CN114365853B - Method for preparing antioxidant dietary fibers in citrus peel residues - Google Patents
Method for preparing antioxidant dietary fibers in citrus peel residues Download PDFInfo
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- CN114365853B CN114365853B CN202210138502.5A CN202210138502A CN114365853B CN 114365853 B CN114365853 B CN 114365853B CN 202210138502 A CN202210138502 A CN 202210138502A CN 114365853 B CN114365853 B CN 114365853B
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- 241000207199 Citrus Species 0.000 title claims abstract description 80
- 235000020971 citrus fruits Nutrition 0.000 title claims abstract description 80
- 235000013325 dietary fiber Nutrition 0.000 title claims abstract description 44
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 34
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000000605 extraction Methods 0.000 claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000004108 freeze drying Methods 0.000 claims abstract description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 114
- 239000000243 solution Substances 0.000 claims description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 73
- 239000007864 aqueous solution Substances 0.000 claims description 30
- 239000001913 cellulose Substances 0.000 claims description 29
- 229920002678 cellulose Polymers 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 29
- 239000000706 filtrate Substances 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 25
- 241001528187 Paliurus Species 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 23
- 238000004321 preservation Methods 0.000 claims description 20
- 241000233779 Cyclocarya paliurus Species 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000010298 pulverizing process Methods 0.000 claims description 17
- 240000000851 Vaccinium corymbosum Species 0.000 claims description 13
- 235000003095 Vaccinium corymbosum Nutrition 0.000 claims description 13
- 235000017537 Vaccinium myrtillus Nutrition 0.000 claims description 13
- 235000021014 blueberries Nutrition 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 10
- 108010059892 Cellulase Proteins 0.000 claims description 9
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- 239000000084 colloidal system Substances 0.000 claims description 9
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- 238000002360 preparation method Methods 0.000 claims description 9
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- 238000005406 washing Methods 0.000 claims description 9
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- 244000000383 Allium odorum Species 0.000 claims description 6
- 238000012545 processing Methods 0.000 abstract description 11
- 235000013365 dairy product Nutrition 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 4
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- 238000009920 food preservation Methods 0.000 abstract description 4
- 235000013376 functional food Nutrition 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract 1
- 235000006708 antioxidants Nutrition 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 9
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- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- JPFCOVZKLAXXOE-XBNSMERZSA-N (3r)-2-(3,5-dihydroxy-4-methoxyphenyl)-8-[(2r,3r,4r)-3,5,7-trihydroxy-2-(4-hydroxyphenyl)-3,4-dihydro-2h-chromen-4-yl]-3,4-dihydro-2h-chromene-3,5,7-triol Chemical compound C1=C(O)C(OC)=C(O)C=C1C1[C@H](O)CC(C(O)=CC(O)=C2[C@H]3C4=C(O)C=C(O)C=C4O[C@@H]([C@@H]3O)C=3C=CC(O)=CC=3)=C2O1 JPFCOVZKLAXXOE-XBNSMERZSA-N 0.000 description 1
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 description 1
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 1
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
- OEIJRRGCTVHYTH-UHFFFAOYSA-N Favan-3-ol Chemical compound OC1CC2=CC=CC=C2OC1C1=CC=CC=C1 OEIJRRGCTVHYTH-UHFFFAOYSA-N 0.000 description 1
- CITFYDYEWQIEPX-UHFFFAOYSA-N Flavanol Natural products O1C2=CC(OCC=C(C)C)=CC(O)=C2C(=O)C(O)C1C1=CC=C(O)C=C1 CITFYDYEWQIEPX-UHFFFAOYSA-N 0.000 description 1
- 108010024636 Glutathione Proteins 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001991 Proanthocyanidin Polymers 0.000 description 1
- 230000002292 Radical scavenging effect Effects 0.000 description 1
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920002770 condensed tannin Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 description 1
- 229940114124 ferulic acid Drugs 0.000 description 1
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 description 1
- 235000001785 ferulic acid Nutrition 0.000 description 1
- QOLIPNRNLBQTAU-UHFFFAOYSA-N flavan Chemical compound C1CC2=CC=CC=C2OC1C1=CC=CC=C1 QOLIPNRNLBQTAU-UHFFFAOYSA-N 0.000 description 1
- 235000011987 flavanols Nutrition 0.000 description 1
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Natural products O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 1
- 150000007946 flavonol Chemical class 0.000 description 1
- 235000011957 flavonols Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 229960003180 glutathione Drugs 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
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- 230000002000 scavenging effect Effects 0.000 description 1
