CN114504058A - Efficient composite mildew inhibitor for feed and preparation method thereof - Google Patents
Efficient composite mildew inhibitor for feed and preparation method thereof Download PDFInfo
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- CN114504058A CN114504058A CN202210198452.XA CN202210198452A CN114504058A CN 114504058 A CN114504058 A CN 114504058A CN 202210198452 A CN202210198452 A CN 202210198452A CN 114504058 A CN114504058 A CN 114504058A
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- extract
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- mildew
- feed
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- 239000003112 inhibitor Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims description 22
- 239000000284 extract Substances 0.000 claims abstract description 113
- 235000000604 Chrysanthemum parthenium Nutrition 0.000 claims abstract description 52
- 241000207925 Leonurus Species 0.000 claims abstract description 52
- 235000000802 Leonurus cardiaca ssp. villosus Nutrition 0.000 claims abstract description 52
- 239000004288 Sodium dehydroacetate Substances 0.000 claims abstract description 30
- 235000019259 sodium dehydroacetate Nutrition 0.000 claims abstract description 30
- 229940079839 sodium dehydroacetate Drugs 0.000 claims abstract description 30
- DSOWAKKSGYUMTF-GZOLSCHFSA-M sodium;(1e)-1-(6-methyl-2,4-dioxopyran-3-ylidene)ethanolate Chemical compound [Na+].C\C([O-])=C1/C(=O)OC(C)=CC1=O DSOWAKKSGYUMTF-GZOLSCHFSA-M 0.000 claims abstract description 30
- 150000001875 compounds Chemical class 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 244000062241 Kaempferia galanga Species 0.000 claims abstract description 19
- BAIBRYAATTUQMG-UHFFFAOYSA-N azane;propanoic acid Chemical compound [NH4+].CCC(O)=O.CCC([O-])=O BAIBRYAATTUQMG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 16
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 16
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 15
- 230000003449 preventive effect Effects 0.000 claims abstract description 11
- 244000269722 Thea sinensis Species 0.000 claims abstract 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 58
- 229920000858 Cyclodextrin Polymers 0.000 claims description 33
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 22
- 239000001116 FEMA 4028 Substances 0.000 claims description 19
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 19
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 19
- 229960004853 betadex Drugs 0.000 claims description 19
- PGRHXDWITVMQBC-UHFFFAOYSA-N dehydroacetic acid Natural products CC(=O)C1C(=O)OC(C)=CC1=O PGRHXDWITVMQBC-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000004287 Dehydroacetic acid Substances 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 235000019258 dehydroacetic acid Nutrition 0.000 claims description 10
- 229940061632 dehydroacetic acid Drugs 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 9
- 229920000053 polysorbate 80 Polymers 0.000 claims description 9
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 239000007790 solid phase Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 230000000855 fungicidal effect Effects 0.000 claims 7
- 239000000417 fungicide Substances 0.000 claims 7
- JEQRBTDTEKWZBW-UHFFFAOYSA-N dehydroacetic acid Chemical compound CC(=O)C1=C(O)OC(C)=CC1=O JEQRBTDTEKWZBW-UHFFFAOYSA-N 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 25
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 6
- 230000003385 bacteriostatic effect Effects 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 37
- 239000000843 powder Substances 0.000 description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 36
- 238000001035 drying Methods 0.000 description 32
- 230000002829 reductive effect Effects 0.000 description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 21
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 20
- 239000001639 calcium acetate Substances 0.000 description 19
- 235000011092 calcium acetate Nutrition 0.000 description 19
- 229960005147 calcium acetate Drugs 0.000 description 19
- 238000010411 cooking Methods 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 238000004821 distillation Methods 0.000 description 16
- 239000012153 distilled water Substances 0.000 description 16
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 13
- 238000001914 filtration Methods 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 241001122767 Theaceae Species 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 238000000498 ball milling Methods 0.000 description 8
- 238000005469 granulation Methods 0.000 description 8
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- 238000010438 heat treatment Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000001694 spray drying Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 6
- SQFSKOYWJBQGKQ-UHFFFAOYSA-N kaempferide Chemical compound C1=CC(OC)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 SQFSKOYWJBQGKQ-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 230000002401 inhibitory effect Effects 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 241000193830 Bacillus <bacterium> Species 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 3
- 206010061218 Inflammation Diseases 0.000 description 3
- 235000013421 Kaempferia galanga Nutrition 0.000 description 3
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000004054 inflammatory process Effects 0.000 description 3
- 230000007794 irritation Effects 0.000 description 3
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- 238000012360 testing method Methods 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- -1 organic acid salt Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
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- 230000001737 promoting effect Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 1
- 229920000856 Amylose Polymers 0.000 description 1
- 206010002660 Anoxia Diseases 0.000 description 1
