CN110301572A - The method for preparing food preservative using Chinese anise oil extract waste liquid - Google Patents
The method for preparing food preservative using Chinese anise oil extract waste liquid Download PDFInfo
- Publication number
- CN110301572A CN110301572A CN201910642507.XA CN201910642507A CN110301572A CN 110301572 A CN110301572 A CN 110301572A CN 201910642507 A CN201910642507 A CN 201910642507A CN 110301572 A CN110301572 A CN 110301572A
- Authority
- CN
- China
- Prior art keywords
- anise
- anisic
- waste liquid
- water phase
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 62
- 239000002699 waste material Substances 0.000 title claims abstract description 38
- 239000010617 anise oil Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 27
- 235000019249 food preservative Nutrition 0.000 title claims abstract description 18
- 239000005452 food preservative Substances 0.000 title claims abstract description 18
- ZEYHEAKUIGZSGI-UHFFFAOYSA-N 4-methoxybenzoic acid Chemical compound COC1=CC=C(C(O)=O)C=C1 ZEYHEAKUIGZSGI-UHFFFAOYSA-N 0.000 claims abstract description 114
- 235000007265 Myrrhis odorata Nutrition 0.000 claims abstract description 98
- 235000012550 Pimpinella anisum Nutrition 0.000 claims abstract description 98
- ZRSNZINYAWTAHE-UHFFFAOYSA-N p-methoxybenzaldehyde Chemical compound COC1=CC=C(C=O)C=C1 ZRSNZINYAWTAHE-UHFFFAOYSA-N 0.000 claims abstract description 77
- WXCMHFPAUCOJIG-UHFFFAOYSA-N 4'-tert-Butyl-2',6'-dimethyl-3',5'-dinitroacetophenone Chemical compound CC(=O)C1=C(C)C([N+]([O-])=O)=C(C(C)(C)C)C([N+]([O-])=O)=C1C WXCMHFPAUCOJIG-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000203 mixture Substances 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000003921 oil Substances 0.000 claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 17
- 230000002000 scavenging effect Effects 0.000 claims abstract description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 15
- 241000228197 Aspergillus flavus Species 0.000 claims abstract description 14
- 241000228245 Aspergillus niger Species 0.000 claims abstract description 14
- 241000228153 Penicillium citrinum Species 0.000 claims abstract description 14
- 241000588724 Escherichia coli Species 0.000 claims abstract description 12
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 241000191967 Staphylococcus aureus Species 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 8
- -1 DPPH free radical Chemical class 0.000 claims abstract description 7
- 230000003385 bacteriostatic effect Effects 0.000 claims abstract description 7
- 239000001103 potassium chloride Substances 0.000 claims abstract description 6
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 6
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 240000009023 Myrrhis odorata Species 0.000 claims abstract 10
- 241000894006 Bacteria Species 0.000 claims description 61
- 230000000844 anti-bacterial effect Effects 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 235000013305 food Nutrition 0.000 claims description 9
- 239000003755 preservative agent Substances 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- 230000002335 preservative effect Effects 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 238000005292 vacuum distillation Methods 0.000 claims description 4
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 230000003064 anti-oxidating effect Effects 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000010902 straw Substances 0.000 claims description 2
- 241000193830 Bacillus <bacterium> Species 0.000 abstract description 15
- 239000003205 fragrance Substances 0.000 abstract description 6
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 240000004760 Pimpinella anisum Species 0.000 description 88
- 239000000243 solution Substances 0.000 description 25
- 239000000178 monomer Substances 0.000 description 20
- 239000010676 star anise oil Substances 0.000 description 18
- 239000000341 volatile oil Substances 0.000 description 18
- 239000000725 suspension Substances 0.000 description 16
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 15
- 230000002401 inhibitory effect Effects 0.000 description 13
- 230000008859 change Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 239000001963 growth medium Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 241000212314 Foeniculum Species 0.000 description 6
- 235000004204 Foeniculum vulgare Nutrition 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 6
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 240000007232 Illicium verum Species 0.000 description 4
- 235000008227 Illicium verum Nutrition 0.000 description 4
- 241001052560 Thallis Species 0.000 description 4
- 235000009754 Vitis X bourquina Nutrition 0.000 description 4
- 235000012333 Vitis X labruscana Nutrition 0.000 description 4
- 240000006365 Vitis vinifera Species 0.000 description 4
- 235000014787 Vitis vinifera Nutrition 0.000 description 4
- 239000004599 antimicrobial Substances 0.000 description 4
- 239000008280 blood Substances 0.000 description 4
- 210000004369 blood Anatomy 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 230000001408 fungistatic effect Effects 0.000 description 4
- 239000006916 nutrient agar Substances 0.000 description 4
- 239000002504 physiological saline solution Substances 0.000 description 4
