traditional Chinese medicine considers that the medicine has cool nature and sweet taste, has the effects of clearing heat, quenching thirst, moistening lung and relieving cough, and is generally used for treating symptoms such as laryngalgia, aphonia of throat, chronic bronchitis, asthma, constipation and the like. In addition, modern pharmacological research shows that the compound preparation has low toxicity and high safety factor, and has the effects of reducing blood sugar, protecting liver, resisting oxidation, improving the immunity of the organism and the like.
Through research and development for many years, the momordica grosvenori contains a large amount of saccharides (polysaccharides, reducing sugars and the like), protein amino acids, polyphenols, fatty acids, vitamins and the like in addition to the well-known sweetening substances of the cucurbitane triterpenoid glycosides (the percentage of dry fruits is about 4%, and momordica grosvenori sweet glycoside V is a main component). Wherein, the weight of protein amino acid accounts for 8.67-13.35 percent of the weight of dry fruits, most flavonoids are flavonoid glycoside, kaempferol and quercetin are used as main aglycone, and the VC content is as high as 339.68-461.12 mg/100g of fresh fruits. There are studies on[3]It is pointed out that the total sugar content of the dried fructus momordicae is about 25.18-38.15%, the reducing sugar content is about 16.01-32.94%, and the reducing sugar contains glucose and fructose as main components, and the proportion of the fructose is highest (see "analysis of sugar content of fructus momordicae", xu Kun et al, Guangxi agricultural science, 1980, 3 rd edition, page 29). The researchers also detected glucose, fructose, sucrose, raffinose, mannose and other small molecular sugars from the siraitia grosvenorii pulp by high performance liquid chromatography. Further analysis indicates that the sugar components in different momordica grosvenori varieties are consistent and the content is different. The relative content of sucrose and glucose in the freeze-dried fruit is highest, the sucrose and glucose in the dried fruit are reduced, and the relative content of fructose and polysaccharide is increased. In addition, some researchers also separate D-mannitol from fructus momordicae, which can be used as a sweetener, an anti-sticking agent, a quality modifier, a humectant and the like in food, and the sweetness of the D-mannitol is 0.55-0.65 times of that of sucrose, so that the D-mannitol can provide good flavor to the fructus momordicae (see 'analysis of the composition and content of saccharide substances in the pulp of the fructus momordicae', such as 'Wanghai Ying', etc. 'in Guangxi plant' 2015, volume 35, stage 6, page 774 and 780).
In the deep processing of the momordica grosvenori, people generally focus on triterpene glycoside substances, waste liquid for producing the momordica grosvenori glycoside is generally sent to a sewage treatment station or is simply treated and then discharged, other beneficial components in the momordica grosvenori are lost, and the overall value of momordica grosvenori resources cannot be fully applied. Moreover, the environmental problem is becoming urgent, the reasonable and effective treatment of the production sewage becomes inevitable, and the waste liquid rich in organic matters brings serious pressure to the sewage treatment station, which directly leads to the increase of the sewage treatment cost and increases the enterprise cost. For some enterprises without the condition for advanced sewage treatment, the direct discharge of the waste liquid with high COD value can cause the pollution of the surrounding environment, hinder the normal growth activities of animals and plants, seriously destroy the ecological balance and further influence the human health.
The existing preparation process of the momordica grosvenori condensed juice mostly takes fresh momordica grosvenori as raw materials, and the process of preparing the condensed juice by taking momordica grosvenori sweet glycoside column chromatography waste liquid as the raw materials has no marketization application. The recycling of waste liquid from mogroside production is mostly used to separate some single substances such as polysaccharide, pectin, protein or D-mannitol (see separation and identification of mannitol in Grosvenor momordica, Xueshuan et al, Guangxi plant, 1990, 3 rd phase, page 254-.
