CN114514979B - Green method for reducing aflatoxin - Google Patents
Green method for reducing aflatoxin Download PDFInfo
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- CN114514979B CN114514979B CN202011303022.7A CN202011303022A CN114514979B CN 114514979 B CN114514979 B CN 114514979B CN 202011303022 A CN202011303022 A CN 202011303022A CN 114514979 B CN114514979 B CN 114514979B
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- aflatoxin
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- 229930195730 Aflatoxin Natural products 0.000 title claims abstract description 59
- XWIYFDMXXLINPU-UHFFFAOYSA-N Aflatoxin G Chemical compound O=C1OCCC2=C1C(=O)OC1=C2C(OC)=CC2=C1C1C=COC1O2 XWIYFDMXXLINPU-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000005409 aflatoxin Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 98
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 12
- 230000001699 photocatalysis Effects 0.000 claims abstract description 12
- 239000004065 semiconductor Substances 0.000 claims abstract description 9
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000019483 Peanut oil Nutrition 0.000 claims description 24
- 239000000312 peanut oil Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 9
- 239000008157 edible vegetable oil Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 235000005687 corn oil Nutrition 0.000 claims description 4
- 239000002285 corn oil Substances 0.000 claims description 4
- 239000002135 nanosheet Substances 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 4
- 239000007966 viscous suspension Substances 0.000 claims description 4
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 238000010345 tape casting Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical group [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 230000009467 reduction Effects 0.000 description 10
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000003053 toxin Substances 0.000 description 8
- 231100000765 toxin Toxicity 0.000 description 8
- 108700012359 toxins Proteins 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 150000002989 phenols Chemical class 0.000 description 4
- 230000027756 respiratory electron transport chain Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 244000105624 Arachis hypogaea Species 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- VCUVETGKTILCLC-UHFFFAOYSA-N 5,5-dimethyl-1-pyrroline N-oxide Chemical compound CC1(C)CCC=[N+]1[O-] VCUVETGKTILCLC-UHFFFAOYSA-N 0.000 description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 description 2
- 235000008692 Carum bulbocastanum Nutrition 0.000 description 2
- 238000004435 EPR spectroscopy Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 2
- 230000003211 malignant effect Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 229930132918 Aflatoxin B2 Natural products 0.000 description 1
- 229930088287 Aflatoxin M2 Natural products 0.000 description 1
- OQLKWHFMUPJCJY-UHFFFAOYSA-N Aflatoxin M2 Chemical compound C1=2C(OC)=CC=3OC4OCCC4(O)C=3C=2OC(=O)C2=C1CCC2=O OQLKWHFMUPJCJY-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000002115 aflatoxin B1 Substances 0.000 description 1
- OQIQSTLJSLGHID-WNWIJWBNSA-N aflatoxin B1 Chemical compound C=1([C@@H]2C=CO[C@@H]2OC=1C=C(C1=2)OC)C=2OC(=O)C2=C1CCC2=O OQIQSTLJSLGHID-WNWIJWBNSA-N 0.000 description 1
- 239000002097 aflatoxin B2 Substances 0.000 description 1
- WWSYXEZEXMQWHT-WNWIJWBNSA-N aflatoxin B2 Chemical compound C=1([C@@H]2CCO[C@@H]2OC=1C=C(C1=2)OC)C=2OC(=O)C2=C1CCC2=O WWSYXEZEXMQWHT-WNWIJWBNSA-N 0.000 description 1
- 229930073161 aflatoxin M1 Natural products 0.000 description 1
- 239000002108 aflatoxin M1 Substances 0.000 description 1
- MJBWDEQAUQTVKK-IAGOWNOFSA-N aflatoxin M1 Chemical compound C=1([C@]2(O)C=CO[C@@H]2OC=1C=C(C1=2)OC)C=2OC(=O)C2=C1CCC2=O MJBWDEQAUQTVKK-IAGOWNOFSA-N 0.000 description 1
- 239000002087 aflatoxin M2 Substances 0.000 description 1
- 229930020125 aflatoxin-B1 Natural products 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- -1 comprises chemical Chemical compound 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002596 lactones Chemical group 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- VVRQVWSVLMGPRN-UHFFFAOYSA-N oxotungsten Chemical group [W]=O VVRQVWSVLMGPRN-UHFFFAOYSA-N 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 229960003742 phenol Drugs 0.000 description 1