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- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 description 1
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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
- A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING OR TREATMENT THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
- A23C9/156—Flavoured milk preparations ; Addition of fruits, vegetables, sugars, sugar alcohols or sweeteners
-
- A23L3/3562—
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Mycology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for preparing antioxidant dietary fibers in citrus peel residues. The method takes citrus peel residues as raw materials, the citrus peel residues are obtained through freeze drying, low-temperature superfine grinding and other technologies, and then the antioxidant dietary fibers are extracted by dynamic high-pressure microjet treatment, enzymolysis treatment and high-intensity ultrasonic assisted alcohol extraction, and then the antioxidant dietary fiber extract is subjected to vacuum concentration, recrystallization and drying to obtain the antioxidant dietary fibers. The food physical processing technology disclosed by the invention is simple to operate, is nontoxic and harmless, is easy to realize, has high content of the prepared antioxidant dietary fiber, has higher antioxidant activity, has high practical value in dairy products, food preservation and functional foods, and has important practical significance and social value for solving the problem of waste of processing byproducts of agricultural and sideline products.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a method for preparing antioxidant dietary fibers in citrus peel residues.
Background
Citrus is the second largest fruit in china with annual yields exceeding 1.225 million tons. In China, the citrus is still mainly sold, the processing proportion is about 35% and is used for processing and preparing citrus products, however, 40% -50% of peel residues are generated in the processing process, the peel residues are one of main byproducts in the citrus processing process, and contain a large amount of antioxidant dietary fibers, water-soluble antioxidant dietary fibers and other nutrient substances, and the peel residues are used as Chinese medicinal materials and food processing raw materials except a very small part and are treated as wastes in the rest, so that not only is the resource waste caused, but also the economic loss is caused, and serious environmental pollution is caused.
The antioxidant dietary fiber (insoluble antioxidant dietary fiber, IADF) is rich in natural antioxidant components such as flavonoid (anthocyanin, flavan, flavone, flavonol, flavanol), phenolic acid (gallic acid, ferulic acid), condensed tannin (polymerized proanthocyanidin and high molecular weight hydrolyzed tannin), etc. IADF has been proved to have remarkable antioxidant activity, can effectively remove oxygen free radicals in vivo, improve the stability and nutritive value of dairy products, improve the flavor of the dairy products, enable the dairy products to have better taste, and be widely applied to food preservation and functional food research, thereby being a good dietary fiber source. However, the domestic market lacks high quality citrus dietary fiber, and does not form a mass production and consumer market. Therefore, the method for searching the simple and efficient extraction of the antioxidant dietary fiber is favorable for the application of the antioxidant dietary fiber in dairy products, food preservation and functional foods, and has important practical significance and social value for solving the problem of waste of processing byproducts of agricultural and sideline products.
Disclosure of Invention
The invention provides a method for preparing antioxidant dietary fibers in citrus peel residues, which comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: putting the dried citrus peel residues into a colloid mill for crushing;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer;
(4) And (3) enzymolysis treatment: preparing an acetic acid and cellulase aqueous solution, adding the citrus peel residue subjected to dynamic high-pressure microjet treatment into the acetic acid and cellulase aqueous solution, keeping the temperature in a water bath to 45+/-2 ℃, keeping the temperature for 10-15 min, adding an extract of leek-blueberry-cyclocarya paliurus leaves into the solution, adjusting the pH value of the solution to 5.4 by using the acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in the water bath for 3-4 h at the constant temperature of 45+/-2 ℃, cooling to room temperature after the heat preservation is finished, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to obtain concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72%, carrying out alcohol extraction under an ultrasonic environment, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
Further, in the step (2), the crushing time is 10-30 min.
Further, in the step (3), the pressure of the dynamic high-pressure micro-jet homogenizer is 50-200 MPa, and the treatment is carried out for 3-5 times.