CN103145869B discloses a method for obtaining a grosvenor momordica fruit extract rich in polysaccharide by carrying out enzymolysis on a sweet glycoside production waste liquid by using pectinase and papain, filtering, sterilizing, carrying out nanofiltration, concentrating and spraying to dry. CN110105458A discloses a method for extracting polysaccharide and D-mannitol from sweet glycoside production wastewater by processes of ultrafiltration, decoloration, gel column chromatography, alcohol precipitation, crystallization and the like. The two components in the waste liquid are separated, and other substances are still discarded as the waste liquid.
CN108813257A discloses a method for obtaining concentrated juice of momordica grosvenori by selecting fresh momordica grosvenori and carrying out the processes of airing, crushing, cooking, filtering and concentrating, wherein the process flow is simple and easy to operate, but the prepared concentrated juice is not uniform, precipitates are easy to generate, and the juice is dark in color after being brewed and is not clear and transparent.
CN107397103A discloses a method for preparing decolorized momordica grosvenori concentrated juice by selecting fresh momordica grosvenori and carrying out flash extraction, centrifugal filtration, enzymolysis, ultrafiltration, decolorization, nanofiltration, concentration, sterilization and other processes. In addition, the enzymolysis process may additionally add other components or change the proportion of the components in the extract, for example, the proportion of galacturonic acid is increased, so that the pH value of the material system is reduced, the taste of the finished product is affected, and the finished product does not have the characteristics of pure nature.
According to the technical scheme disclosed by CN107156563B, fresh momordica grosvenori is also used as a raw material, the process flow comprises 15 steps of saccharification, fruit selection, crushing, percolation extraction, disc centrifugation, 0.45um ceramic membrane microfiltration and the like, and the fresh momordica grosvenori concentrated juice is obtained, although the concentrated juice is good in clarity, light in color and high in quality, the whole process flow is very complicated, the investment of production equipment and labor cost is large, the production period is long, and the actual production cost is extremely high.
CN106923113A discloses a process for producing momordica grosvenori concentrated juice by using waste liquid discharged from momordica grosvenori sweet glycoside adsorption resin column, which comprises the steps of clarifying the waste liquid by 0.45um ceramic membrane, adjusting pH to 5.5-6.5 by anion resin, concentrating by reverse osmosis membrane to 8-10 Brix, decolorizing by resin column, decolorizing by active carbon (using amount is 0.2-0.3%), filtering by plate frame, finely filtering by titanium rod, concentrating by reverse osmosis membrane, cryogenically cooling, clarifying by 0.22um ceramic membrane microfiltration, concentrating under vacuum reduced pressure, sterilizing and the like. In the process, the material is alkaline after the resin column is decolorized, and the decolorization effect under the subsequent alkaline condition of activated carbon is not ideal. And the use of the activated carbon increases the investment of subsequent plate frame and titanium rod fine filtration, and because macromolecular polysaccharide, pectin and protein substances exist in the material, the material is subjected to microfiltration and clarification by using ceramic membranes with different pores, so that the whole process has more investment on equipment, complex working procedures and higher production cost.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a method for preparing the momordica grosvenori condensed juice with rich sugar flavor by utilizing the momordica grosvenori sweet glycoside production waste liquid, which has the advantages of low production cost, good product taste, clear and transparent appearance, so that the utilization rate of momordica grosvenori resources is improved, and the discharge of production sewage is reduced.
The technical scheme adopted for solving the technical problems is that the preparation method of the sugar-rich flavor momordica grosvenori condensed juice comprises the following steps: taking waste liquid generated in the process of preparing the mogroside as a raw material, filtering the waste liquid, carrying out vacuum concentration, carrying out alcohol precipitation, recovering alcohol, carrying out resin decoloration, adjusting the pH value, and then carrying out vacuum concentration.