- 229940067631 phospholipid Drugs 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000007723 transport mechanism Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 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 COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
- A23L5/273—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption using adsorption or absorption agents, resins, synthetic polymers, or ion exchangers
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/06—Preservation of finished products
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Microbiology (AREA)
- Wood Science & Technology (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a green method for reducing aflatoxin. The method comprises the steps of fully contacting a sample containing aflatoxin with a composite film for reducing aflatoxin, selectively adsorbing and removing the aflatoxin in the sample by the composite film, then placing the composite film under a sunlight or xenon lamp light source for irradiation, and gradually degrading the aflatoxin, wherein the composite film for reducing the aflatoxin comprises a substrate and g-C on the substrate 3 N 4 /WO 3 Composite material, g-C 3 N 4 Is of laminated structure, WO 3 The nano particles are uniformly dispersed in the sheet layer g-C 3 N 4 The surface is tightly combined to form the composite semiconductor photocatalysis material.
Description
Technical Field
The invention belongs to the technical field of food harmful pollutant control, and particularly relates to a green method for reducing aflatoxin.
Background
Edible vegetable oil such as peanut oil, corn oil and the like is rich in unsaturated fatty acid, has good fatty acid composition, and is easy to digest and absorb by human bodies. Peanut oil is also rich in various functional nutrients such as sterols, wheat germ phenol, vitamin E, choline, phospholipids and the like, and is favored by the vast consumers. In recent years, however, media report the event that aflatoxin in a plurality of edible vegetable oils exceeds standard, and the aflatoxin in the edible oils is out of standard mainly because individuals or enterprises are in the process of purchasing peanuts and because the earthnuts are not tightly closed or the storage conditions after harvest are limited, the earthnuts and corn raw materials polluted by the toxins are processed. Aflatoxins have potent carcinogenicity and are identified by the international organization for cancer as class i carcinogens. The toxic and malignant events of people and livestock caused by overstepping of aflatoxin occur at home and abroad, and the toxic and malignant events become important factors for restricting the consumption safety and the industrial development. Therefore, how to safely and efficiently remove aflatoxin and ensure the life health and the consumption safety of consumers becomes a focus of current attention, and is a difficulty of interest of researchers in various countries.
At present, the detoxification and attenuation of aflatoxin mainly comprises chemical, physical, biological and other methods, and the chemical method generally uses a strong oxidant to destroy the structure of aflatoxin, but at the same time, the flavor or nutrient substances in food or grease can be influenced; the physical method has water washing or adsorption, but the molecular structure of the toxin is not changed, and secondary pollution can be caused when the toxin exists in the environment; the biological method has the characteristics of high efficiency, high selectivity and the like, but needs more objective theoretical data support in the aspects of large-scale application and safety evaluation. Therefore, from the viewpoint of high quality development, a novel, energy-saving and green aflatoxin reduction technology is a great need for the development of the industry at present.
Disclosure of Invention
The invention aims to provide a green reduction method of aflatoxin. The method is used for reducing aflatoxin, has the characteristics of green, high efficiency and safety, and does not influence the nutritional functional components in the sample, such as phenol substances containing benzene ring structures, which are similar to the benzene ring structures of the aflatoxin.