Further, the pH value of the aqueous solution of acetic acid and cellulase is 5.4, the mass percentage of cellulase is 3% -4%, and the solvent is water; and adding the citrus peel residues subjected to dynamic high-pressure microjet treatment into the acetic acid and cellulose water solution, wherein the solid-liquid ratio solid/liquid=1 g/20mL.
Further, the preparation method of the leek-blueberry-cyclocarya paliurus leaf extracting solution comprises the following steps: the mass ratio of the Chinese chives leaves is as follows: blueberry pulp: the cyclocarya paliurus leaves=5:1-3:1-2, the leek leaves, the blueberry pulp and the cyclocarya paliurus leaves are weighed, then the leek leaves, the blueberry pulp and the cyclocarya paliurus leaves are mixed and chopped and then mixed with deionized water, and the mass ratio of the mixture to the deionized water is 1:6; the mixture is subjected to water bath constant temperature to 65+/-5 ℃ and heat preservation extraction for 2-3 hours, air cooling is carried out to normal temperature after heat preservation is finished, the mixture is filtered, and the liquid phase is decompressed and concentrated to 1/2 of the volume before concentration, so that the leek-blueberry-cyclocarya paliurus leaf extract is obtained.
Further, the adding mass of the leek-blueberry-cyclocarya paliurus leaf extracting solution is 2-3 times of the mass of the citrus peel residue after dynamic high-pressure micro-jet treatment.
Further, in the step (5), the filter residue is added into the ethanol water solution, wherein the mass ratio of liquid to material is (liquid/material=20-100:1); the ultrasonic power is 200-600W, and the alcohol extraction time is 1-6 h.
The invention has the beneficial effects that: the food physical processing technology disclosed by the invention is simple to operate, is nontoxic and harmless, is easy to realize, has high content of the prepared antioxidant dietary fiber, has higher antioxidant activity, has high practical value in dairy products, food preservation and functional foods, and has important practical significance and social value for solving the problem of waste of processing byproducts of agricultural and sideline products.
Detailed Description
The following is a detailed description of embodiments:
example 1
A method for preparing antioxidant dietary fiber in citrus peel residue comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: pulverizing dried citrus peel residue in colloid mill for 20min;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer, wherein the pressure of the dynamic high-pressure micro-jet homogenizer is 100Mpa, and treating for 4 times;
(4) And (3) enzymolysis treatment: preparing an aqueous solution of acetic acid and cellulose, wherein the pH of the aqueous solution of acetic acid and cellulose is 5.4, the mass percentage of cellulose is 3%, and the solvent is water; adding the citrus peel residue subjected to dynamic high-pressure micro-jet treatment into the acetic acid and cellulose water solution according to the solid-liquid ratio solid/liquid=1 g/20mL, keeping the temperature in a water bath to 45+/-2 ℃, and after keeping the temperature for 10min, adding the leek-blueberry-cyclocarya paliurus leaf extract into the solution, wherein the adding mass of the leek-blueberry-cyclocarya paliurus leaf extract is 2 times of the mass of the citrus peel residue subjected to dynamic high-pressure micro-jet treatment. Adjusting the pH value of the solution to 5.4 by using an acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in a water bath at the constant temperature of 45+/-2 ℃ for 3 hours, cooling to room temperature after the temperature is kept, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to 1/3 of the volume before concentration to obtain a concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72% according to the mass ratio of liquid/material=50:1, carrying out alcohol extraction for 3 hours under an ultrasonic environment, carrying out ultrasonic power of 400W, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to 1/10 of the volume before concentration to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
The preparation method of the leek-blueberry-cyclocarya paliurus leaf extracting solution comprises the following steps: the mass ratio of the Chinese chives leaves is as follows: blueberry pulp: folium cyclocarya paliurus=5:1:1, folium Allii tuberosi, fructus Myrtilli pulp and folium cyclocarya paliurus are weighed, mixed and chopped, and then mixed with deionized water, wherein the mass ratio of the mixture to deionized water is (1:6); and (3) carrying out water bath constant temperature of the mixture to 65+/-5 ℃, carrying out heat preservation and extraction for 2 hours, carrying out air cooling to normal temperature after heat preservation, filtering the mixture, and concentrating the liquid phase under reduced pressure to 1/2 of the volume before concentration to obtain the leek-blueberry-cyclocarya paliurus leaf extract.