- 241000976983 Anoxia Species 0.000 description 1
- 108010025880 Cyclomaltodextrin glucanotransferase Proteins 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 231100000678 Mycotoxin Toxicity 0.000 description 1
- 241000244206 Nematoda Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 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 1
- 208000037386 Typhoid Diseases 0.000 description 1
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- 230000017531 blood circulation Effects 0.000 description 1
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- 229940097362 cyclodextrins Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- LDCRTTXIJACKKU-ONEGZZNKSA-N dimethyl fumarate Chemical compound COC(=O)\C=C\C(=O)OC LDCRTTXIJACKKU-ONEGZZNKSA-N 0.000 description 1
- 229960004419 dimethyl fumarate Drugs 0.000 description 1
- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 description 1
- 229930004069 diterpene Natural products 0.000 description 1
- 150000004141 diterpene derivatives Chemical class 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
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- 229910001872 inorganic gas Inorganic materials 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000002636 mycotoxin Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
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- 230000020477 pH reduction Effects 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 235000017454 sodium diacetate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 201000008297 typhoid fever Diseases 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K30/00—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/163—Sugars; Polysaccharides
-
- 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3481—Organic compounds containing oxygen
- A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Animal Husbandry (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Botany (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of feeds, and particularly relates to an efficient compound mildew preventive for feeds and a preparation method thereof, wherein the efficient compound mildew preventive comprises the following components in parts by mass: 5-10 parts of propionic acid-ammonium propionate mixture, 1-2 parts of rhizoma kaempferiae extract, 1-2 parts of motherwort herb extract, 5-7 parts of tea polyphenol, 5-10 parts of sodium dehydroacetate, 0.1-0.3 part of emulsifier and 30-40 parts of carrier. The invention solves the problem of poor effect of the existing mildew inhibitor, a double-effect antibacterial bacteriostatic system is formed by combining sodium dehydroacetate with a propionic acid-ammonium propionate mixture, the integral mildew-resistant effect is improved, and meanwhile, the tea polyphenol, the motherwort herb extract and the kaempferia galangal extract are used as auxiliary mildew inhibitors, so that the mildew inhibitor has a good bacteriostatic effect and has the characteristics of long acting, safety, high stability and the like.
Description
Technical Field
The invention belongs to the technical field of feeds, and particularly relates to an efficient compound mildew preventive for a feed and a preparation method thereof.
Background
With the development of the feed industry, the feed is inevitably polluted by the mildew during the storage and circulation processes, the reduction of the feed nutritive value caused by the mildew of the feed and the generation of mycotoxin bring great harm to the feed safety, and meanwhile, the food safety of human beings is seriously threatened. In order to prevent the feed from mildewing, the simplest, most economical and most effective method is to add a mildew inhibitor into the feed to inhibit the growth of the mildews.
The existing feed mildew inhibitor mainly comprises propionic acid, propionate, organic acid salt and esters, such as fumaric acid, dimethyl fumarate, sodium diacetate and the like. The mildew preventive has poor mildew preventive effect on the feed or has strong irritation, so that the feed intake of animals is reduced, the residue is serious, and certain side effect is caused on the animals.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an efficient composite mildew inhibitor for feed, which solves the problem of poor effect of the existing mildew inhibitor, a double-effect antibacterial and bacteriostatic system is formed by combining sodium dehydroacetate with a propionic acid-ammonium propionate mixture, the integral mildew inhibition effect is improved, and meanwhile, tea polyphenol, a motherwort herb extract and a kaempferia galangal extract are taken as auxiliary mildew inhibitors, so that the efficient composite mildew inhibitor has a good antibacterial effect and has the characteristics of long acting, safety, high stability and the like.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
an efficient composite mildew inhibitor for feed comprises the following components in parts by mass:
5-10 parts of propionic acid-ammonium propionate mixture,
1-2 parts of kaempferia galangal extract,
1-2 parts of motherwort extract,
5-7 parts of tea polyphenol,
5-10 parts of sodium dehydroacetate,
0.1 to 0.3 portion of emulsifier,
30-40 parts of a carrier.