The preparation method of the sugar-rich flavor fructus momordicae concentrated juice comprises the following specific steps:
(1) preparing raw materials: collecting waste liquid generated in the process of preparing the mogroside;
(2) and (3) filtering: filtering the waste liquid to remove impurities to obtain filtrate;
(3) and (3) vacuum concentration: concentrating the filtrate obtained in the step (2) by using vacuum concentration equipment to obtain a concentrated solution;
(4) alcohol precipitation: adding ethanol into the concentrated solution obtained in the step (3), stirring and adding the ethanol, standing the mixture after uniformly stirring, and centrifuging the mixture; recovering ethanol from the centrifugated clear liquid to obtain centrifugate; centrifuging and precipitating for further separating and purifying polysaccharide, cellulose, pectin or protein;
(5) decoloring and removing impurities: passing the centrifugate obtained in the step (4) through a weak alkaline anion resin column, carrying out decolorization and impurity removal treatment, and collecting effluent liquid; after the centrifugal liquid is loaded on the column, washing with water at the same flow rate, and merging the water washing liquid into the effluent liquid to obtain alkaline destaining liquid;
(6) adjusting the pH value: adjusting the pH value of the decolorized solution obtained in the step (5) through an acidic cation resin column, and collecting an effluent liquid, wherein the pH value of the effluent liquid is acidic to obtain an acidic effluent liquid;
(7) and (3) ultrafiltration: filtering the acidic effluent obtained in the step (6) by using an ultrafiltration membrane, and collecting ultrafiltration permeate;
(8) and (4) vacuum concentration: and (4) carrying out vacuum reduced pressure concentration on the ultrafiltration permeate obtained in the step (7) to obtain the sugar-rich flavor momordica grosvenori concentrated juice.
Further, in the step (1), the raw material for preparing the mogroside can be dry momordica grosvenori or fresh momordica grosvenori;
further, in the step (2), the aperture of the filter membrane used for filtering is 0.6-10 μm, preferably 0.8-2 μm;
further, in the step (3), the temperature of vacuum concentration is less than or equal to 65 ℃; vacuum concentrating until the concentration of the concentrated solution is 20-25 Brix; (detection with an ATAGO PAL-1 model portable glucometer);
further, the vacuum concentration device, in a laboratory, may be a rotary evaporator; in a production workshop, the device can be a single-effect concentrator, a double-effect concentrator, a scraper concentrator or a spherical concentrator.
Further, in the step (4), in the alcohol precipitation system, the volume fraction (V/V) of the ethanol is 70-85%, preferably 78-83%; the standing time is 8-24 h, the temperature is 3-5 ℃, and the optimal temperature is 4 ℃.
Further, in the step (4), the equipment used for centrifugation is centrifugation equipment with a separation factor of 3000-5000. Processing for 15-25 min at 3500-4000 rpm of a desktop centrifuge in a laboratory; and carrying out centrifugal precipitation and alcohol washing for 1-2 times.
Further, in the step (4), alcohol in the centrifugal clear liquid is recovered, and the recovered alcohol is free from alcohol smell until the concentration reaches 8-10 Brix.
Further, in the step (5), the type of the weak base anion resin used for decoloring and impurity removal is one or more of D941, D285, ZG A398 or LSA-700B; the dosage of the used weak-base anion resin is 8-10 times of the weight of dry matters in the material to be decolorized; the height-diameter ratio of the weakly basic anion resin column is 4-6: 1; the flow rate of the material on the column is less than or equal to 1.8BV/h, preferably 1.0-1.5 BV/h.
Further, in the step (5), after the material is loaded on the column, washing the column with water at the same flow rate for 0.8-1.2 h, and merging the water washing liquid into the effluent liquid; the pH value of the destaining solution is 8.0-10.0.
Further, in the step (6), the type of the acidic cation resin is one or more of 001 × 7, 001 × 12, WA-2 or modified 732 resin; the dosage of the acidic cationic resin is 1/6-1/5 of the dosage of the decolorizing resin in the step (5); the height-diameter ratio of the resin column is preferably 3-6: 1.
Further, in the step (6), the flow rate of the decolored solution passing through the acidic cation resin column is 1.5-2.5 BV/h, and after the column feeding is finished, the decolored solution is washed with water at the same flow rate for 0.5-1.0 h; the pH value of the obtained acidic effluent is 5.0-6.0.