Example 2
A method for preparing antioxidant dietary fiber in citrus peel residue comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: pulverizing dried citrus peel residue in colloid mill for 20min;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer, wherein the pressure of the dynamic high-pressure micro-jet homogenizer is 100Mpa, and treating for 4 times;
(4) And (3) enzymolysis treatment: preparing an aqueous solution of acetic acid and cellulose, wherein the pH of the aqueous solution of acetic acid and cellulose is 5.4, the mass percentage of cellulose is 3%, and the solvent is water; adding the citrus peel residue subjected to dynamic high-pressure micro-jet treatment into the acetic acid and cellulose water solution according to the solid-liquid ratio solid/liquid=1 g/20mL, keeping the temperature in a water bath to 45+/-2 ℃, and after keeping the temperature for 10min, adding the leek-blueberry-cyclocarya paliurus leaf extract into the solution, wherein the adding mass of the leek-blueberry-cyclocarya paliurus leaf extract is 2 times of the mass of the citrus peel residue subjected to dynamic high-pressure micro-jet treatment. Adjusting the pH value of the solution to 5.4 by using an acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in a water bath at the constant temperature of 45+/-2 ℃ for 3 hours, cooling to room temperature after the temperature is kept, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to 1/3 of the volume before concentration to obtain a concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72% according to the mass ratio of liquid/material=50:1, carrying out alcohol extraction for 3 hours under an ultrasonic environment, carrying out ultrasonic power of 400W, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to 1/10 of the volume before concentration to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
The preparation method of the leek-blueberry-cyclocarya paliurus leaf extracting solution comprises the following steps: the mass ratio of the Chinese chives leaves is as follows: blueberry pulp: folium cyclocarya paliurus=5:2:1, namely, folium Allii tuberosi, blueberry pulp and cyclocarya paliurus are weighed, mixed and chopped, and then mixed with deionized water, wherein the mass ratio of the mixture to the deionized water is (1:6); and (3) carrying out water bath constant temperature of the mixture to 65+/-5 ℃, carrying out heat preservation and extraction for 2 hours, carrying out air cooling to normal temperature after heat preservation, filtering the mixture, and concentrating the liquid phase under reduced pressure to 1/2 of the volume before concentration to obtain the leek-blueberry-cyclocarya paliurus leaf extract.
Example 3
A method for preparing antioxidant dietary fiber in citrus peel residue comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: pulverizing dried citrus peel residue in colloid mill for 20min;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer, wherein the pressure of the dynamic high-pressure micro-jet homogenizer is 100Mpa, and treating for 4 times;
(4) And (3) enzymolysis treatment: preparing an aqueous solution of acetic acid and cellulose, wherein the pH of the aqueous solution of acetic acid and cellulose is 5.4, the mass percentage of cellulose is 4%, and the solvent is water; adding the citrus peel residue subjected to dynamic high-pressure micro-jet treatment into the acetic acid and cellulose water solution according to the solid-liquid ratio solid/liquid=1 g/20mL, keeping the temperature in a water bath to 45+/-2 ℃, and after keeping the temperature for 15min, adding the leek-blueberry-cyclocarya paliurus leaf extract into the solution, wherein the adding mass of the leek-blueberry-cyclocarya paliurus leaf extract is 3 times of the mass of the citrus peel residue subjected to dynamic high-pressure micro-jet treatment. Adjusting the pH value of the solution to 5.4 by using an acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in a water bath at the constant temperature of 45+/-2 ℃ for 4 hours, cooling to room temperature after the temperature is kept, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to 1/3 of the volume before concentration to obtain a concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72% according to the mass ratio of liquid/material=50:1, carrying out alcohol extraction for 3 hours under an ultrasonic environment, carrying out ultrasonic power of 400W, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to 1/10 of the volume before concentration to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
The preparation method of the leek-blueberry-cyclocarya paliurus leaf extracting solution comprises the following steps: the mass ratio of the Chinese chives leaves is as follows: blueberry pulp: folium cyclocarya paliurus=5:2:2, folium Allii tuberosi, fructus Myrtilli pulp and folium cyclocarya paliurus are weighed, mixed and chopped, and then mixed with deionized water, wherein the mass ratio of the mixture to the deionized water is (1:6); and (3) carrying out water bath constant temperature of the mixture to 65+/-5 ℃, carrying out heat preservation and extraction for 3 hours, carrying out air cooling to normal temperature after heat preservation, filtering the mixture, and concentrating the liquid phase under reduced pressure to 1/2 of the volume before concentration to obtain the leek-blueberry-cyclocarya paliurus leaf extract.