Wherein the content of the first and second substances,the carrier consists of beta-cyclodextrin and calcium carbonate, and the calcium carbonate is light calcium carbonate; further, the mass ratio of the beta-cyclodextrin to the light calcium carbonate is 3-4: 1. The beta-cyclodextrin wraps the light calcium carbonate; cyclodextrins are the generic term for a series of cyclic oligosaccharides produced from amylose by the action of cyclodextrin glycosyltransferases produced by Bacillus bacteria, usually containing 6-12D-glucopyranose units. The cyclodextrin molecule has a slightly tapered hollow cylindrical three-dimensional ring structure, and in the hollow structure, the upper end (larger opening end) of the outer side is formed by C2And C3Is composed of secondary hydroxyl groups, the lower end (smaller open end) is composed of C6The primary hydroxyl group is formed and has hydrophilicity, and a hydrophobic area is formed in the cavity due to the shielding effect of C-H. Therefore, various organic compounds can be embedded into the hydrophobic holes of the cyclodextrin to form an inclusion complex, and the physical and chemical properties of the inclusion complex are changed; the cyclodextrin molecule can be crosslinked with a plurality of functional groups or the cyclodextrin is crosslinked on a polymer to carry out chemical modification or carry out polymerization by taking the cyclodextrin as a monomer. Because the cyclodextrin is hydrophilic at its outer edge and hydrophobic in its inner cavity, it can provide a hydrophobic binding site like an enzyme, serving as a host to encapsulate various suitable guests, such as organic molecules, inorganic ions, and gas molecules. The hydrophobic property of the inner cavity and the hydrophilic property of the outer part enable the inner cavity to form an inclusion compound and a molecular assembly system with a plurality of organic and inorganic molecules according to Van der Waals force, hydrophobic interaction force, matching action among host molecules and guest molecules and the like. In the whole system, the cyclodextrin can adsorb effective components, the effective components are classified and gathered by utilizing the special properties of internal hydrophobicity and external hydrophilicity, the protection effect is achieved, meanwhile, in the using process, the cyclodextrin has a good slow release effect, the long-acting property of the mildew preventive in the feed is kept, and the service life of the feed is prolonged. The light calcium carbonate has good carrier fluidity, meanwhile, the light calcium carbonate particles are fine, the surface is rough, the specific surface area is large, and when the cyclodextrin is combined with the light calcium carbonate, the large surface area of the light calcium carbonate ensures that the cyclodextrin forms large-area exposure, so that the adsorption and slow release effects are better formed; the preparation method of the carrier comprises the following steps: a1, adding calcium acetate toPerforming ball milling treatment in absolute ethyl alcohol to form fine powder particles, and then drying at constant temperature to obtain calcium acetate fine powder, wherein the mass ratio of the ethyl alcohol to the calcium acetate is 1:10-15, the ball milling treatment temperature is 30-50 ℃, the pressure is 0.2-0.4MPa, and the constant temperature drying temperature is 90-100 ℃; 2, adding beta-cyclodextrin into calcium acetate fine powder, stirring uniformly, performing press granulation to obtain carrier particles, and then standing for 10-30min in a water vapor environment to obtain a composite pre-carrier, wherein the stirring speed is 1000-2000r/min, the press granulation temperature is 70-90 ℃, the pressure is 0.2-0.4MPa, the water vapor volume percentage of the water vapor environment is 10-20%, the temperature is 95-105 ℃, the cyclodextrin at the temperature can absorb the water vapor to form certain fluidity, the calcium acetate is stably wrapped by the cyclodextrin, the wrapping effect is improved, and meanwhile, the water solubility of the calcium acetate can ensure that the calcium acetate is wrapped and divided by the cyclodextrin, so that the wrapping effect is greatly improved; 3, standing the composite pre-carrier for 1-2h at constant temperature, introducing steam for secondary standing for 20-40min, and drying to obtain the carrier, wherein the temperature of the constant temperature standing is 170-180 ℃, the volume of the steam accounts for 10-14% in the environment after the steam is introduced, the temperature of the secondary standing is 95-100 ℃, and the temperature of the drying is 120-140 ℃; in the process of standing at constant temperature, calcium acetate forms stable decomposition, calcium carbonate and acetone are converted in situ to form a structure with rough and concave surfaces of light calcium carbonate, so that the specific surface area of beta-cyclodextrin is increased, water molecules on a pre-carrier are converted into steam and the acetone is taken away quickly, and the conversion effect is greatly improved; the beta-cyclodextrin on the surface can flow secondarily by secondary standing, air holes formed by water vapor and acetone are completely blocked, and the light calcium carbonate with rough surface is wrapped by the cyclodextrin.
The emulsifier adopts Tween 80, and the Tween 80 adopts food-grade Tween 80.
The sodium dehydroacetate is a new food preservative after sodium benzoate, nipagin and potassium sorbate, has good inhibition effect on mould, yeast and bacteria, is widely applied to the processing industries of beverages, foods and feeds, can prolong the storage period and avoid mildewing loss. The action mechanism is that the preservative film effectively permeates into cells to inhibit the respiration of microorganisms, thereby achieving the effects of corrosion prevention, mildew prevention, fresh keeping, moisture preservation and the like. The sodium dehydroacetate has broad-spectrum antibacterial ability, and has strong antibacterial ability to mould and yeast, and has strong action to the yeast and mould which cause food putrefaction, and simultaneously, the sodium dehydroacetate has good light and heat resistance, and can not be decomposed and evaporated with water vapor in the food processing process. Tests prove that the sodium dehydroacetate has no toxic or side effect, high safety and no abnormal peculiar smell when used in food. The sodium dehydroacetate is prepared by reacting ethyl acetoacetate with sodium bicarbonate to obtain dehydroacetic acid, and the dehydroacetic acid is purified and then reacts with sodium hydroxide solid phase to obtain the sodium dehydroacetate.