Further, in the step (7), the aperture of the ultrafiltration membrane is 5000-10000 Da, and the treatment pressure is 0.1-0.3 Mpa; until the concentration of the permeation solution reaches 0.0 to 0.2 Brix.
Further, in the step (8), the vacuum degree is controlled to be 0.075-0.090 Mpa, the temperature is not more than 65 ℃, and the concentrated solution is concentrated under reduced pressure until the concentration is 65-70 Brix.
The invention adopts an alcohol precipitation process to remove most macromolecular insoluble components in the waste liquid, including polysaccharide, pectin, protein, fiber and the like, and aims to ensure the clarity and excellent taste of the final product; moreover, the use of the ethanol is safe and reliable, and the treatment of the step greatly facilitates the effective implementation of the subsequent process; the ultrafiltration further filters out the residual macromolecular substances in the materials, and ensures the clarity and the uniform texture of the concentrated juice.
The method has simple process flow, easily controlled process parameters and no need of excessive equipment investment, and the used equipment is common and necessary equipment in the industry; because the used raw material is waste liquid generated in the production process of the momordica grosvenori glycoside, excessive sewage discharge is avoided, the sewage treatment pressure is reduced, the comprehensive utilization rate of the momordica grosvenori resource is improved, and the momordica grosvenori glycoside has important revelation significance on the development and application of other plant resources; in addition, harmful solvents, enzyme preparations or other non-natural auxiliary materials or processing aids are not introduced in the whole process of the method, so that the pure natural characteristic of the product is ensured; the obtained concentrated juice has uniform texture, light yellow to yellowish color, clear and bright color after brewing, fragrant and sweet taste, rich flavor, and unique fresh and fragrant quality of fructus Siraitiae Grosvenorii.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
(1) Preparing raw materials: collecting waste liquid generated in the process of preparing mogroside by taking fresh ripe momordica grosvenori fruits as raw materials;
(2) and (3) filtering: filtering the waste liquid by a fine filtering membrane of 0.8 mu m, and filtering to remove impurities to obtain filtrate;
(3) and (3) vacuum concentration: concentrating the filtrate obtained in the step (2) by using vacuum concentration equipment to obtain a concentrated solution with the concentration of 22.3 Brix;
(4) alcohol precipitation: putting 500mL of the concentrated solution obtained in the step (3) into a big beaker, adding absolute ethyl alcohol while stirring, and detecting by an alcohol meter until the alcoholic strength of the system reaches 80%; after uniform stirring, transferring the materials into a refrigerator with the temperature of 4 ℃, standing for 16h, centrifuging for 20min at 3500rpm under a laboratory table centrifuge, and collecting the centrifuged clear liquid; recovering ethanol from the supernatant under reduced pressure, and cooling to room temperature to obtain centrifugate with concentration of 8.7 Brix;
centrifuging and precipitating for further separation and purification of polysaccharide, cellulose, pectin or protein;
(5) decoloring and removing impurities: enabling the centrifugate obtained in the step (4) to pass through a D941 weak-base anion resin column (900 mL of resin is filled, the height-diameter ratio is 4: 1) at the flow rate of 1.0BV/h, carrying out decolorization and impurity removal treatment, and collecting effluent liquid; after the centrifugal liquid is loaded on the column, washing for 1h at the same flow rate, and merging the water washing liquid into the effluent liquid to obtain an alkaline destaining liquid with the pH value of 9.23;
(6) adjusting the pH value: adjusting the pH value of the decolorized solution obtained in the step (5) by passing through a 001X 7 acidic cation resin column at the flow rate of 2.3BV/h (the resin is filled with 155mL, the height-diameter ratio is 3: 1), collecting effluent, washing with water at the same flow rate for 0.5h after the effluent is loaded on the column, and combining the water washing solution and the effluent to obtain an acidic material with the pH value of 5.57;
(7) and (3) ultrafiltration: treating the acidic material obtained in the step (6) by using a 10000Da ultrafiltration system, controlling the pressure to be stable at 0.15Mpa, and collecting an ultrafiltration permeate;
(8) and (4) vacuum concentration: and (4) concentrating the ultrafiltration permeate obtained in the step (7) by using a rotary evaporation concentrator, and controlling the concentration temperature to be less than or equal to 65 ℃ to obtain 59mL of sugar-rich flavor momordica grosvenori concentrated juice.