The method for reducing aflatoxin comprises the steps of fully contacting a sample containing aflatoxin with a composite film for reducing aflatoxin, selectively adsorbing and removing the aflatoxin in the sample by the composite film, then placing the composite film under a sunlight or xenon lamp light source for irradiation, and gradually degrading the aflatoxin, wherein the composite film for reducing the aflatoxin comprises a substrate and g-C on the substrate 3 N 4 /WO 3 Composite material, g-C 3 N 4 Is of laminated structure, WO 3 The nano particles are uniformly dispersed in the sheet layer g-C 3 N 4 The surface is tightly combined to form the composite semiconductor photocatalysis material.
According to the scheme, g-C 3 N 4 /WO 3 WO in composite materials 3 The mass ratio of (2) is 5-20%; WO (WO) 3 The nano particles have uniform size, about 10nm and g-C 3 N 4 The size of the sheet layer is 100-200nm.
According to the scheme, the substrate is ITO glass or fluorine-doped SnO 2 Conductive glass FTO.
According to the scheme, the wavelength of the xenon lamp light source is 420-700 nm.
According to the scheme, the method for contacting the sample containing the aflatoxin with the composite film comprises the following steps: fixing the composite film on a production line, and enabling a sample to slowly flow through the composite film in the production process to be in contact with the composite film; or fixing the composite film on the blade of the propeller type stirrer, placing the composite film into a container for storing samples, stirring and contacting, and convenient operation.
According to the scheme, the sample is edible vegetable oil, including peanut oil, corn oil and the like which are easy to be polluted by aflatoxin.
Providing the composite film for reducing aflatoxin, comprising a substrate and g-C on the substrate 3 N 4 /WO 3 Composite material, g-C 3 N 4 Is of laminated structure, WO 3 The nano particles are uniformly dispersed in the sheet layer g-C 3 N 4 The surface is tightly combined to form the composite semiconductor photocatalysis material.
According to the scheme, the methodComposite material WO 3 /g-C 3 N 4 WO in 3 The mass proportion of (2) is 5-20wt%, preferably 5-15 wt%, more preferably 10%, WO 3 The nano particles have uniform size, about 10nm and g-C 3 N 4 The size of the sheet layer is 100-200nm.
According to the scheme, the substrate is ITO glass or fluorine-doped SnO 2 Conductive glass FTO.
The preparation method of the composite film material capable of selectively adsorbing and utilizing visible light to catalyze and reduce aflatoxin is provided:
1) Firstly, preparing carbon nitride by a high-temperature pyrolysis method, peeling at a high temperature, and performing aftertreatment to obtain carbon nitride nano-sheets;
2) Dispersing carbon nitride nano-sheets in water, stirring, ultrasonic dispersing, adding a certain amount of sodium tungstate, stirring for dissolving, adding acid, converting sodium tungstate into precipitate, centrifuging to obtain yellow precipitate, cleaning, adding acid, adjusting pH value to 1.2-1.5, placing in a reaction kettle, and performing hydrothermal reaction at 180-200 ℃ to prepare WO 3 /g-C 3 N 4 A composite material;
3) Adding water to disperse the composite material, adding an organic solvent, fully grinding to obtain a uniform and viscous suspension, then dripping the suspension on a substrate for natural tape casting to form a film, and calcining, fixing and sintering under the protection of inert gas to enable the composite material to be combined with the substrate more tightly, thus preparing the aflatoxin-reducing composite film.
According to the scheme, the preparation of the carbon nitride by the pyrolysis method in the step 1) comprises the following steps: urea and dicyandiamide are mixed according to the mass ratio of 1: 2-3 are dissolved in distilled water at 50-60 ℃, placed in an oven for recrystallization, after being evenly ground, placed in a crucible, capped, then placed in a tube furnace or a muffle furnace, heated to 550-560 ℃ and kept for 3-4 hours;
the high-temperature stripping temperature is 580-600 ℃, and the stripping time is kept for 2-3 hours.
The post-treatment is as follows: grinding, respectively cleaning with dilute nitric acid and ethanol solution for three times, and oven drying to obtain carbon nitride powder.