The motherwort extract is rich in alkaloid, diterpene, flavone, polyphenol, polysaccharide and other substances, and has the functions of calming, easing pain, inhibiting bacteria, resisting inflammation, resisting anoxia, resisting oxidation, resisting stress, resisting fatigue, enriching blood, promoting blood circulation to remove blood stasis and promoting blood coagulation, and meanwhile, the motherwort extract has the functions of enhancing the immune system, inhibiting bacteria and the like. The motherwort extract is a motherwort hydroalcoholic compound extract, and the preparation method of the motherwort extract comprises the following steps: b1, cutting and crushing fresh motherwort to form motherwort powder, adding the motherwort powder into distilled water, stirring to form suspension, wherein the concentration of the motherwort powder in the distilled water is 100-300g/L, b2, heating and cooking the suspension for 1-2h, then adjusting the pH to 5-6, standing for 20-40min, cooking for 1-2h after standing, filtering to obtain an extracting solution and filter residue, wherein the temperature of the heating and cooking is 80-95 ℃, the pH is adjusted by concentrated hydrochloric acid, and the temperature of the secondary cooking is 90-95 ℃; the treatment mode is beneficial to dissolving out the effective components, reduces the loss of the effective components, recovers the effective components of the motherwort to the maximum extent, simultaneously, an acidic extraction system can be formed by acidification and standing, secondary acid extraction is formed, hydrochloric acid is taken out in secondary cooking, cooking extraction is formed again, and the release of the effective substances is greatly improved; b3, centrifugally separating the extracting solution, and concentrating under reduced pressure to obtain an extract, wherein the pressure of the concentration under reduced pressure is 70-80% of the atmospheric pressure, and the temperature is 90-95 ℃; 4, drying the extract, placing the dried extract into absolute ethyl alcohol for microwave treatment for 20-40min, filtering to obtain a high-purity extract, and carrying out reduced pressure distillation to obtain the high-purity extract, wherein the mass ratio of the extract to the ethyl alcohol is 4:5-7, the power of the microwave treatment is 200-400W, the temperature is 20-40 ℃, the temperature of the reduced pressure distillation is 70-80 ℃, and the pressure is 70-90% of atmospheric pressure; based on the fact that the water extract of the motherwort contains a small amount of impurities and is difficult to remove in the extract, aiming at the problem, the water extract of the motherwort is subjected to alcohol washing to remove the impurities in the water extract, so that a good purification effect is achieved, and the effective components of the obtained motherwort extract are greatly improved; b5, spray drying the high-purity extract to obtain the motherwort extract, wherein the temperature of the spray drying is 80-90 ℃. The herba Leonuri extract prepared by the method has high purity of the retained effective components, and effectively reduces impurities in the extraction process, and after water extraction and alcohol extraction, the impurities in the herba Leonuri extract are greatly reduced, and the purity of active substances is improved.
The kaempferide volatile oil and partial monomer compounds have a series of physiological activities of resisting inflammation, resisting oxidation, resisting and preventing cancer, killing nematodes and the like, and the kaempferide has an inhibiting effect on staphylococcus aureus, typhoid bacillus, pseudomonas aeruginosa, dysentery bacillus and the like. Has effects in inhibiting inflammation of rat implanted wool ball. Kaempferide contains multiple phenolic hydroxyl groups and has strong antioxidation. The Kaempferia galanga extract has inhibitory effect on many human enzymes, such as tyrosinase activity. The preparation method of the kaempferia galangal extract comprises the following steps: c1, cleaning the rhizoma kaempferiae, adding the rhizoma kaempferiae into the reaction kettle, introducing low-temperature nitrogen for quick freezing, and crushing to obtain fine rhizoma kaempferiae powder; the temperature of the low-temperature nitrogen is minus 20 ℃; c2, adding absolute ethyl alcohol into the quick-frozen rhizoma kaempferiae fine powder, and performing microwave reaction for 2-4 hours to obtain rhizoma kaempferiae ethanol extract; the mass ratio of the anhydrous ethanol to the kaempferia galangal fine powder is 20-50:1, the microwave reaction temperature is 0-5 ℃, and the microwave power is 400-600W; c3, adding ether into the kaempferia galanga extracting solution, carrying out ultrasonic reaction for 30-50min, filtering, and drying the filtrate to obtain an extract, wherein the addition amount of the ether is 120-200% of the volume of the kaempferia galanga extracting solution, the ultrasonic reaction temperature is 20-30 ℃, the ultrasonic frequency is 40-70kHz, and the drying temperature is 80-85 ℃; c4, adding the extract into distilled water for microwave treatment for 30-60min, centrifuging to extract supernatant, carrying out reduced pressure distillation, and drying to obtain rhizoma kaempferiae extract, wherein the concentration of the extract in the distilled water is 30-60g/L, the microwave power of the microwave treatment is 300-500W, and the temperature is 50-70 ℃; the reduced pressure distillation temperature is 95-100 deg.C, and the pressure is 80-90% of atmospheric pressure.
The preparation method of the compound mildew inhibitor comprises the following steps:
step 1, mixing and weighing rhizoma kaempferiae extract, motherwort extract, tea polyphenol and propionic acid-ammonium propionate, and uniformly stirring to form a mixture;
and 2, adding sodium dehydroacetate and an emulsifier into the mixture, uniformly stirring, adding the carrier, performing ultrasonic dispersion for 20-30min, and inspecting and packaging to obtain the composite mildew inhibitor, wherein the ultrasonic dispersion temperature is 20-30 ℃, and the ultrasonic frequency is 30-50 kHz.
The addition amount of the compound mildew preventive in the feed is 0.1-0.4%.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of poor effect of the existing mildew inhibitor, a double-effect antibacterial bacteriostatic system is formed by combining sodium dehydroacetate with a propionic acid-ammonium propionate mixture, the integral mildew-resistant effect is improved, and meanwhile, the tea polyphenol, the motherwort herb extract and the kaempferia galangal extract are used as auxiliary mildew inhibitors, so that the mildew inhibitor has a good bacteriostatic effect and has the characteristics of long acting, safety, high stability and the like.
2. The invention effectively solves the problem that the single use of the propionic acid-ammonium propionate mixture and the sodium dehydroacetate has large irritation, and effectively reduces the use amount and the irritation of the mildew preventive by utilizing the cooperative matching mode of the propionic acid-ammonium propionate mixture and the sodium dehydroacetate.