Through detection, the concentration of the obtained sugar-rich flavor fructus momordicae concentrated juice is 68.5Brix, the content of polyphenol is 1.8%, flavone is 0.05%, polysaccharide is 0.88%, and total sugar is 61.8%. The concentrated solution is light yellow, has uniform and stable texture, is colorless after being brewed, is clear and transparent, has fragrant and sweet taste and has the unique fresh and fragrant flavor of the momordica grosvenori.
Example 2
(1) Preparing raw materials: collecting waste liquid generated in the process of preparing mogroside by taking low-temperature dry fruits of mature momordica grosvenori as raw materials;
(2) and (3) filtering: filtering the waste liquid by a fine filtering membrane of 10 mu m, and filtering to remove impurities to obtain filtrate;
(3) and (3) vacuum concentration: carrying out rotary concentration on the filtrate obtained in the step (2) to obtain a concentrated solution with the concentration of 25 Brix;
(4) alcohol precipitation: putting 300mL of the concentrated solution obtained in the step (3) into a big beaker, adding absolute ethyl alcohol while stirring, and detecting by an alcohol meter until the alcoholic strength of the system reaches 83%; after stirring uniformly, transferring the material into a refrigerator at 4 ℃, standing for 12h, centrifuging for 15min at 3500r under a laboratory table centrifuge, and collecting a centrifuged clear solution; recovering ethanol from the supernatant under reduced pressure, and cooling to room temperature to obtain centrifugate with concentration of 9.2 Brix;
centrifuging and precipitating for further separation and purification of polysaccharide, cellulose, pectin or protein;
(5) decoloring and removing impurities: enabling the centrifugate obtained in the step (4) to pass through a D285 weak base anion resin column (350 mL of resin is filled, the height-diameter ratio is =6: 1) at the flow rate of 1.2BV/h, carrying out decolorization and impurity removal treatment, and collecting effluent liquid; after the centrifugal liquid is loaded on the column, washing for 1h at the same flow rate, and merging the washing liquid into the effluent liquid to obtain an alkaline destaining liquid with the pH value of 9.51;
(6) adjusting the pH value: adjusting the pH value of the decolorized solution obtained in the step (5) by passing through a 001 × 7 acidic cation resin column at the flow rate of 2.0BV/h (65 mL of resin is filled, and the height-diameter ratio =6: 1), collecting effluent, washing with water at the same flow rate for 1.0h after the effluent is loaded on the column, and combining the water washing solution and the effluent to obtain an acidic material with the pH value of 5.24;
(7) and (3) ultrafiltration: treating the acidic effluent obtained in the step (6) by using a 5000Da ultrafiltration system, controlling the pressure to be stable at 0.20Mpa, and collecting an ultrafiltration permeate;
(8) and (4) vacuum concentration: and (4) concentrating the ultrafiltration permeate obtained in the step (7) by using a rotary evaporation concentrator, and controlling the concentration temperature to be less than or equal to 63 ℃ to obtain 32.5mL of sugar-rich flavor momordica grosvenori concentrated juice.
Through detection, the concentration of the obtained sugar-rich flavor fructus momordicae concentrated juice is 67.2Brix, the polyphenol content is 1.3%, the flavone content is 0.02%, the polysaccharide content is 0.72%, and the total sugar content is 57.4%. The concentrated solution is yellowish, has uniform and stable texture, is light yellow after being brewed, is clear and transparent, has fragrant and sweet taste and has the unique flavor of the momordica grosvenori.