The hydrothermal time in the step 2) is 24-30h. The post-treatment is as follows: centrifuging to obtain yellow solid substances, respectively washing with ethanol and distilled water for three times, and oven drying for use;
step 3) weighing 1.0-2.0g of composite photocatalytic material, dissolving in 20-30mL of distilled water, performing ultrasonic dispersion, adding 3-5mL of dimethylformamide or methanol, fully grinding to uniform and viscous suspension, dripping the suspension on an ITO glass sheet, naturally casting to form a film, and adding inert gas N 2 Under the protection, calcining, fixing and sintering are carried out at 300-350 ℃ to ensure that the composite filter membrane is combined more tightly, thus preparing the aflatoxin-reducing composite membrane.
The invention uses the method of g-C 3 N 4 Nanoplatelets, WO 3 The composite film composed of the nano particles and the ITO glass is used for reducing aflatoxins including aflatoxin B1, aflatoxin B2, aflatoxin M1, aflatoxin M2 and the like, and has excellent selective adsorption and visible light catalytic performance, and specifically: on the one hand, based on pi-pi stacking effect of an aromatic conjugated structure in graphite-type carbon nitride and a benzene ring in an aflatoxin structure, on the other hand, an oxygen lone pair electron on a lactone ring in the aflatoxin structure forms a coordination bond with a tungsten atom 5d empty orbit, and the excellent capability of selectively adsorbing and removing aflatoxin can be realized by mainly utilizing the cooperative adsorption performance of two materials, so that the aim of high-selectivity adsorption is fulfilled; the composite film can adsorb aflatoxin and does not influence the nutritional functional components in a sample system, such as phenols containing benzene ring structures, which are similar to the benzene ring structures of aflatoxin. In addition, the composite film also has excellent visible light catalytic activity, the Z-shaped semiconductor composite material is formed by two semiconductor catalysts of carbon nitride and tungsten oxide, the Z-shaped semiconductor composite material has strong reducing capability and oxidation capability, and under the excitation of visible light, a large number of active groups such as hydroxyl free radicals and superoxide free radicals are generated, aflatoxin is gradually reduced, and finally CO is mineralized 2 And H 2 And O, the toxin is prevented from entering the environment or a food chain, and secondary pollution is avoided. Therefore, the composite film based on the principle has excellent selective adsorption and photocatalysis performance, and can safely and efficiently reduce aflatoxin in a sample.
Briefly, the present invention is directed toThrough the combination of visible light catalysis and selective adsorption technology, aflatoxin is removed by selective adsorption to achieve 'reduction', then the composite film is placed in sunlight or xenon lamp light source for irradiation, based on the excellent visible light catalytic activity of the composite film, carbon nitride and tungsten oxide form a Z-type semiconductor composite material, the Z-type semiconductor composite material has strong reducing capability and oxidation capability, the toxin is gradually degraded, and the final product is CO 2 And H 2 O achieves 'eliminating', thereby realizing the green and high-efficiency technical safety for reducing aflatoxin in the sample.
The composite film prepared by the invention has good performance of reducing aflatoxin in the middle, and is used as AFB 1 Initial concentration of 16.8ppb,10% WO 3 /g-C 3 N 4 (WO 3 ：g-C 3 N 4 After one-time filtration of the composite filter membrane with the mass ratio of 10 percent, the aflatoxin reduction rate is 92.2 percent, and the composite membrane can be recycled, has the advantages of good economy, energy conservation, green, high efficiency, no secondary pollution and the like, and is expected to be used for AFB in samples such as peanut oil, corn oil and the like 1 The toxin is controlled and removed, and a new path is provided for guaranteeing the consumption safety and the industrial development of edible vegetable oil such as peanut oil.
Drawings
FIG. 1 is an electron diffraction XRD pattern of the composite developed in example 1;
FIG. 2 is a TEM image of the composite material developed in example 1;
FIG. 3 is an AFM spectrum of a composite filter membrane developed in example 1;
FIG. 4 is a graph of AFB in peanut oil depleted by composite filter membrane of example 2 1 Performance;
FIG. 5 is a graph of AFB reduction in peanut oil by composite filter membrane reuse of example 2 1 An effect map;
FIG. 6 is a graph of the effect of a composite filter on total phenol content in peanut oil.