3. According to the invention, calcium carbonate and beta-cyclodextrin are utilized to form an organic-inorganic carrier, the wrapping property and slow release effect of organic matters are fully utilized, the slow release property and long-acting property of the mildew preventive are ensured, and meanwhile, the beta-cyclodextrin effectively improves the taste of the feed.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
An efficient composite mildew inhibitor for feed comprises the following components in parts by mass:
5 parts of propionic acid-ammonium propionate mixture,
1 part of kaempferia galangal extract,
1 part of motherwort extract,
5 portions of tea polyphenol,
5 parts of sodium dehydroacetate,
0.1 portion of emulsifier,
And 30 parts of a carrier.
Wherein the carrier consists of beta-cyclodextrin and calcium carbonate, and the calcium carbonate is light calcium carbonate; the mass ratio of the beta-cyclodextrin to the light calcium carbonate is 3: 1. The preparation method of the carrier comprises the following steps: 1, adding calcium acetate into absolute ethyl alcohol, performing ball milling treatment to form fine powder particles, and then drying at constant temperature to obtain calcium acetate fine powder, wherein the mass ratio of the ethyl alcohol to the calcium acetate is 1:10, the ball milling treatment temperature is 30 ℃, the pressure is 0.2MPa, and the constant-temperature drying temperature is 90 ℃; a2, adding beta-cyclodextrin into calcium acetate fine powder, uniformly stirring, performing press granulation to obtain carrier particles, and then standing for 10min in a water vapor environment to obtain a composite pre-carrier, wherein the stirring speed is 1000-2000r/min, the press granulation temperature is 70 ℃, the pressure is 0.2MPa, the water vapor volume percentage in the water vapor environment is 10%, and the temperature is 95 ℃; a3, standing the composite pre-carrier for 1 hour at constant temperature, introducing water vapor for secondary standing for 20min, and drying to obtain the carrier, wherein the temperature of the constant-temperature standing is 170 ℃, the volume of the water vapor accounts for 10% of the environment after the water vapor is introduced, the temperature of the secondary standing is 95 ℃, and the temperature of the drying is 120 ℃.
The emulsifier adopts food-grade Tween 80.
The sodium dehydroacetate is prepared by reacting ethyl acetoacetate with sodium bicarbonate to obtain dehydroacetic acid, and the dehydroacetic acid is purified and then reacts with sodium hydroxide solid phase to obtain the sodium dehydroacetate.
The motherwort extract is a motherwort hydroalcoholic compound extract, and the preparation method of the motherwort extract comprises the following steps: b1, cutting and crushing fresh motherwort to form motherwort powder, adding the motherwort powder into distilled water, stirring to form turbid liquid, wherein the concentration of the motherwort powder in the distilled water is 100g/L, b2, heating and cooking the turbid liquid for 1 hour, adjusting the pH value to 5, standing for 20min, cooking for 1 hour for the second time after standing, filtering to obtain an extracting solution and filter residue, wherein the temperature of heating and cooking is 80 ℃, the pH value is adjusted by concentrated hydrochloric acid, and the temperature of cooking for the second time is 90 ℃; b3, centrifugally separating the extracting solution, and concentrating under reduced pressure to obtain an extract, wherein the pressure of the concentration under reduced pressure is 70% of the atmospheric pressure, and the temperature is 90 ℃; b4, drying the extract, placing the dried extract into absolute ethyl alcohol for microwave treatment for 20min, filtering to obtain a high-purity extract, and carrying out reduced pressure distillation to obtain the high-purity extract, wherein the mass ratio of the extract to the ethyl alcohol is 4:5, the microwave treatment power is 200W, the temperature is 20 ℃, the reduced pressure distillation temperature is 70 ℃, and the pressure is 70% of the atmospheric pressure; b5, spray drying the high-purity extract to obtain the motherwort extract, wherein the temperature of the spray drying is 80 ℃.
The preparation method of the kaempferia galangal extract comprises the following steps: c1, cleaning the rhizoma kaempferiae, adding the rhizoma kaempferiae into the reaction kettle, introducing low-temperature nitrogen for quick freezing, and crushing to obtain fine rhizoma kaempferiae powder; the temperature of the low-temperature nitrogen is minus 20 ℃; c2, adding absolute ethyl alcohol into the quick-frozen rhizoma kaempferiae fine powder, and performing microwave reaction for 2 hours to obtain rhizoma kaempferiae alcohol extract; the mass ratio of the absolute ethyl alcohol to the kaempferia galangal fine powder is 20:1, the microwave reaction temperature is 0 ℃, and the microwave power is 400W; c3, adding diethyl ether into the rhizoma kaempferiae extract, carrying out ultrasonic reaction for 30min, filtering, and drying the filtrate to obtain an extract, wherein the addition amount of the diethyl ether is 120% of the volume of the rhizoma kaempferiae extract, the ultrasonic reaction temperature is 20 ℃, the ultrasonic frequency is 40kHz, and the drying temperature is 80 ℃; c4, adding the extract into distilled water for microwave treatment for 30min, centrifuging to extract supernatant, carrying out reduced pressure distillation, and drying to obtain rhizoma kaempferiae extract, wherein the concentration of the extract in distilled water is 30g/L, the microwave power of the microwave treatment is 300W, and the temperature is 50 ℃; the reduced pressure distillation temperature is 95 ℃, and the pressure is 80-90% of the atmospheric pressure.