Example 4
A method for preparing antioxidant dietary fiber in citrus peel residue comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: pulverizing dried citrus peel residue in colloid mill for 20min;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer, wherein the pressure of the dynamic high-pressure micro-jet homogenizer is 100Mpa, and treating for 4 times;
(4) And (3) enzymolysis treatment: preparing an aqueous solution of acetic acid and cellulose, wherein the pH of the aqueous solution of acetic acid and cellulose is 5.4, the mass percentage of cellulose is 4%, and the solvent is water; adding the citrus peel residue subjected to dynamic high-pressure micro-jet treatment into the acetic acid and cellulose water solution according to the solid-liquid ratio solid/liquid=1 g/20mL, keeping the temperature in a water bath to 45+/-2 ℃, and after keeping the temperature for 15min, adding the leek-blueberry-cyclocarya paliurus leaf extract into the solution, wherein the adding mass of the leek-blueberry-cyclocarya paliurus leaf extract is 3 times of the mass of the citrus peel residue subjected to dynamic high-pressure micro-jet treatment. Adjusting the pH value of the solution to 5.4 by using an acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in a water bath at the constant temperature of 45+/-2 ℃ for 4 hours, cooling to room temperature after the temperature is kept, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to 1/3 of the volume before concentration to obtain a concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72% according to the mass ratio of liquid/material=50:1, carrying out alcohol extraction for 3 hours under an ultrasonic environment, carrying out ultrasonic power of 400W, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to 1/10 of the volume before concentration to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
The preparation method of the leek-blueberry-cyclocarya paliurus leaf extracting solution comprises the following steps: the mass ratio of the Chinese chives leaves is as follows: blueberry pulp: folium cyclocarya paliurus=5:3:2, namely, folium Allii tuberosi, blueberry pulp and cyclocarya paliurus are weighed, mixed and chopped, and then mixed with deionized water, wherein the mass ratio of the mixture to the deionized water is (1:6); and (3) carrying out water bath constant temperature of the mixture to 65+/-5 ℃, carrying out heat preservation and extraction for 3 hours, carrying out air cooling to normal temperature after heat preservation, filtering the mixture, and concentrating the liquid phase under reduced pressure to 1/2 of the volume before concentration to obtain the leek-blueberry-cyclocarya paliurus leaf extract.
Comparative example 1
A method for preparing dietary fiber comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: pulverizing dried citrus peel residue in colloid mill for 20min;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer, wherein the pressure of the dynamic high-pressure micro-jet homogenizer is 100Mpa, and treating for 4 times;
(4) And (3) enzymolysis treatment: preparing an aqueous solution of acetic acid and cellulose, wherein the pH of the aqueous solution of acetic acid and cellulose is 5.4, the mass percentage of cellulose is 4%, and the solvent is water; and adding the citrus peel residue subjected to the dynamic high-pressure micro-jet treatment into the acetic acid and cellulase water solution according to the solid-liquid ratio solid/liquid=1 g/20mL, keeping the temperature in a water bath to 45+/-2 ℃, and after keeping the temperature for 15min, adding the Chinese chive extract into the solution, wherein the adding mass of the Chinese chive extract is 3 times that of the citrus peel residue subjected to the dynamic high-pressure micro-jet treatment. Adjusting the pH value of the solution to 5.4 by using an acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in a water bath at the constant temperature of 45+/-2 ℃ for 4 hours, cooling to room temperature after the temperature is kept, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to 1/3 of the volume before concentration to obtain a concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72% according to the mass ratio of liquid/material=50:1, carrying out alcohol extraction for 3 hours under an ultrasonic environment, carrying out ultrasonic power of 400W, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to 1/10 of the volume before concentration to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
The preparation method of the Chinese chive extract comprises the following steps: cutting leek leaves, mixing the crushed leek leaves with deionized water, wherein the mass ratio of the leek She Suiding to the deionized water is 1:6; the mixture is subjected to water bath constant temperature to 65+/-5 ℃ and heat preservation extraction for 3 hours, air cooling is carried out to normal temperature after heat preservation is finished, the mixture is filtered, and the liquid phase is decompressed and concentrated to 1/2 of the volume before concentration, so that the Chinese chive extract of the comparative example is obtained.