FIG. 7 is a graph of ESR test hydroxyl radical profile and Z-type formal electron transport mechanism for a composite filter;
Detailed Description
Example 1: development of composite filter membrane
Dissolving 5.0g of urea and 10.0g of dicyandiamide in distilled water at 50 ℃, placing the mixture in an oven for recrystallization, placing the mixture in a crucible after uniform crystallization and grinding, capping, placing the crucible in a tube furnace or a muffle furnace, heating to 550 ℃ at a heating speed of 5 DEG/min, keeping for 3 hours, heating to 580 ℃, keeping for 2 hours, carrying out high-temperature stripping to obtain yellow powder, grinding, respectively cleaning with dilute nitric acid and ethanol solution for three times, and drying to obtain carbon nitride powder. Dispersing 1.0g of carbon nitride in 100mL of distilled water, stirring, performing ultrasonic dispersion, adding a certain amount of sodium tungstate, stirring for dissolution, adding hydrochloric acid solution, adjusting the pH value to 1.2, centrifuging to obtain precipitate, washing with ethanol and distilled water, adding nitric acid solution, placing in a reaction kettle, performing hydrothermal treatment at 200 ℃ for 24 hours, separating and centrifuging to obtain yellow solid substances, washing with ethanol and distilled water for three times respectively, and drying at 60 ℃ for standby to obtain a composite material (composite material WO) 3 /g-C 3 N 4 WO in 3 5%,10%,15%, 20%) by mass.
Weighing 2.0g of composite photocatalytic material, dissolving in 20mL of distilled water, uniformly dispersing by ultrasonic for 30min, adding 5mL of dimethylformamide, fully grinding to obtain uniform and viscous suspension, casting the suspension on ITO glass plates (20 cm multiplied by 20 cm) for natural casting to form a film, and adding inert gas N 2 Under the protection, calcining, fixing and sintering at 300 ℃ to ensure that the materials are combined more tightly, and the aflatoxin-reducing composite film is prepared.
FIG. 1 is a 10% WO developed in example 1 3 /g-C 3 N 4 Electron diffraction XRD pattern of the composite material;
FIG. 2 is a TEM spectrum of a composite developed in example 1 at different magnifications; wherein the lamellar is g-C 3 N 4 Length of 100-200nm, WO 3 Is granular and has a size of about 10 nm;
FIG. 3 is an AFM spectrum of a composite filter membrane developed in example 1. The film thickness was uniform, about 25nm.
Example 2: AFB in peanut oil 1 Evaluation of subtractive Performance
Formulated to contain 5.6,11.2,16.8 and 22.4ppb AFB 1 Is allowed to flow at a rate of 50mL/minThe resulting solution was allowed to flow on the composite filter membrane developed in example 1, and then the composite filter membrane was subjected to natural sun irradiation for 10 hours, and the surface was washed 3 times with distilled water and methanol, and the composite filter membrane was recovered, and the above procedure was repeated. Testing AFB in peanut oil using liquid chromatography 1 The subtraction rate is calculated.
FIG. 4 is 10% WO 3 /g-C 3 N 4 The composite film reduces AFB with different initial concentrations 1 According to the peanut oil effect graph, through one-time reduction, the reduction of the toxin of the composite film can reach more than 80%, which shows that the composite film can efficiently reduce the aflatoxin in the peanut oil.
FIG. 5 is 10% WO 3 /g-C 3 N 4 The repeated use performance evaluation of the composite film shows that the composite filter membrane repeatedly reduces peanut oil with the initial concentration of 16.8ppb, the reduction rate is about 92%, and the composite film has stable performance and can be repeatedly used.