The preparation method of the compound mildew inhibitor comprises the following steps:
step 1, mixing and weighing rhizoma kaempferiae extract, motherwort extract, tea polyphenol and propionic acid-ammonium propionate, and uniformly stirring to form a mixture;
and 2, adding sodium dehydroacetate and an emulsifier into the mixture, uniformly stirring, adding a carrier, performing ultrasonic dispersion for 20min, and inspecting and packaging to obtain the composite mildew inhibitor, wherein the ultrasonic dispersion temperature is 20 ℃ and the ultrasonic frequency is 30 kHz.
Example 2
The efficient composite mildew inhibitor for the feed comprises the following components in percentage by mass:
10 portions of propionic acid-ammonium propionate mixture,
2 parts of kaempferia galangal extract,
2 portions of motherwort extract,
7 portions of tea polyphenol,
10 parts of sodium dehydroacetate,
0.3 portion of emulsifier
40 parts of a carrier.
The carrier consists of beta-cyclodextrin and calcium carbonate, and the calcium carbonate is light calcium carbonate; the mass ratio of the beta-cyclodextrin to the light calcium carbonate is 4: 1. The preparation method of the carrier comprises the following steps: 1, adding calcium acetate into absolute ethyl alcohol, performing ball milling treatment to form fine powder particles, and then drying at constant temperature to obtain calcium acetate fine powder, wherein the mass ratio of the ethyl alcohol to the calcium acetate is 1:15, the ball milling treatment temperature is 50 ℃, the pressure is 0.4MPa, and the drying temperature at constant temperature is 100 ℃; a2, adding beta-cyclodextrin into calcium acetate fine powder, uniformly stirring, performing press granulation to obtain carrier particles, and then standing for 30min in a water vapor environment to obtain a composite pre-carrier, wherein the stirring speed is 2000r/min, the press granulation temperature is 90 ℃, the pressure is 0.4MPa, the water vapor volume percentage in the water vapor environment is 20%, and the temperature is 105 ℃; a3, standing the composite pre-carrier for 2 hours at constant temperature, introducing steam for secondary standing for 40min, and drying to obtain the carrier, wherein the temperature of the constant temperature standing is 180 ℃, the volume of the steam accounts for 14% in the environment after the steam is introduced, the temperature of the secondary standing is 100 ℃, and the temperature of the drying is 140 ℃.
The emulsifier adopts food-grade Tween 80.
The sodium dehydroacetate is prepared by reacting ethyl acetoacetate with sodium bicarbonate to obtain dehydroacetic acid, and the dehydroacetic acid is purified and then reacts with sodium hydroxide solid phase to obtain the sodium dehydroacetate.
The motherwort extract is a motherwort hydroalcoholic compound extract, and the preparation method of the motherwort extract comprises the following steps: b1, cutting and crushing fresh motherwort to form motherwort powder, adding the motherwort powder into distilled water, stirring to form turbid liquid, wherein the concentration of the motherwort powder in the distilled water is 300g/L, b2, heating and cooking the turbid liquid for 2 hours, adjusting the pH value to 6, standing for 40min, cooking for 2 hours for the second time after the standing is finished, filtering to obtain an extracting solution and filter residues, wherein the temperature of the heating and cooking is 95 ℃, the pH value is adjusted by concentrated hydrochloric acid, and the temperature of the cooking for the second time is 95 ℃; b3, centrifugally separating the extracting solution, and concentrating under reduced pressure to obtain an extract, wherein the pressure of the concentration under reduced pressure is 80% of the atmospheric pressure, and the temperature is-95 ℃; b4, drying the extract, placing the dried extract into absolute ethyl alcohol for microwave treatment for 40min, filtering to obtain a high-purity extract, and carrying out reduced pressure distillation to obtain the high-purity extract, wherein the mass ratio of the extract to the ethyl alcohol is 4:7, the microwave treatment power is 400W, the temperature is 40 ℃, the reduced pressure distillation temperature is 80 ℃, and the pressure is 90% of the atmospheric pressure; b5, spray drying the high-purity extract to obtain the motherwort extract, wherein the temperature of the spray drying is 90 ℃.
The preparation method of the kaempferia galangal extract comprises the following steps: c1, cleaning the rhizoma kaempferiae, adding the rhizoma kaempferiae into the reaction kettle, introducing low-temperature nitrogen for quick freezing, and crushing to obtain fine rhizoma kaempferiae powder; the temperature of the low-temperature nitrogen is minus 20 ℃; c2, adding absolute ethyl alcohol into the quick-frozen rhizoma kaempferiae fine powder, and performing microwave reaction for 4 hours to obtain rhizoma kaempferiae alcohol extract; the mass ratio of the absolute ethyl alcohol to the kaempferia galangal fine powder is 50:1, the microwave reaction temperature is 5 ℃, and the microwave power is 600W; c3, adding diethyl ether into the rhizoma kaempferiae extract, carrying out ultrasonic reaction for 50min, filtering, and drying the filtrate to obtain an extract, wherein the addition amount of the diethyl ether is 200% of the volume of the rhizoma kaempferiae extract, the ultrasonic reaction temperature is 30 ℃, the ultrasonic frequency is 70kHz, and the drying temperature is 85 ℃; c4, adding the extract into distilled water for microwave treatment for 60min, centrifuging to extract supernatant, carrying out reduced pressure distillation, and drying to obtain rhizoma kaempferiae extract, wherein the concentration of the extract in distilled water is 60g/L, the microwave power of the microwave treatment is 500W, and the temperature is 70 ℃; the temperature of the reduced pressure distillation is 100 ℃, and the pressure is 90% of the atmospheric pressure.
