CN113925146B - Debitterized ultrafine shaddock powder and production method and application thereof - Google Patents
Debitterized ultrafine shaddock powder and production method and application thereof Download PDFInfo
- Publication number
- CN113925146B CN113925146B CN202111213278.3A CN202111213278A CN113925146B CN 113925146 B CN113925146 B CN 113925146B CN 202111213278 A CN202111213278 A CN 202111213278A CN 113925146 B CN113925146 B CN 113925146B
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- pulp
- fine
- debitterized
- shaddock
- powder
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Classifications
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- A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
- A23L19/01—Instant products; Powders; Flakes; Granules
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- A—HUMAN NECESSITIES
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- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Molecular Biology (AREA)
- Dispersion Chemistry (AREA)
- Microbiology (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a debitterized ultramicro shaddock powder and a production method and application thereof, wherein the debitterized ultramicro shaddock powder can be prepared by adopting fresh shaddock cut pieces to mechanically pulp, breaking ultrasonic cells, inactivating enzyme for the first time, debitterizing enzyme for the second time, inactivating enzyme for the second time, soaking and extracting, precipitating and separating out and the like, the temperature in the preparation process is low, the loss of nutrient components can be reduced, sodium salt and a thickening agent are added during pulping, part of bitter and astringent can be well removed, and the generation of limonin is prevented; the ultrasonic microwave primary enzyme deactivation can well deactivate and remove limonin D-ring lactone hydrolase in the fruit pulp, and prevent limonin A-ring lactone from being hydrolyzed to generate limonin; then the limonin and naringin can be removed, dried and superfine crushed by the action of debittering enzyme and cholesterol ethanol solution, so as to obtain the superfine powder of the pomelo, and the superfine powder of the pomelo can be used for preparing meal replacement powder, meal replacement bars, beverages and food processing auxiliary materials in the food industry.
Description
Technical Field
The invention relates to the field of food processing, in particular to debitterized ultrafine shaddock powder and a production method and application thereof.
Background
Grapefruit is a plant of the genus Citrus of the family Rutaceae, and is widely distributed in Fujian, jiangxi, guangxi and other provinces. As functional health care fruit, the dietary fiber content of the pomelo pulp and peel is extremely high, and the fiber content in the pomelo peel reaches 18 percent. The number of amino acids in the grapefruit is up to 17, the essential amino acids account for about 50% of the total amino acids, and especially the aspartic acid content is the highest. The grapefruit pulp contains more than 10 trace elements necessary for human bodies, such as magnesium, calcium, copper, iron, aluminum, titanium, manganese, vanadium, phosphorus, chlorine and the like, and the magnesium, the calcium and the copper are higher than those of other fruits; the pomelo peel contains a large amount of dietary fibers, unsaturated fatty acid in the pomelo seeds is 67.42%, and especially linoleic acid content is the greatest, so that the pomelo peel has remarkable effects of protecting cardiovascular diseases, reducing blood cholesterol and the like.
Naringin is a natural dihydroflavonoid compound widely existing in citrus plants of Rutaceae and having high safety, and the extraction amount of flavone in naringin is 70.69mg/g, wherein the naringin has a mass fraction of 64.27% and a bitter taste threshold of about 20ppm. Naringin has antibacterial, antiinflammatory, anticancer, antimutagenic, blood pressure lowering, blood cholesterol lowering, and thrombosis reducing effects.
Limonin compounds are triterpene substances, and are mainly found in various plants of Rutaceae and Meliaceae. The limonin is extracted from the pomelo by Soxhlet method, the maximum extraction rate is 11.36mg/g, and the limonin accounts for 0.40% of the lyophilized extract of the pomelo peel. Studies have shown that the limonin precursor substance limonin a-Lactone (LARL) is gradually glycosylated into a glycoside (LG) by limonin UDP-glucosyltransferase (limoid-UDP-glycosyl Transferases, LGT) during normal fruit ripening, which is not bitter. When the fruits are subjected to external environmental stress such as certain mechanical damage, the limonin A-cyclic lactone can be rapidly converted into limonin with strong bitter taste under the catalysis of limonin D-cyclic lactone hydrolase under the acidic condition.