- QTENRWWVYAAPBI-YCRXJPFRSA-N streptomycin sulfate Chemical compound OS(O)(=O)=O.OS(O)(=O)=O.OS(O)(=O)=O.CN[C@H]1[C@H](O)[C@@H](O)[C@H](CO)O[C@H]1O[C@@H]1[C@](C=O)(O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](N=C(N)N)[C@H](O)[C@@H](N=C(N)N)[C@H](O)[C@H]1O.CN[C@H]1[C@H](O)[C@@H](O)[C@H](CO)O[C@H]1O[C@@H]1[C@](C=O)(O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](N=C(N)N)[C@H](O)[C@@H](N=C(N)N)[C@H](O)[C@H]1O QTENRWWVYAAPBI-YCRXJPFRSA-N 0.000 description 4
- 229920001817 Agar Polymers 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 3
- 239000008272 agar Substances 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- VNFPBHJOKIVQEB-UHFFFAOYSA-N clotrimazole Chemical compound ClC1=CC=CC=C1C(N1C=NC=C1)(C=1C=CC=CC=1)C1=CC=CC=C1 VNFPBHJOKIVQEB-UHFFFAOYSA-N 0.000 description 3
- 229960004022 clotrimazole Drugs 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 210000002429 large intestine Anatomy 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000013641 positive control Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 3
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 3
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 2
- 241000722824 Ardisia crenata Species 0.000 description 2
- 244000063299 Bacillus subtilis Species 0.000 description 2
- 235000014469 Bacillus subtilis Nutrition 0.000 description 2
- 241001478240 Coccus Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 239000001888 Peptone Substances 0.000 description 2
- 108010080698 Peptones Proteins 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- 230000003260 anti-sepsis Effects 0.000 description 2
- 230000002421 anti-septic effect Effects 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 235000015278 beef Nutrition 0.000 description 2
- 235000019282 butylated hydroxyanisole Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 235000011194 food seasoning agent Nutrition 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 235000019319 peptone Nutrition 0.000 description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 2
- 229920000053 polysorbate 80 Polymers 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- 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
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000004255 Butylated hydroxyanisole Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 1
- 241000186031 Corynebacteriaceae Species 0.000 description 1
- 239000004278 EU approved seasoning Substances 0.000 description 1
- 206010016952 Food poisoning Diseases 0.000 description 1
- 208000019331 Foodborne disease Diseases 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 241000191940 Staphylococcus Species 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000003851 azoles Chemical class 0.000 description 1
- 230000000721 bacterilogical effect Effects 0.000 description 1
- 239000000022 bacteriostatic agent Substances 0.000 description 1
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 description 1
- 229940043253 butylated hydroxyanisole Drugs 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229930016911 cinnamic acid Natural products 0.000 description 1
- 235000013985 cinnamic acid Nutrition 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000012376 hot air sterilization Methods 0.000 description 1
- 238000009630 liquid culture Methods 0.000 description 1
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 235000012015 potatoes Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000013558 reference substance 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
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- RUVINXPYWBROJD-ONEGZZNKSA-N trans-anethole Chemical group COC1=CC=C(\C=C\C)C=C1 RUVINXPYWBROJD-ONEGZZNKSA-N 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT 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
- A23L3/3499—Organic compounds containing oxygen with doubly-bound oxygen
-
- 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)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Botany (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The method that the present invention prepares food preservative using Chinese anise oil extract waste liquid, from the water phase distillate flowed out in the oil water separator of oil of badian extractor or the water phase distillate that will be collected after the brown color muddiness waste liquid re-distillation in extractor, by the way that sodium chloride or potassium chloride is added, make the anisic aldehyde in water phase distillate, anise ketone musk and anisic acid mixture are precipitated, organic solvent is added to be extracted, then organic solvent is evaporated under reduced pressure, obtain pale yellow oily liquid, by this pale yellow oily liquid cryogenic freezing, crystallization is precipitated, quickly filtering obtains anisic aldehyde, anise ketone musk and anisic acid mixture, the mixture is to staphylococcus aureus, Escherichia coli, hay bacillus, aspergillus niger, aspergillus flavus and Penicillium citrinum have bacteriostatic activity, there is scavenging effect to DPPH free radical, and Fragrance is suitable for that can be used as food preservative.This method is easy to operate, it is environmentally friendly, at low cost, convenient for promoting the use of.
Description
Technical field
The present invention relates to a kind of method for preparing preservative, especially a kind of method for preparing food preservative.