Example 3
(1) Preparing raw materials: collecting waste liquid generated in the process of preparing mogroside by taking high-temperature dried fruits of momordica grosvenori as raw materials;
(2) and (3) filtering: filtering the waste liquid by a fine filtering membrane of 2 mu m, and filtering to remove impurities to obtain filtrate;
(3) and (3) vacuum concentration: concentrating the filtrate obtained in the step (2) by using vacuum concentration equipment to obtain a concentrated solution with the concentration of 25 Brix;
(4) alcohol precipitation: putting 300mL of the concentrated solution obtained in the step (3) into a big beaker, adding absolute ethyl alcohol while stirring, and detecting by an alcohol meter until the alcoholic strength of the system reaches 85%; after stirring uniformly, transferring the material into a refrigerator at 4 ℃, standing for 12h, centrifuging for 15min at 3500r under a laboratory table centrifuge, and collecting a centrifuged clear solution; recovering ethanol from the supernatant under reduced pressure, and cooling to room temperature to obtain centrifugate with concentration of 8.4 Brix;
centrifuging and precipitating for further separating and purifying polysaccharide, cellulose, pectin or protein;
(5) decoloring and removing impurities: enabling the centrifugate obtained in the step (4) to pass through a D285 weak-base anion resin column (350 mL of resin is filled, the height-diameter ratio is =6: 1) at the flow rate of 1.0BV/h, carrying out decolorization and impurity removal treatment, and collecting effluent liquid; after the centrifugal liquid is loaded on the column, washing for 1h at the same flow rate, and merging the water washing liquid into the effluent liquid to obtain an alkaline destaining liquid with the pH value of 9.75;
(6) adjusting the pH value: adjusting the pH value of the decolorized solution obtained in the step (5) by passing through a 001 × 12 acidic cation resin column at the flow rate of 2.0BV/h (65 mL of resin is filled, and the height-diameter ratio =6: 1), collecting effluent, washing with water at the same flow rate for 1.0h after the effluent is loaded on the column, and combining the water washing solution and the effluent to obtain acidic effluent with the pH value of 5.32; (7) and (3) ultrafiltration: treating the acidic effluent obtained in the step (6) by using a 5000Da ultrafiltration system, controlling the pressure to be stable at 0.15Mpa, and collecting an ultrafiltration permeate;
(8) and (4) vacuum concentration: and (4) concentrating the ultrafiltration permeate obtained in the step (7) by using a rotary evaporation concentrator, and controlling the concentration temperature to be less than or equal to 65 ℃ to obtain 35mL of sugar-rich flavor momordica grosvenori concentrated juice.
Through detection, the concentration of the obtained sugar-rich flavor fructus momordicae concentrated juice is 65Brix, the polyphenol content is 2.3%, the flavone content is 0.03%, the polysaccharide content is 1.05%, and the total sugar content is 52.7%. The concentrated solution is yellowish brown, has uniform texture, is light brown after being brewed, is clear and transparent, has sweet and slightly bitter taste and has the special flavor of the momordica grosvenori. The whole quality deviation suggests that the waste liquid of the sweet glycoside production which does not adopt the high-temperature dry fruit raw material is used as the raw material of the invention.