Because of the influence of limonin, the traditional shaddock powder production mainly adopts the superfine grinding technology to crush pulp, the utilization rate of shaddock peel and shaddock kernel is low, and the produced shaddock powder has large fiber granularity and is difficult to accept by consumers.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides debitterized ultrafine shaddock powder and a production method and application thereof.
In order to achieve the above object, the technical scheme of the present invention is specifically implemented as follows:
a method for producing debitterized ultra-micro shaddock powder comprises the following steps:
step 1): selecting fresh grapefruits, cleaning, cutting into small pieces, adding sodium salt and a thickening agent, mechanically pulping to obtain jelly-like thick crude fruit pulp, and performing ultrasonic cell crushing on the crude fruit pulp to obtain fine fruit pulp;
step 2): adding the fine pulp into an ultrasonic microwave chemical reactor for primary enzyme deactivation treatment, wherein the enzyme deactivation temperature is 50-90 ℃, the ultrasonic frequency is 28-40 KHz, the microwave frequency is 2400-2500 MHz, and the treatment time is 10-50 min;
step 3): adding debittering enzyme into the fine fruit pulp, wherein the enzymolysis temperature is 45-60 ℃ and the enzymolysis time is 15-120 min;
step 4): adding the fine pulp into an ultrasonic microwave chemical reactor for secondary enzyme deactivation, carrying out vacuum freeze drying on the fine pulp after enzyme deactivation, soaking the fine pulp in 70% ethanol with the volume of 5-15 times after removing water in the pulp, and filtering to obtain a solid product and filtrate;
step 5): heating the filtrate, adding cholesterol ethanol solution gradually in the heating process of the filtrate until precipitation is not separated out, and removing the precipitation in the filtrate;
step 6): mixing the solid product with the filtrate, drying, and micronizing to obtain the superfine powder of fructus Citri Grandis with particle diameter of 0.7-5 μm.
Preferably, in the step 1), the mass ratio of the sodium salt to the grapefruit is 1:5 to 50, sodium salt can be one or more than one of the following: sodium chloride, sodium carbonate, sodium bicarbonate. The sodium chloride is added to form concentration inside and outside the shaddock cells, the concentration inside the cells is lower than the concentration outside the cells according to the permeation principle, the precipitation of water and nutrient substances in the cells can be accelerated, such as plant acid, flavonoid compounds, trace elements and the like, the plant acid can not only enable the fruit pulp to generate sour feel, but also enable the pH value in the fruit pulp to be reduced, and the acidic environment is an important condition for limonin formation, so that the edible alkaline sodium salt sodium carbonate and/or sodium bicarbonate are added to neutralize the plant acid in the fruit pulp, enable the fruit pulp to be neutral or slightly alkaline, remove the sour taste brought by the plant acid and prevent further generation of limonin.
Preferably, in the step 1), the mass ratio of the thickener to the grapefruit is 2-3: 10, the thickener may be one or more of the following: beta-cyclodextrin, sodium carboxymethyl cellulose, propylene glycol alginate, sodium alginate and sodium carboxymethyl starch. In the application, the thickening agent not only can increase the viscosity of the fruit pulp, is favorable for carrying out ultrasonic cell crushing and ultrasonic microwave enzyme deactivation treatment in the later stage, but also can be used as a debitterizing accelerator for effectively removing limonin and naringin in the fruit pulp.
Preferably, in the step 1), the frequency of ultrasonic cell pulverization is 20-25 KHz, the pressure is 1-5 MPa, the temperature is 30-50 ℃ and the time is 10-30 min; the grain size of the fine fruit pulp is 1-178 mu m. The ultrasonic cell crushing can further crush the pulp to obtain fine pulp with finer taste, at the moment, the integration level of the grapefruit fiber is low, the cell crushing degree is high, and substances in the cells can be well separated out, so that the method is favorable for further removing bitter components in the later period.
Preferably, in the step 3), the addition amount of the debittering enzyme is 1-5 g/L, and the debittering enzyme can be one or more than one of the following: cellobiase, pectinase, cellulase, naringinase, globus hystericus, and Pseudomonas.
Preferably, in the step 4), the fine pulp is pre-cooled for 2-8 hours in an environment of minus 20 ℃ to minus 120 ℃ before vacuum freeze drying, and the pre-cooled pulp is placed in a freeze dryer for vacuum freeze drying for 12-36 hours, wherein the vacuum degree is 5-15 Pa, and the drying temperature is minus 36 ℃ to minus 60 ℃. Vacuum freeze drying can dehydrate fruit pulp at lower temperature, and can prevent nutrition loss and taste change caused by high temperature drying.