The preparation method of the compound mildew inhibitor comprises the following steps:
step 1, mixing and weighing rhizoma kaempferiae extract, motherwort extract, tea polyphenol and propionic acid-ammonium propionate, and uniformly stirring to form a mixture;
and 2, adding sodium dehydroacetate and an emulsifier into the mixture, uniformly stirring, adding a carrier, performing ultrasonic dispersion for 30min, and inspecting and packaging to obtain the composite mildew inhibitor, wherein the ultrasonic dispersion temperature is 30 ℃ and the ultrasonic frequency is 50 kHz.
Example 3
The efficient composite mildew inhibitor for the feed comprises the following components in percentage by mass:
8 parts of propionic acid-ammonium propionate mixture,
2 parts of kaempferia galangal extract,
1 part of motherwort extract,
4 portions of tea polyphenol,
8 parts of sodium dehydroacetate,
0.2 portion of emulsifier
And 35 parts of a carrier.
Wherein the carrier consists of beta-cyclodextrin and calcium carbonate, and the calcium carbonate is light calcium carbonate; the mass ratio of the beta-cyclodextrin to the light calcium carbonate is 4: 1. The preparation method of the carrier comprises the following steps: 1, adding calcium acetate into absolute ethyl alcohol, performing ball milling treatment to form fine powder particles, and then drying at constant temperature to obtain calcium acetate fine powder, wherein the mass ratio of the ethyl alcohol to the calcium acetate is 1:12, the ball milling treatment temperature is 40 ℃, the pressure is 0.3MPa, and the constant-temperature drying temperature is 95 ℃; a2, adding beta-cyclodextrin into calcium acetate fine powder, uniformly stirring, performing press granulation to obtain carrier particles, and then standing for 20min in a steam environment to obtain a composite pre-carrier, wherein the stirring speed is 1500r/min, the press granulation temperature is 80 ℃, the pressure is 0.3MPa, the steam volume percentage in the steam environment is 15%, and the temperature is 100 ℃; a3, standing the composite pre-carrier for 2 hours at constant temperature, introducing steam for secondary standing for 30 minutes, and drying to obtain the carrier, wherein the temperature of the constant-temperature standing is 175 ℃, the volume of the steam accounts for 12% in the environment after the steam is introduced, the temperature of the secondary standing is 98 ℃, and the temperature of the drying is 130 ℃.
The emulsifier adopts food-grade Tween 80.
The sodium dehydroacetate is prepared by reacting ethyl acetoacetate with sodium bicarbonate to obtain dehydroacetic acid, and the dehydroacetic acid is purified and then reacts with sodium hydroxide solid phase to obtain the sodium dehydroacetate.
The motherwort extract is a motherwort hydroalcoholic compound extract, and the preparation method of the motherwort extract comprises the following steps: b1, cutting and crushing fresh motherwort to form motherwort powder, adding the motherwort powder into distilled water, stirring to form turbid liquid, wherein the concentration of the motherwort powder in the distilled water is 200g/L, b2, heating and cooking the turbid liquid for 2 hours, adjusting the pH value to 6, standing for 30 minutes, cooking for 2 hours for the second time after the standing is finished, filtering to obtain an extracting solution and filter residues, wherein the temperature of the heating and cooking is 90 ℃, the pH value is adjusted by concentrated hydrochloric acid, and the temperature of the cooking for the second time is 93 ℃; b3, centrifugally separating the extracting solution, and concentrating under reduced pressure to obtain an extract, wherein the pressure of the concentration under reduced pressure is 75% of the atmospheric pressure, and the temperature is 93 ℃; b4, drying the extract, placing the dried extract into absolute ethyl alcohol for microwave treatment for 30min, filtering to obtain a high-purity extract, and carrying out reduced pressure distillation to obtain the high-purity extract, wherein the mass ratio of the extract to the ethyl alcohol is 4:6, the microwave treatment power is 300W, the temperature is 30 ℃, the reduced pressure distillation temperature is 75 ℃, and the pressure is 80% of the atmospheric pressure; b5, spray drying the high-purity extract to obtain the motherwort extract, wherein the temperature of the spray drying is 85 ℃.