Background technique
Chinese anise (Illicium verum Hook.f.) is referred to as octagonal, is commonly called as anise, the whole world is mainly distributed on east
Sub-, Southeast Asia and America, wherein with China be it is most, followed by Vietnam, Cambodia, Burma, Indonesia etc. is national and ground
Area.It is mainly distributed on a few provinces and regions such as Guangxi, Yunnan, Guangdong at home.Chinese anise is all Southern Subtropic Zone of China
The important economic tree in area is had widely by the essential oil product that Chinese anise is extracted in the industries such as flavors and fragrances and food
Purposes.
The production of star anise oil mostly uses greatly traditional steam distillation technique, general in steam distillation technique
It only collects oil phase part in distillate to be allocated as essential oil product, main component is trans-anethole, from oil of badian extractor
The brown color waste liquid in water phase distillate and oil of badian extractor flowed out in oil water separator is usually discarded.In essential oil
Production process in due to essential oil molecule in distillation process with vapor keep for a long time contact, so the polarity in essential oil and
Hydrophilic composition partly dissolves in water, as the water-soluble volatile ingredient of essential oil.This part is slightly soluble in the volatile component of water,
The mainly containing oxygen derivative of terpene substances, these substances give off a strong fragrance, and represent the distinctive fragrance of essential oil, are most had in essential oil
The part of value, and since the oil-water ratio of distillate is small, this Some essential oils is suitable entirely distillating ratio shared in essential oil
Considerable.
As people gradually deepen the understanding of water-soluble volatile ingredient, find water-soluble volatile ingredient due to rich in oxygen-containing
Not only there is terpenoid aromatic odor can be applied to cosmetics and food additives, but also have antibacterial, antiviral etc. raw
Object active function, has broad application prospects.The water-soluble volatile ingredient in spice berry is usually with vinasse at present
And discarded, cause huge waste.Therefore extraction and research for application and development in relation to volatile ingredient water-soluble in spice berry
Increasingly by attention both domestic and external.
Food preservative is generally divided into chemical synthesis preservative and natural antiseptic agent.The still benzene that China largely uses at present
Formic acid and its chemical syntheses preservative such as salt, sorbic acid and its salt, parabens.Through long-term application and research hair
The problems such as existing some synthetic preservatives lure carcinous, teratogenesis and easily cause food poisoning.Long-term consumption or the excessive appearance of amount
Easily in people's internal deposition, therefore there is carcinogenic possibility.And in the production process of synthetic preservative, poison gas can have been generated
Body has certain harm to the working environment of people, and be easy to cause environmental pollution.A large amount of result of study shows one in recent years
A little natural plants and its extract have certain antiseptic and inhibiting bacteria function effect.Natural antiseptic agent is harmful to human health, the peace used
Full property has also sufficiently been confirmed.
Summary of the invention
The purpose of the present invention is in view of the above-mentioned drawbacks of the prior art, providing a kind of useless using Chinese anise oil extract
The method that liquid prepares food preservative, this method is environmentally friendly, it is at low cost, there is antibacterial antioxidation, convenient for promoting the use of, and institute
Food preservative obtained is the suitable natural food antiseptic agent of fragrance.
The present invention to achieve the above object the technical solution adopted is that: it is anti-to prepare food using Chinese anise oil extract waste liquid
The method of rotten agent, includes the following steps:
A. extraction anisic aldehyde, anise ketone musk and anisic acid mixture from Chinese anise oil extract waste liquid, including with
Lower step:
(1) water phase distillate is collected, water phase distillate is flowed out from the oil water separator of oil of badian extractor
Water phase distillate, or the water phase collected after the brown color muddiness waste liquid re-distillation in Chinese anise oil extractor is distillated
Liquid；
(2) sodium chloride or potassium chloride are added into water phase distillate acquired by step (1), makes big in water phase distillate
Anisaldehyde, anise ketone musk and anisic acid are precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is
Methylene chloride or petroleum ether or n-hexane or acetone or ethyl acetate, organic solvent are with the water phase distillate volume ratio taken
1/10, organic solvent phase is taken after extraction；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, obtains pale yellow oily liquid；
(5) cryogenic freezing is carried out to pale yellow oily liquid acquired by step (4), wait which crystallization is precipitated, rapid filtration under suction is
Anisic aldehyde, anise ketone musk and anisic acid mixture are obtained, the content of anisic aldehyde is 56~67%, anise in mixture
The content of ketone is 17~20%, the content of anisic acid is 5~8%；
B. prepared anisic aldehyde, anise ketone musk and the anisic acid mixture obtained of above-mentioned steps a, has stronger antibacterial
Antioxidant activity can be used as food using the anisic aldehyde, anise ketone musk and the anisic acid mixture that obtain prepared by above-mentioned steps a
Preservative.