Alternatively, in the step 4), the pulp is dehydrated and then immersed in 70% ethanol for 0.5-10 hours, and the solid product and the filtrate are obtained by filtering with filter paper.
Preferably, in the step 5), the filtrate is heated by a constant temperature water bath at a temperature of 35-50 ℃ and the concentration of the cholesterol ethanol solution is 3.5-5.2 mmol/L. Dropping cholesterol ethanol solution into the filtrate, reacting naringin, limonin and cholesterol to generate insoluble molecular compound, filtering to remove naringin and limonin.
Preferably, in the step 5), the cholesterol powder is added into 70% ethanol of 10 times volume, and heated and refluxed for 1 hour to obtain a cholesterol ethanol solution.
The debittered ultrafine shaddock powder is prepared by adopting the debittered ultrafine shaddock powder production method.
Preferably, the debittered ultra-micro shaddock powder is applied to the food industry.
Preferably, the debitterized ultrafine shaddock powder is used for preparing meal replacement powder, meal replacement bars, beverages and food processing auxiliary materials.
The invention has the beneficial effects that:
compared with the prior art, the method for producing the debitterized ultrafine shaddock powder can realize that the whole shaddock is prepared into the debitterized ultrafine shaddock powder, and the debitterized ultrafine shaddock powder is prepared by adopting fresh shaddock dicks through the steps of mechanical pulping, ultrasonic cell disruption, primary enzyme deactivation, debitterizing by debitterizing enzyme, secondary enzyme deactivation, dipping extraction, precipitation and the like, the temperature in the preparation process is low, the loss of nutrient components can be reduced, sodium salt and a thickening agent are added during pulping, part of bitterness can be well removed, and the generation of limonin is prevented; the ultrasonic microwave primary enzyme deactivation can well deactivate and remove limonin D-ring lactone hydrolase in the fruit pulp, and prevent limonin A-ring lactone from being hydrolyzed to generate limonin; then the limonin and naringin can be removed, dried and superfine crushed by the action of debittering enzyme and cholesterol ethanol solution, thus obtaining the superfine pomelo powder.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Unless otherwise indicated, the starting materials and methods employed in the examples of the present invention are those conventionally commercially available in the art and those conventionally used, and the equipment used is conventional in the art.
In the embodiment of the application, the mechanical beating adopts a DRB-32L barrel crusher; the ultrasonic cell crushing adopts a JY99-III ultrasonic continuous flow cell crusher; the ultrasonic microwave chemical reactor adopts an XO-SM series ultrasonic microwave combined reaction system; the vacuum freeze drying adopts TF-FD series experimental freeze dryer; the superfine grinding adopts a WF-18 superfine grinder; the funnel for filtering adopts a buchner funnel, and the filter paper adopts flat spreading.
Example 1
A method for producing debitterized ultra-micro shaddock powder comprises the following steps:
step 1): selecting fresh grapefruits, cleaning, cutting into small pieces, adding sodium salt and a thickening agent, then mechanically pulping to obtain colloidal and sticky crude fruit pulp, carrying out ultrasonic cell crushing on the crude fruit pulp, wherein the frequency of ultrasonic cell crushing is 24KHz, the pressure is 5MPa, the temperature is 42-45 ℃, the time is 15min, and the particle size is 1-178 mu m; the size of the cut pieces meets the pulping requirement, the sodium salt is formed by mixing sodium chloride and sodium bicarbonate in a mass ratio of 1:1.5, and the mass ratio of the sodium salt to the grapefruit is 1:8, 8; the thickener is formed by mixing beta-cyclodextrin and propylene glycol alginate in a mass ratio of 2:1, and the mass ratio of the thickener to the grapefruit is 2:10;
step 2): adding the fine pulp into an ultrasonic microwave chemical reactor for primary enzyme deactivation, wherein the enzyme deactivation temperature is 60 ℃, the ultrasonic frequency is 32KHz, the microwave frequency is 2450MHz, and the treatment time is 35min;
step 3): adding 3g/L debittering enzyme into the fine fruit pulp, wherein the enzymolysis temperature is 48-55 ℃ and the enzymolysis time is 90min; the debittering enzyme is formed by mixing cellobiase and naringinase according to a mass ratio of 1:2;
step 4): adding the fine pulp into an ultrasonic microwave chemical reactor for secondary enzyme deactivation, carrying out vacuum freeze drying on the fine pulp subjected to enzyme deactivation for 12 hours, wherein the vacuum degree is 10Pa, the drying temperature is-48 ℃, soaking the fine pulp in 70% ethanol with the volume of 12 times of that of the fine pulp for 2 hours after removing the water in the pulp, and filtering with filter paper to obtain a solid product and filtrate; the fine fruit pulp is placed in an environment of minus 20 ℃ to minus 30 ℃ for precooling for 6 hours before vacuum freeze drying;
step 5): heating the filtrate in a constant-temperature water bath at 45 ℃, gradually adding 4mmol/L cholesterol ethanol solution in the filtrate heating process until precipitation is not separated out, and filtering to remove the precipitate in the filtrate;
step 6): mixing the solid product with the filtrate, vacuum freeze-drying, and superfine pulverizing to obtain the superfine powder of the grapefruit with the particle size of 0.7-5 μm.