Different mass ratios WO 3 And g-C 3 N-developed composite filter membrane for reducing AFB in peanut oil at one time 1 The results are shown in Table 1 below, and from the results, 10% WO 3 /g-C 3 N 4 Best effect (AFB) 1 Initial concentration was 16.8 ppb). In conclusion, the composite filter membrane can not only remove aflatoxin efficiently, but also degrade toxin by utilizing sunlight catalysis, and the technology has the advantages of being green, energy-saving, economical and the like, and is expected to become one of the aflatoxin prevention and control technologies in edible vegetable oil such as peanut oil and the like.
TABLE 1 photocatalytic reduction of initial concentration of 16.8ppb AFB for composites of different mass ratios 1 Peanut oil properties
Example 3: effect of composite film on Total phenols in peanut oil
The total phenol content of peanut oil was tested using the Fu Lin Fen method to evaluate the effect of the filtration abatement process on total phenol content of peanut oil and the results are shown in FIG. 6. After 4 rounds of repeated filtration, the total phenol content in the peanut oil does not change obviously, which indicates that the film is not onlyCan effectively remove AFB in peanut oil 1 The method also can ensure that the functional active component phenols containing benzene ring aromatic groups in the peanut oil are not lost, and has the characteristics of green, low energy consumption, high efficiency, safety and the like. This is because although these phenols contain benzene ring structure, pi-pi stacking is likely to be formed with cyclic aromatic conjugated structure in carbon nitride, compared with AFB 1 The combination of the adsorption synergy of the two types of the phenolic substances is not tight, the peanut oil continuously flows in the composite film or is stirred and oscillated, and the phenolic substances can be well stored in the sample.
Example 4: composite film photocatalysis electron transfer mechanism
Oxygen free radicals, particularly hydroxyl free radicals, generated by the composite film are measured by adopting an electron spin resonance ESR method to prove that the photocatalytic electron transfer mechanism of the composite film is a Z-type system. DMPO (5, 5-dimethyl-1-pyrroline N-oxide) is used as a marker, and is measured by using a German Bruce A200S-9.5/12 electron paramagnetic resonance spectrometer under the conditions of 9.8GHz microwave frequency, 2.2mW power and 3500G field intensity, wherein a xenon lamp is used as a light source for illumination in the test process, and the wavelength is as follows: 420-700 nm.
The results of ESR test of hydroxyl radicals are shown in FIG. 7, and the DMPO-OH pattern consists of four split peaks with peak heights of 1:2:2:1, and the existence of hydroxyl radicals is verified, thus proving WO 3 /g-C 3 N 4 Can generate hydroxyl radical after being excited by light. WO (WO) 3 And g-C 3 N 4 Valence bands of 3.2V and 1.4V, respectively, and if both form a heterojunction, photogenerated holes are taken from WO 3 Pass to g-C 3 N 4 It cannot directly generate hydroxyl radicals because of g-C 3 N 4 Valence band ratio OH - H was difficult to oxidize due to the correction of/(OH (+2.4V vs NHE) 2 O or OH - Hydroxyl groups are formed. Thus, WO 3 And g-C 3 N 4 Can be deduced as a Z-type system, WO 3 Electrons on conduction band and g-C 3 N 4 Holes in the valence band recombine, whereas WO 3 The holes of (2) remain in the valence band, have strong oxidizing ability, are more negative than OH-/. OH (+2.4V vs NHE), and have enough ability to oxidize OH in water - Producing hydroxy groupsAnd (3) radical radicals. Therefore, the composite material electron transfer is a Z-shaped system, and the composite material electron transfer can utilize strong oxidation and reduction capability, has excellent photocatalytic activity and can efficiently reduce aflatoxin.