Example 4
(1) Preparing raw materials: collecting waste liquid generated in the process of preparing mogroside by taking fresh ripe momordica grosvenori fruits as raw materials;
(2) and (3) filtering: filtering the waste liquid by a fine filtering membrane of 2 mu m, and filtering to remove impurities to obtain filtrate;
(3) and (3) vacuum concentration: concentrating the filtrate obtained in the step (2) by using pilot plant 50L vacuum concentration equipment to obtain a concentrated solution with the concentration of 24.5 Brix;
(4) alcohol precipitation: putting 20L of the concentrated solution obtained in the step (3) into an alcohol precipitation tank, adding an ethanol solution with the volume concentration of 95%, stirring and adding the ethanol solution, and detecting by using an alcohol meter until the alcoholic strength of the system reaches 83%; stopping stirring, starting cooling with chilled water (the temperature of the system is 8-10 ℃), standing for 16h, after finishing alcohol precipitation, centrifuging the material by using a flat plate sedimentation type centrifuge to remove residues, and collecting a centrifuged clear solution; recovering ethanol from the supernatant under reduced pressure by 50L vacuum concentration equipment, cooling to room temperature, and obtaining centrifugate with concentration of 9.7 Brix;
centrifuging and precipitating for further separating and purifying polysaccharide, cellulose, pectin or protein;
(5) decoloring and removing impurities: enabling the centrifugate obtained in the step (4) to pass through a D941 weak-base anion resin column (about 23L of resin is filled, and the height-diameter ratio =5: 1) at the flow rate of 1.0BV/h, carrying out decolorization and impurity removal treatment, and collecting effluent liquid; washing with water at the same flow rate for 1 hr after the centrifugate is applied to the column, and mixing the water eluate with the effluent to obtain alkaline decolorized solution with pH of 9.37;
(6) adjusting the pH value: adjusting the pH value of the decolorized solution obtained in the step (5) through a 001 × 7 acidic cation resin column at the flow rate of 2.5BV/h (the resin is filled with 4.2L, and the height-diameter ratio is =3: 1), collecting effluent, washing the effluent for 1.0h at the same flow rate after the effluent is loaded on the column, and combining the water washing solution and the effluent to obtain acidic effluent with the pH value of 5.65;
(7) and (3) ultrafiltration: treating the acidic effluent obtained in the step (6) by using a 10000Da ultrafiltration system, controlling the pressure to be stable at 0.18Mpa, and collecting an ultrafiltration permeate;
(8) and (4) vacuum concentration: and (4) concentrating the ultrafiltration permeate obtained in the step (7) by using a pilot plant 50L vacuum concentrator, and controlling the concentration temperature to be less than or equal to 60 ℃ to obtain about 3.02kg of sugar-rich flavor momordica grosvenori concentrated juice.
Through detection, the concentration of the obtained sugar-rich flavor fructus momordicae concentrated juice is 68.2Brix, the content of polyphenol is 1.3%, flavone is 0.07%, polysaccharide is 0.28%, and total sugar is 62.5%. The concentrated solution is light yellow, has uniform and stable texture, is colorless after being brewed, is clear and transparent, has fragrant and sweet taste and has the unique fresh and fragrant flavor of the momordica grosvenori.
Claims (10)
1. A preparation method of a sugar-rich flavor fructus momordicae concentrated juice is characterized by comprising the following steps: taking waste liquid generated in the process of preparing the mogroside as a raw material, filtering the waste liquid, carrying out vacuum concentration, carrying out alcohol precipitation, recovering alcohol, carrying out resin decoloration, adjusting the pH value, and then carrying out vacuum concentration.
2. The method for preparing the sugar-enriched flavored fructus momordicae concentrated juice according to claim 1, wherein the method comprises the following steps:
(1) preparing raw materials: collecting waste liquid generated in the process of preparing the mogroside;
(2) and (3) filtering: filtering the waste liquid to remove impurities to obtain filtrate;
(3) and (3) vacuum concentration: concentrating the filtrate obtained in the step (2) by using vacuum concentration equipment to obtain a concentrated solution;
(4) alcohol precipitation: adding ethanol into the concentrated solution obtained in the step (3), stirring and adding the ethanol, standing the mixture after uniformly stirring, and centrifuging the mixture; recovering ethanol from the centrifugated clear liquid to obtain centrifugate; centrifuging and precipitating for further separating and purifying polysaccharide, cellulose, pectin or protein;
(5) decoloring and removing impurities: passing the centrifugate obtained in the step (4) through a weak alkaline anion resin column, carrying out decolorization and impurity removal treatment, and collecting effluent liquid; after the centrifugal liquid is loaded on the column, washing with water at the same flow rate, and merging the water washing liquid into the effluent liquid to obtain alkaline destaining liquid;
(6) adjusting the pH value: adjusting the pH value of the decolorized solution obtained in the step (5) through an acidic cation resin column, and collecting an effluent liquid, wherein the pH value of the effluent liquid is acidic to obtain an acidic effluent liquid;
(7) and (3) ultrafiltration: filtering the acidic effluent obtained in the step (6) by using an ultrafiltration membrane, and collecting ultrafiltration permeate;
(8) and (4) vacuum concentration: and (4) carrying out vacuum reduced pressure concentration on the ultrafiltration permeate obtained in the step (7) to obtain the sugar-rich flavor momordica grosvenori concentrated juice.