Example 2
A method for producing debitterized ultra-micro shaddock powder comprises the following steps:
step 1): selecting fresh grapefruits, cleaning, cutting into small pieces, adding sodium salt and a thickening agent, then mechanically pulping to obtain colloidal and sticky crude fruit pulp, carrying out ultrasonic cell crushing on the crude fruit pulp, wherein the frequency of ultrasonic cell crushing is 25KHz, the pressure is 3MPa, the temperature is 45-50 ℃, the time is 20min, and the particle size is 1-178 mu m; the size of the cut pieces meets the pulping requirement, the sodium salt is formed by mixing sodium chloride, sodium carbonate and sodium bicarbonate in a mass ratio of 1.2:1:1, and the mass ratio of the sodium salt to the grapefruit is 1:15; the thickener is formed by mixing sodium carboxymethyl cellulose, sodium alginate and sodium carboxymethyl starch in a mass ratio of 1:1:1, and the mass ratio of the thickener to the grapefruit is 3:10;
step 2): adding the fine pulp into an ultrasonic microwave chemical reactor for primary enzyme deactivation, wherein the enzyme deactivation temperature is 55 ℃, the ultrasonic frequency is 40KHz, the microwave frequency is 2500MHz, and the treatment time is 25min;
step 3): adding 2.5g/L debittering enzyme into the fine fruit pulp, wherein the enzymolysis temperature is 55-60 ℃ and the enzymolysis time is 70min; the debittering enzyme is formed by mixing cellobiase, pseudomonas and naringinase according to a mass ratio of 1:1:1;
step 4): adding the fine pulp into an ultrasonic microwave chemical reactor for secondary enzyme deactivation, carrying out vacuum freeze drying on the fine pulp subjected to enzyme deactivation for 15 hours, wherein the vacuum degree is 15Pa, the drying temperature is-36 ℃, soaking the fine pulp in 70% ethanol with 15 times of the volume of the pulp for 1.5 hours after removing the water in the pulp, and filtering by filter paper to obtain a solid product and filtrate; the fine fruit pulp is placed in an environment of minus 40 ℃ to minus 50 ℃ for precooling for 5 hours before vacuum freeze drying;
step 5): heating the filtrate in a constant-temperature water bath at 35 ℃, gradually adding 5mmol/L cholesterol ethanol solution in the filtrate heating process until precipitation is not separated out, and filtering to remove the precipitate in the filtrate;
step 6): mixing the solid product with the filtrate, vacuum freeze-drying, and superfine pulverizing to obtain the superfine powder of the grapefruit with the particle size of 0.7-5 μm.