Claims (9)
1. The preparation method of the composite film material for reducing aflatoxin is characterized by comprising the following steps: the method comprises the following steps:
1) Firstly preparing carbon nitride by high-temperature pyrolysis, and then obtaining carbon nitride nano-sheets, g-C by high-temperature stripping treatment 3 N 4 The size of the sheet layer is 100-200nm, the high-temperature stripping temperature is 580-600 ℃, and the sheet layer is kept for 2-3h;
2) Dispersing carbon nitride nano-sheet in water, stirring, ultrasonic dispersing, adding a certain amount of sodium tungstate, stirring for dissolving, adding acid, converting sodium tungstate into yellow tungstic acid precipitate, centrifuging to obtain precipitate, cleaning, adding acid, regulating pH value to 1.2-1.5, placing in a reaction kettle, and performing hydrothermal reaction at 180-200 ℃ to prepare WO 3 /g-C 3 N 4 A composite material;
3) Adding water to disperse the composite material, adding an organic solvent, fully grinding to obtain a uniform and viscous suspension, then dripping the suspension on a substrate for natural tape casting to form a film, and calcining, fixing and sintering under the protection of inert gas to enable the composite material to be combined with the substrate more tightly, thus preparing the composite film for reducing aflatoxin.
2. The method of manufacturing according to claim 1, characterized in that: the preparation of the carbon nitride by the pyrolysis method in the step 1) is as follows: urea and dicyandiamide are mixed according to the mass ratio of 1: 2-3 are dissolved in distilled water at 50-60 ℃, placed in an oven for recrystallization, after being evenly ground, placed in a crucible, capped, then placed in a tube furnace or a muffle furnace, heated to 550-560 ℃ and kept for 3-4h.
3. The method of manufacturing according to claim 1, characterized in that: the hydrothermal time in the step 2) is 24-30h.
4. The method of manufacturing according to claim 1, characterized in that: and 3) weighing 1.0-2.0g of the composite photocatalytic material, dissolving in 20-30mL of distilled water, performing ultrasonic dispersion, adding 3-5mL of dimethylformamide or methanol, sufficiently grinding to obtain a uniform and sticky suspension, then dripping the suspension on a substrate for natural tape casting to form a film, and calcining and fixedly sintering at 300-350 ℃ under the protection of inert gas to enable the composite filter film to be combined more tightly, thus preparing the composite film for reducing aflatoxin.
5. The method for reducing aflatoxin is characterized by comprising the following steps: the edible vegetable oil sample containing the aflatoxin is fully contacted with the composite film for reducing the aflatoxin, which is prepared by the preparation method of claim 1, the composite film is firstly used for selectively adsorbing and removing the aflatoxin in the sample, then the composite film is placed under the light source of sunlight or a xenon lamp for irradiation, the aflatoxin is gradually degraded, and the composite film for reducing the aflatoxin comprises a substrate and g-C on the substrate 3 N 4 /WO 3 Composite material, g-C 3 N 4 Is of laminated structure, WO 3 The nano particles are uniformly dispersed in the sheet layer g-C 3 N 4 The surface and the combination are tight, and the Z-type semiconductor composite photocatalytic material, the composite material WO 3 /g-C 3 N 4 WO in 3 The mass ratio of (C) is 5-20wt%, g-C 3 N 4 The size of the sheet layer is 100-200nm.
6. The method for reducing aflatoxin according to claim 5, wherein: WO (WO) 3 The nano particles are uniform in size and about 10nm in size.
7. The method for reducing aflatoxin according to claim 5, wherein: the substrate is Indium Tin Oxide (ITO) glass or fluorine-doped SnO 2 Conductive glass FTO.
8. The method for reducing aflatoxin according to claim 5, wherein: the method for contacting the sample containing the aflatoxin with the composite film comprises the following steps: fixing the composite film on a production line, and enabling a sample to slowly flow through the composite film in the production process to be in contact with the composite film; or fixing the composite film on the blade of a propeller type stirrer, placing the composite film into a container for storing samples, and stirring and contacting.
9. The method for reducing aflatoxin according to claim 5, wherein: the edible vegetable oil sample is peanut oil or corn oil which is easy to be polluted by aflatoxin.
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