3. The method for preparing the concentrated juice of momordica grosvenori with sugar-rich flavor according to claim 2, wherein the pore size of the filter membrane used in the filtering in the step (2) is 0.6 μm to 10 μm, preferably 0.8 μm to 2 μm.
4. The method for preparing the concentrated juice of momordica grosvenori with sugar-rich flavor according to claim 2 or 3, wherein in the step (3), the temperature of vacuum concentration is less than or equal to 65 ℃; vacuum concentrating until the concentration of the concentrated solution is 20-25 Brix.
5. The method for preparing the concentrated juice of momordica grosvenori with sugar-rich flavor according to one of claims 2-4, wherein in the step (4), the volume fraction of ethanol in the ethanol precipitation system is 70-85%, preferably 78-83%; the standing time is 8-24 h, the temperature is 3-5 ℃, and the optimal temperature is 4 ℃.
6. The method for preparing the sugar-enriched flavor fructus momordicae concentrated juice according to one of claims 2 to 5, wherein in the step (4), the equipment used for centrifugation is centrifugation equipment with a separation factor of 3000-5000; and recovering alcohol from the centrifuged clear liquid until no alcohol smell exists, wherein the concentration of the alcohol reaches 8-10 Brix.
7. The method for preparing a concentrated juice of momordica grosvenori having rich sugar flavor according to any one of claims 2 to 6, wherein the weak basic anion resin used for decoloring and decontaminating in step (5) is one or more of D941, D285, ZG A398 or LSA-700B; the dosage of the used weak-base anion resin is 8-10 times of the weight of dry matters in the material to be decolorized; the height-diameter ratio of the resin column is 4-6: 1; the flow rate of the upper column material is less than or equal to1.8BV/h, preferably 1.0-1.5 BV/h; after the material is loaded on the column, washing the column with water at the same flow rate for 0.8-1.2 h, and merging the water washing liquid into the effluent liquid; the pH value of the obtained decolored liquid is 8.0-10.0.
8. The method for preparing a concentrated juice of momordica grosvenori with sugar-rich flavor according to any one of claims 2 to 7, wherein in the step (6), the type of the acidic cationic resin is one or more of 001 x 7, 001 x 12, WA-2 or modified 732 resin; the dosage of the acidic cationic resin is preferably 1/6-1/5 of the dosage of the decolorizing resin in the step (5); the height-diameter ratio of the acidic cation resin column is preferably 3-6: 1, the flow rate of the decoloration solution passing through the acidic cation resin column is 1.5-2.5 BV/h, and after the column feeding is finished, the decoloration solution is washed for 0.5-1.0 h by water at the same flow rate; the pH value of the obtained acidic effluent is 5.0-6.0.
9. The method for preparing the concentrated juice of momordica grosvenori with sugar-rich flavor according to one of claims 2 to 8, wherein in the step (7), the pore diameter of the ultrafiltration membrane is 5000 to 10000Da, and the processing pressure is 0.1 to 0.3 Mpa; until the concentration of the permeation solution reaches 0.0 to 0.2 Brix.
10. The method for preparing the concentrated juice with rich sugar and flavor from momordica grosvenori according to any one of claims 2 to 9, wherein in the step (8), the vacuum degree is controlled to be 0.075 to 0.090Mpa, the temperature is controlled to be less than or equal to 65 ℃, and the concentrated juice is concentrated under reduced pressure until the concentration of the concentrated juice is 65 to 70 Brix.
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