Example 3
A method for producing debitterized ultra-micro shaddock powder comprises the following steps:
step 1): selecting fresh grapefruits, cleaning, cutting into small pieces, adding sodium salt and a thickening agent, then mechanically pulping to obtain colloidal and sticky crude fruit pulp, carrying out ultrasonic cell crushing on the crude fruit pulp, wherein the frequency of ultrasonic cell crushing is 25KHz, the pressure is 1MPa, the temperature is 45-50 ℃, the time is 30min, and the particle size is 1-178 mu m; the size of the cut pieces meets the pulping requirement, the sodium salt is formed by mixing sodium chloride and sodium carbonate in a mass ratio of 1:1.3, and the mass ratio of the sodium salt to the grapefruit is 1:12; the thickener is formed by mixing beta-cyclodextrin, sodium carboxymethyl cellulose and propylene glycol alginate in a mass ratio of 1:1:1, and the mass ratio of the thickener to the grapefruit is 3:10;
step 2): adding the fine pulp into an ultrasonic microwave chemical reactor for primary enzyme deactivation treatment, wherein the enzyme deactivation temperature is 65 ℃, the ultrasonic frequency is 32KHz, the microwave frequency is 2500MHz, and the treatment time is 28min;
step 3): adding 1g/L debittering enzyme into the fine fruit pulp, wherein the enzymolysis temperature is 55-60 ℃ and the enzymolysis time is 120min; the debittering enzyme is prepared by mixing cellobiase, nodular cast iron enzyme, naringinase and pectase according to a mass ratio of 2:1:2:1;
step 4): adding the fine pulp into an ultrasonic microwave chemical reactor for secondary enzyme deactivation, carrying out vacuum freeze drying on the fine pulp subjected to enzyme deactivation for 20 hours, wherein the vacuum degree is 8Pa, the drying temperature is-55 ℃, soaking the fine pulp in 70% ethanol with the volume of 11 times of that of the fine pulp for 8 hours after removing the water in the pulp, and filtering with filter paper to obtain a solid product and filtrate; the fine pulp is placed in an environment of minus 60 ℃ to minus 65 ℃ for precooling for 2 hours before vacuum freeze drying;
step 5): heating the filtrate in a constant-temperature water bath at 50 ℃, sequentially adding 4.6mmol/L cholesterol ethanol solution in the filtrate heating process until precipitation is not separated out, and filtering to remove the precipitate in the filtrate;
step 6): mixing the solid product with the filtrate, vacuum freeze-drying, and superfine pulverizing to obtain the superfine powder of the grapefruit with the particle size of 0.7-5 μm.
Example 4
A method for producing debitterized ultra-micro shaddock powder comprises the following steps:
step 1): selecting fresh grapefruits, cleaning, cutting into small pieces, adding sodium salt and a thickening agent, then mechanically pulping to obtain colloidal and sticky crude fruit pulp, carrying out ultrasonic cell crushing on the crude fruit pulp, wherein the frequency of ultrasonic cell crushing is 22KHz, the pressure is 4.5MPa, the temperature is 30-35 ℃ and the time is 22min, and obtaining fine fruit pulp with the particle size of 1-178 mu m; the size of the cut pieces meets the pulping requirement, the sodium salt is formed by mixing sodium chloride, sodium carbonate and sodium bicarbonate in a mass ratio of 1:1:1, and the mass ratio of the sodium salt to the grapefruit is 1:18; the thickener is beta-cyclodextrin, and the mass ratio of the thickener to the grapefruit is 2:10;
step 2): adding the fine pulp into an ultrasonic microwave chemical reactor for primary enzyme deactivation, wherein the enzyme deactivation temperature is 80 ℃, the ultrasonic frequency is 28KHz, the microwave frequency is 2400MHz, and the treatment time is 50min;
step 3): adding 5g/L debittering enzyme into the fine fruit pulp, wherein the enzymolysis temperature is 45-50 ℃ and the enzymolysis time is 100min; the debittering enzyme is formed by mixing cellobiase, naringinase and globose stalk enzyme according to a mass ratio of 1:1:1;
step 4): adding the fine pulp into an ultrasonic microwave chemical reactor for secondary enzyme deactivation, carrying out vacuum freeze drying on the fine pulp subjected to enzyme deactivation for 24 hours, wherein the vacuum degree is 10Pa, the drying temperature is-60 ℃, soaking the fine pulp in 70% ethanol with the volume of 12 times of that of the fine pulp for 5 hours after removing the water in the pulp, and filtering with filter paper to obtain a solid product and filtrate; the fine fruit pulp is placed in an environment of minus 30 ℃ to minus 40 ℃ for precooling for 6 hours before vacuum freeze drying;
step 5): heating the filtrate in a constant-temperature water bath at a temperature of 42 ℃, sequentially adding 3.8mmol/L cholesterol ethanol solution in the filtrate heating process until precipitation is not separated out, and filtering to remove the precipitate in the filtrate;
step 6): mixing the solid product with the filtrate, vacuum freeze-drying, and superfine pulverizing to obtain the superfine powder of the grapefruit with the particle size of 0.7-5 μm.