Comparative example 2
A method for preparing antioxidant dietary fiber in citrus peel residue comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: pulverizing dried citrus peel residue in colloid mill for 20min;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer, wherein the pressure of the dynamic high-pressure micro-jet homogenizer is 100Mpa, and treating for 4 times;
(4) And (3) enzymolysis treatment: preparing an aqueous solution of acetic acid and cellulose, wherein the pH of the aqueous solution of acetic acid and cellulose is 5.4, the mass percentage of cellulose is 4%, and the solvent is water; and adding the citrus peel residue subjected to the dynamic high-pressure micro-jet treatment into the acetic acid and cellulose water solution according to the solid-liquid ratio solid/liquid=1 g/20mL, keeping the temperature in a water bath to 45+/-2 ℃, and after keeping the temperature for 15min, adding a blueberry extract into the solution, wherein the adding mass of the blueberry extract is 3 times that of the citrus peel residue subjected to the dynamic high-pressure micro-jet treatment. Adjusting the pH value of the solution to 5.4 by using an acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in a water bath at the constant temperature of 45+/-2 ℃ for 4 hours, cooling to room temperature after the temperature is kept, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to 1/3 of the volume before concentration to obtain a concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72% according to the mass ratio of liquid/material=50:1, carrying out alcohol extraction for 3 hours under an ultrasonic environment, carrying out ultrasonic power of 400W, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to 1/10 of the volume before concentration to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
The preparation method of the blueberry extract comprises the following steps: cutting blueberry pulp into diced pieces, and mixing the diced pieces with deionized water, wherein the mass ratio of the diced pieces to the deionized water is 1:6; and (3) carrying out heat preservation and extraction on the mixture for 3 hours at the constant temperature of 65+/-5 ℃ in a water bath, carrying out air cooling to normal temperature after heat preservation, filtering the mixture, and concentrating the liquid phase under reduced pressure to 1/2 of the volume before concentration to obtain the blueberry extract of the comparative example.
Comparative example 3
A method for preparing antioxidant dietary fiber in citrus peel residue comprises the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: pulverizing dried citrus peel residue in colloid mill for 20min;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer, wherein the pressure of the dynamic high-pressure micro-jet homogenizer is 100Mpa, and treating for 4 times;
(4) And (3) enzymolysis treatment: preparing an aqueous solution of acetic acid and cellulose, wherein the pH of the aqueous solution of acetic acid and cellulose is 5.4, the mass percentage of cellulose is 4%, and the solvent is water; adding the citrus peel residue subjected to dynamic high-pressure micro-jet treatment into the acetic acid and cellulose water solution according to the solid-liquid ratio solid/liquid=1 g/20mL, keeping the temperature in a water bath to 45+/-2 ℃, and after keeping the temperature for 15min, adding cyclocarya paliurus leaf extract into the solution, wherein the adding mass of the cyclocarya paliurus leaf extract is 3 times of that of the citrus peel residue subjected to dynamic high-pressure micro-jet treatment. Adjusting the pH value of the solution to 5.4 by using an acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in a water bath at the constant temperature of 45+/-2 ℃ for 4 hours, cooling to room temperature after the temperature is kept, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to 1/3 of the volume before concentration to obtain a concentrated solution A;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72% according to the mass ratio of liquid/material=50:1, carrying out alcohol extraction for 3 hours under an ultrasonic environment, carrying out ultrasonic power of 400W, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to 1/10 of the volume before concentration to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
The preparation method of the cyclocarya paliurus leaf extract comprises the following steps: cutting cyclocarya paliurus leaves into diced pieces, and mixing the diced pieces with deionized water, wherein the mass ratio of the diced pieces to the deionized water is 1:6; the mixture is subjected to water bath constant temperature to 65+/-5 ℃ for heat preservation and extraction for 3 hours, air cooling is carried out to normal temperature after heat preservation is finished, the mixture is filtered, and the liquid phase is decompressed and concentrated to 1/2 of the volume before concentration, so that the cyclocarya paliurus leaf extract of the comparative example is obtained.