The preparation method of the kaempferia galangal extract comprises the following steps: c1, cleaning the rhizoma kaempferiae, adding the rhizoma kaempferiae into the reaction kettle, introducing low-temperature nitrogen for quick freezing, and crushing to obtain fine rhizoma kaempferiae powder; the temperature of the low-temperature nitrogen is minus 20 ℃; c2, adding absolute ethyl alcohol into the quick-frozen rhizoma kaempferiae fine powder, and performing microwave reaction for 3 hours to obtain rhizoma kaempferiae alcohol extract; the mass ratio of the absolute ethyl alcohol to the kaempferia galangal fine powder is 40:1, the microwave reaction temperature is 3 ℃, and the microwave power is 500W; c3, adding diethyl ether into the rhizoma kaempferiae extract, carrying out ultrasonic reaction for 40min, filtering, and drying the filtrate to obtain an extract, wherein the addition amount of the diethyl ether is 180% of the volume of the rhizoma kaempferiae extract, the ultrasonic reaction temperature is 25 ℃, the ultrasonic frequency is 60kHz, and the drying temperature is 83 ℃; c4, adding the extract into distilled water for microwave treatment for 50min, centrifuging to extract supernatant, carrying out reduced pressure distillation, and drying to obtain rhizoma kaempferiae extract, wherein the concentration of the extract in distilled water is 50g/L, the microwave power of the microwave treatment is 400W, and the temperature is 60 ℃; the temperature of the reduced pressure distillation is 100 ℃, and the pressure is 85% of the atmospheric pressure.
The preparation method of the compound mildew inhibitor comprises the following steps:
step 1, mixing and weighing rhizoma kaempferiae extract, motherwort extract, tea polyphenol and propionic acid-ammonium propionate, and uniformly stirring to form a mixture;
and 2, adding sodium dehydroacetate and an emulsifier into the mixture, uniformly stirring, adding a carrier, performing ultrasonic dispersion for 25min, and inspecting and packaging to obtain the composite mildew inhibitor, wherein the ultrasonic dispersion temperature is 25 ℃ and the ultrasonic frequency is 40 kHz.
The products of examples 1-3 were used as test examples and some commercially available mildewcide was used as comparative examples, and were added to the feeds in an addition ratio of 0.3%, mixed well, placed in a mold incubator at a temperature of 30 ℃ and a relative humidity of 90%, and the feeds without any mildewcide were used as blank samples, and the mildewing of the feeds was observed and recorded. The feed has the following mildew-proof effect
Blank space | Example 1 | Example 2 | Example 3 | Comparative example | |
Amount of addition | 0 | 0.3% | 0.3% | 0.3% | 0.3% |
3 days | Is normal | Is normal | Is normal | Is normal | Is normal |
5 days | Is normal and normal | Is normal | Is normal | Is normal | Is normal |
7 days | Slight mildew | Is normal | Is normal | Is normal | Is normal |
9 days | The mildew is more serious | Is normal | Is normal | Is normal | Slight mildew |
11 days | Severe mildew | Is normal | Is normal | Is normal | Obviously mildewed |
13 days | Severe mildew | Is normal | Is normal | Is normal | The mildew is more serious |
15 days | Severe mildew | Slight mildew | Is normal | Slight mildew | Severe mildew |
The tests show that the product has a good mildew-proof effect, and the mildew-proof effect has a certain long-acting property and slow release property compared with the mildew-proof effect of the commercially available product.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (9)
1. The efficient composite mildew inhibitor for the feed is characterized by comprising the following components in parts by weight: the mass ratio of the components is as follows:
5-10 parts of propionic acid-ammonium propionate mixture,
1-2 parts of kaempferia galangal extract,
1-2 parts of motherwort extract,
5-7 parts of tea polyphenol,
5-10 parts of sodium dehydroacetate,
0.1 to 0.3 portion of emulsifier,
30-40 parts of a carrier.
2. The efficient compound mildew preventive for feed according to claim 1, characterized in that: the carrier consists of beta-cyclodextrin and calcium carbonate, and the calcium carbonate is light calcium carbonate.
3. The highly effective compound fungicide for feed according to claim 2, characterized in that: the mass ratio of the beta-cyclodextrin to the light calcium carbonate is 3-4: 1.
4. The highly effective compound fungicide for feed according to claim 1, characterized in that: the emulsifier adopts Tween 80, and the Tween 80 adopts food-grade Tween 80.
5. The highly effective compound fungicide for feed according to claim 1, characterized in that: the sodium dehydroacetate is prepared by reacting ethyl acetoacetate with sodium bicarbonate to obtain dehydroacetic acid, and the dehydroacetic acid is purified and then reacts with sodium hydroxide solid phase to obtain the sodium dehydroacetate.
6. The highly effective compound fungicide for feed according to claim 1, characterized in that: the herba Leonuri extract is herba Leonuri water-alcohol compound extract.
7. The highly effective compound fungicide for feed according to claim 1, characterized in that: the preparation method of the compound mildew inhibitor comprises the following steps:
step 1, mixing and weighing rhizoma kaempferiae extract, motherwort extract, tea polyphenol and propionic acid-ammonium propionate, and uniformly stirring to form a mixture;
and 2, adding sodium dehydroacetate and an emulsifier into the mixture, uniformly stirring, adding the carrier, performing ultrasonic dispersion for 20-30min, and inspecting and packaging to obtain the composite mildew inhibitor.
8. The highly effective compound fungicide for feed according to claim 7, characterized in that: the temperature of the ultrasonic dispersion is 20-30 ℃, and the ultrasonic frequency is 30-50 kHz.
9. The highly effective compound fungicide for feed according to claim 1, characterized in that: the addition amount of the compound mildew preventive in the feed is 0.1-0.4%.
Priority Applications (1)
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