Comparative example 1: the preparation method of the debitterized ultra-micro shaddock powder is adopted to obtain the debitterized ultra-micro shaddock powder, and the preparation method is different from the preparation method of the embodiment 1 in the following points: no sodium salt was added in step 1).
Comparative example 2: the preparation method of the debitterized ultra-micro shaddock powder is adopted to obtain the debitterized ultra-micro shaddock powder, and the preparation method is different from the preparation method of the embodiment 1 in the following points: the operation of step 2) is not performed.
Comparative example 3: a method for producing debitterized ultra-micro shaddock powder comprises the following steps:
step 1): selecting fresh grapefruits, cleaning, cutting into small pieces, adding sodium salt and a thickening agent, then mechanically pulping to obtain colloidal and sticky crude fruit pulp, carrying out ultrasonic cell crushing on the crude fruit pulp, wherein the frequency of ultrasonic cell crushing is 24KHz, the pressure is 5MPa, the temperature is 42-45 ℃, the time is 15min, and the particle size is 1-178 mu m; the size of the cut pieces meets the pulping requirement, the sodium salt is formed by mixing sodium chloride and sodium bicarbonate in a mass ratio of 1:1.5, and the mass ratio of the sodium salt to the grapefruit is 1:8, 8; the thickener is formed by mixing beta-cyclodextrin and propylene glycol alginate in a mass ratio of 2:1, and the mass ratio of the thickener to the grapefruit is 2:10;
step 2): adding the fine pulp into an ultrasonic microwave chemical reactor for primary enzyme deactivation, wherein the enzyme deactivation temperature is 60 ℃, the ultrasonic frequency is 32KHz, the microwave frequency is 2450MHz, and the treatment time is 35min;
step 3): adding 3g/L debittering enzyme into the fine fruit pulp, wherein the enzymolysis temperature is 48-55 ℃ and the enzymolysis time is 90min; the debittering enzyme is formed by mixing cellobiase and naringinase according to a mass ratio of 1:2;
step 4): adding the fine pulp into an ultrasonic microwave chemical reactor for secondary enzyme deactivation, carrying out vacuum freeze drying on the fine pulp after enzyme deactivation for 12 hours, wherein the vacuum degree is 10Pa, the drying temperature is-48 ℃, and carrying out superfine grinding after removing the water in the pulp to obtain the grapefruit superfine powder with the particle size of 0.7-5 mu m.
Debittering test
Test sample: selecting 7 freshly picked shaddock (Shatian shaddock in Mei county, guangdong), marking with serial numbers 1-7 respectively, cutting the shaddock into two parts, respectively representing the two parts of the same shaddock with serial numbers +a and +b, obtaining 14 parts of shaddock in total of 1+a-7+a and 1+b-7+b, respectively pulping, vacuum freeze drying and superfine grinding the 7 parts of shaddock in total of 1+a-7+a to prepare 7 parts of the superfine powder of the shaddock before debittering as blank control samples 1-7, preparing the 1+b-4+b in total of 4 parts of shaddock by adopting the debittering superfine shaddock powder production method in the embodiment 1-4 to prepare test samples 1-4, preparing 3 parts of shaddock in total of 5+b-7+b by adopting the debittering superfine shaddock powder production method in the embodiment 1-3 to prepare test samples 5-7, measuring the limonin total of the blank control samples 1-7, and calculating the debittering rate of naringin.
The test method comprises the following steps:
naringin: high performance liquid chromatography was performed with acetonitrile: and (3) filling a chromatographic column with silica gel by using water (22:78), measuring naringin absorbance at 283nm at a flow rate of 1mL/min and a sample injection amount of 10uL at a column temperature of 40 ℃, and substituting the naringin absorbance into standard yeast to obtain naringin content in the solution.
Limonin: high performance liquid chromatography was performed with acetonitrile: water (95:5) is used as a mobile phase, a chromatographic column is filled with H103 macroporous resin, the sample injection amount is 10uL at 220nm with the flow rate of 1mL/min, the absorbance of limonin is measured at the column temperature of 40 ℃, and the limonin content of the solution is obtained after the sample is brought into standard yeast.
test results: as shown in table 1.