Example 5
1. The dietary fibers prepared in each of the above examples and comparative examples were each subjected to measurement of oxygen radical scavenging ability, and the results are shown in table 1. The measuring method comprises the following steps: the extracted antioxidant dietary fiber is diluted to a proper concentration and added into a 96-well ELISA plate, 75 mu L of Tris-HCl buffer solution (50 nmol/L, pH=8.3) is added, the mixture is kept stand at 25 ℃ for 10min, 50 mu L of pyrogallic acid solution (1.5 nmol/L, dissolved in 1.0nmol/L of hydrochloric acid) is added for reaction for 5min, the absorbance at 320nm is measured, the total measurement time is 10min, and the measurement is performed every 1 min. The positive control used glutathione instead of sample and the blank control water instead of sample. O (O) 2 The calculation formula of the scavenging activity is as follows:
(wherein. DELTA.A O The/min is the slope of the absorbance curve of the blank group; ΔA S And/min is the slope of the absorbance curve of the sample group. )
2. The dietary fibers prepared in each of the above examples and comparative examples were subjected to determination of total flavonoids and total phenols, respectively: and respectively adopting an aluminum nitrate color development method and a Fulin-eliminating card method, drawing a standard curve by taking rutin and gallic acid mass concentration as an abscissa and a light absorption value as an ordinate to obtain a regression equation, taking a proper amount of sample solution, measuring the light absorption value according to the same operation steps, and respectively calculating the total flavone and total phenol content according to the regression equation. The results are shown in Table 1.
Table 1 antioxidant capacity of dietary fibers described in examples and comparative examples
The foregoing detailed description of the embodiments of the present invention will be provided to those skilled in the art, and the detailed description and the examples should not be construed as limiting the invention.
Claims (6)
1. A method for preparing antioxidant dietary fibers in citrus peel residues is characterized by comprising the following specific steps:
(1) And (3) freeze drying: washing the citrus peel residues with pure water, and drying the citrus peel residues for 24 hours by adopting a freeze dryer;
(2) Low temperature superfine pulverizing: putting the dried citrus peel residues into a colloid mill for crushing;
(3) Dynamic high-pressure micro-jet pretreatment, namely treating the crushed citrus peel residue solution by a dynamic high-pressure micro-jet homogenizer;
(4) And (3) enzymolysis treatment: preparing an acetic acid and cellulase aqueous solution, adding the citrus peel residue subjected to dynamic high-pressure microjet treatment into the acetic acid and cellulase aqueous solution, keeping the temperature in a water bath to 45+/-2 ℃, keeping the temperature for 10-15 min, adding an extract of leek-blueberry-cyclocarya paliurus leaves into the solution, adjusting the pH value of the solution to 5.4 by using the acetic acid aqueous solution with the concentration of 1mol/L, keeping the temperature in the water bath for 3-4 h at the constant temperature of 45+/-2 ℃, cooling to room temperature after the heat preservation is finished, filtering to obtain filtrate and filter residues, and concentrating the filtrate under reduced pressure to obtain concentrated solution A; the preparation method of the leek-blueberry-cyclocarya paliurus leaf extracting solution comprises the following steps: the mass ratio of the Chinese chives leaves is as follows: blueberry pulp: the cyclocarya paliurus leaves=5:1-3:1-2, the leek leaves, the blueberry pulp and the cyclocarya paliurus leaves are weighed, then the leek leaves, the blueberry pulp and the cyclocarya paliurus leaves are mixed and chopped and then mixed with deionized water, and the mass ratio of the mixture to the deionized water is 1:6; the mixture is subjected to water bath constant temperature to 65+/-5 ℃ and heat preservation extraction for 2-3 hours, air cooling is carried out to normal temperature after heat preservation is finished, the mixture is filtered, and the liquid phase is decompressed and concentrated to 1/2 of the volume before concentration, so that the leek-blueberry-cyclocarya paliurus leaf extract is obtained;
(5) High-intensity ultrasonic-assisted alcohol extraction: adding the filter residues into an ethanol water solution with the volume fraction of 72%, carrying out alcohol extraction under an ultrasonic environment, filtering after the alcohol extraction is finished, concentrating the filtrate in vacuum to obtain a concentrated solution B, combining the concentrated solution A and the concentrated solution B, and recrystallizing to obtain the dietary fiber.