Table 1 shows the results of the debittering test
The foregoing is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Various equivalent changes and modifications can be made by those skilled in the art based on the above embodiments, and all equivalent changes or modifications made within the scope of the claims shall fall within the scope of the present invention.
Claims (9)
1. A method for producing debitterized ultrafine shaddock powder is characterized in that: the method comprises the following steps:
step 1): selecting fresh grapefruits, cleaning, cutting into small pieces, adding sodium salt and a thickening agent, mechanically pulping to obtain jelly-like thick crude fruit pulp, and performing ultrasonic cell crushing on the crude fruit pulp to obtain fine fruit pulp;
step 2): adding the fine pulp into an ultrasonic microwave chemical reactor for primary enzyme deactivation treatment, wherein the enzyme deactivation temperature is 50-90 ℃, the ultrasonic frequency is 28-40 KHz, the microwave frequency is 2400-2500 MHz, and the treatment time is 10-50 min;
step 3): adding debittering enzyme into the thin fruit pulp, wherein the enzymolysis temperature is 45-60 ℃, the enzymolysis time is 15-120 min, the debittering enzyme at least comprises naringinase, and the addition amount of the debittering enzyme is 1-5 g/L;
step 4): adding the fine pulp into an ultrasonic microwave chemical reactor for secondary enzyme deactivation, carrying out vacuum freeze drying on the fine pulp after enzyme deactivation, soaking the fine pulp in ethanol solution with the volume of 5-15 times after removing water in the pulp, and filtering to obtain a solid product and filtrate;
step 5): heating the filtrate, adding cholesterol ethanol solution gradually in the heating process of the filtrate until precipitation is not separated out, and removing the precipitation in the filtrate;
step 6): mixing the solid product with the filtrate, drying, and micronizing to obtain the superfine powder of fructus Citri Grandis with particle diameter of 0.7-5 μm.
2. The method for producing debitterized ultra-fine shaddock powder according to claim 1, wherein the method comprises the following steps: in the step 1), the mass ratio of the sodium salt to the grapefruit is 1:5 to 50, sodium salt can be one or more than one of the following: sodium chloride, sodium carbonate, sodium bicarbonate.
3. The method for producing debitterized ultra-fine shaddock powder according to claim 1, wherein the method comprises the following steps: in the step 1), the mass ratio of the thickener to the grapefruit is 2-3: 10, the thickener may be one or more of the following: beta-cyclodextrin, sodium carboxymethyl cellulose, propylene glycol alginate, sodium alginate and sodium carboxymethyl starch.
4. The method for producing debitterized ultra-fine shaddock powder according to claim 1, wherein the method comprises the following steps: in the step 1), the frequency of ultrasonic cell pulverization is 20-25 KHz, the pressure is 1-5 MPa, the temperature is 30-50 ℃ and the time is 10-30 min; the grain size of the fine fruit pulp is 1-178 mu m.
5. The method for producing debitterized ultra-fine shaddock powder according to claim 1, wherein the method comprises the following steps: in the step 4), the fine pulp is pre-cooled for 2-8 hours in an environment of minus 20 ℃ to minus 120 ℃ before vacuum freeze drying, and the pre-cooled pulp is placed in a freeze dryer for vacuum freeze drying for 12-36 hours, wherein the vacuum degree is 5-15 Pa, and the drying temperature is minus 36 ℃ to minus 60 ℃.
6. The method for producing the debitterized ultra-micro shaddock powder according to claim 1, which is characterized in that: in the step 5), the filtrate is heated by adopting a constant-temperature water bath, the heating temperature is 35-50 ℃, and the concentration of the cholesterol ethanol solution is 3.5-5.2 mmol/L.
7. A debitterized ultramicro shaddock powder, which is characterized in that: the debitterized ultra-micro shaddock powder produced by the method according to any one of claims 1 to 6.
8. The use of the debittered ultra-fine grapefruit powder of claim 7 in the food industry.
9. The use of the debittered ultra-micro shaddock powder according to claim 8 in the food industry, wherein: the debitterized ultrafine shaddock powder is used for preparing meal replacement powder, meal replacement bars, beverages and food processing auxiliary materials.
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