2. The method for preparing the antioxidant dietary fiber in citrus peel residue according to claim 1, wherein in the step (2), the pulverizing time is 10-30 min.
3. The method for preparing antioxidant dietary fiber in citrus peel residue according to claim 1, wherein in the step (3), the dynamic high-pressure micro-jet homogenizer pressure is 50MPa to 200MPa, and the treatment is performed 3 to 5 times.
4. The method for preparing the antioxidant dietary fiber in the citrus peel residue according to claim 1, wherein the pH of the aqueous solution of acetic acid and cellulase is 5.4, the mass percentage of cellulase is 3% -4%, and the solvent is water; and adding the citrus peel residues subjected to dynamic high-pressure microjet treatment into the acetic acid and cellulose water solution, wherein the solid-liquid ratio solid/liquid=1 g/20mL.
5. The method for preparing the antioxidant dietary fiber in the citrus peel residue, according to claim 1, wherein the adding mass of the leek-blueberry-cyclocarya paliurus leaf extract is 2-3 times of the mass of the citrus peel residue after dynamic high-pressure micro-jet treatment.
6. The method for preparing antioxidant dietary fiber from citrus peel residue according to claim 1, wherein in the step (5), the filter residue is added into an ethanol aqueous solution at a liquid/material ratio of (liquid/material=20-100:1); the ultrasonic power is 200-600W, and the alcohol extraction time is 1-6 h.
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| CN103585424A (en) * | 2013-11-21 | 2014-02-19 | 华东理工大学 | Method for extracting total flavone from Chinese chive seeds |
| CN110051726A (en) * | 2019-04-16 | 2019-07-26 | 浙江大学 | The preparation method and application of general flavone and total starches in a kind of Qingqian Willow leaf |
| CN110063503A (en) * | 2019-04-29 | 2019-07-30 | 陕西科技大学 | A kind of natural dietary fiber replenishers and preparation method thereof with blood sugar reducing function |
| CN111450160A (en) * | 2020-01-19 | 2020-07-28 | 杭州师范大学 | Method for extracting antioxidant active substance from ugly orange peel |
| WO2020259098A1 (en) * | 2019-06-26 | 2020-12-30 | 浙江大学 | Green preparation method for soluble and insoluble dietary fibers in fruit and vegetable residues |
| CN112316008A (en) * | 2020-10-22 | 2021-02-05 | 燕山大学 | Preparation method of cherry soluble antioxidant dietary fiber/quercetin nano preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103585424A (en) * | 2013-11-21 | 2014-02-19 | 华东理工大学 | Method for extracting total flavone from Chinese chive seeds |
| CN110051726A (en) * | 2019-04-16 | 2019-07-26 | 浙江大学 | The preparation method and application of general flavone and total starches in a kind of Qingqian Willow leaf |
| CN110063503A (en) * | 2019-04-29 | 2019-07-30 | 陕西科技大学 | A kind of natural dietary fiber replenishers and preparation method thereof with blood sugar reducing function |
| WO2020259098A1 (en) * | 2019-06-26 | 2020-12-30 | 浙江大学 | Green preparation method for soluble and insoluble dietary fibers in fruit and vegetable residues |
| CN111450160A (en) * | 2020-01-19 | 2020-07-28 | 杭州师范大学 | Method for extracting antioxidant active substance from ugly orange peel |
| CN112316008A (en) * | 2020-10-22 | 2021-02-05 | 燕山大学 | Preparation method of cherry soluble antioxidant dietary fiber/quercetin nano preparation |
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