The further technical solution that the present invention uses is: the amount of sodium chloride or potassium chloride being added in the step (2) are as follows: make
The 30~70% of concentration when the concentration of sodium chloride or Klorvess Liquid is saturation solubility.
The further technical solution that the present invention uses is: the vacuum distillation in the step (4) are as follows: in temperature be 55 DEG C~
It is evaporated under reduced pressure under conditions of 85 DEG C by Rotary Evaporators.
The further technical solution that the present invention uses is: the temperature of the cryogenic freezing in the step (5) is -10 DEG C
~-30 DEG C, cooling time is 5~10 hours.
The further technical solution that the present invention uses is: anisic aldehyde, anise ketone musk and anisic acid mixture are to golden yellow
Color staphylococcus, Escherichia coli, hay bacillus, aspergillus niger, aspergillus flavus and Penicillium citrinum have bacteriostatic activity, to DPPH free radical
With scavenging effect, food preservative can be used as.
Due to the adoption of the above technical scheme, the side that food preservative is prepared using Chinese anise oil extract waste liquid of the present invention
Method compared with prior art, has the advantages that
1. having antisepsis:
The present invention is anisic aldehyde, anise ketone musk and the anise extracted from Chinese anise oil extract waste liquid using raw material
Acid blend has good antisepsis, to Escherichia coli, hay bacillus, staphylococcus aureus, aspergillus niger, aspergillus flavus
There is bacteriostatic activity with the common pathogen in the food and environment such as Penicillium citrinum, there is scavenging effect to DPPH free radical.
2. fragrance is suitable for, suitable for the use in food:
Chinese anise acrid-sweet flavor, pleasantly sweet and strong aromatic odor are the most common seasonings of family, are largely used to eat
Product seasoning and non-staple foodstuff processing.Anisic aldehyde, anise ketone musk and the anisic acid mixing extracted from Chinese anise oil extract waste liquid
Object also has octagonal characteristic perfume, suitable for using food antiseptic.
3. reducing costs, being small to human body toxic side effect:
And main material used in the present invention is the anisic aldehyde extracted from Chinese anise oil extract waste liquid, anise
Ketone and anisic acid mixture belong to natural antiseptic agent of plant source, are the artificial synthesized anti-of representative with potassium sorbate, sodium benzoate
Rotten agent is compared, small to the toxic side effect of human body；Meanwhile the cost of raw material is on the one hand greatly reduced, another aspect Chinese anise
Oil extract waste liquid is typically all to be discharged into environment as waste liquid, and the present invention carries out the Chinese anise oil extract waste liquid
It recycles, increases the comprehensive utilization value of Chinese anise.
4. method is simple and convenient to operate:
Main material used in the present invention is not only the nothing flowed out from the oil water separator of oil of badian extractor
Color transparency liquid water phase distillate, that is, the remaining distilled water after isolating oil of badian can also be and collects Chinese anise
Brown color muddiness vinasse in oil extractor, then by this vinasse re-distillation, collect distillate, other raw material
Existing material in the market, and the present invention use mainly comprise the following steps solution modeling, extraction, vacuum distillation and mixed dissolution etc.
Some simple chemical methodes, method are simple and convenient to operate, convenient for popularization and use.
Prepare the side of food preservative using Chinese anise oil extract waste liquid to the present invention with reference to the accompanying drawings and examples
Method is further described.
Detailed description of the invention
Fig. 1 is that anisic aldehyde, anise ketone musk and anisic acid mixture change feelings with concentration to the scavenging effect of DPPH
Condition；
Fig. 2 is for star anise oil to the scavenging effect of DPPH with concentration situation of change；
Fig. 3 is for anisic aldehyde to the scavenging effect of DPPH with concentration situation of change；
Fig. 4 is for anise ketone musk to the scavenging effect of DPPH with concentration situation of change.
Specific embodiment
The method that the present invention prepares food preservative using Chinese anise oil extract waste liquid, includes the following steps:
A. extraction anisic aldehyde, anise ketone musk and anisic acid mixture from Chinese anise oil extract waste liquid, including with
Lower step:
(1) water phase distillate is collected, water phase distillate is flowed out from the oil water separator of oil of badian extractor
Water phase distillate, or the water phase collected after the brown color muddiness waste liquid re-distillation in oil of badian extractor is distillated
Liquid；The water phase distillate wherein flowed out in the oil water separator of oil of badian extractor is colourless transparent liquid, to isolate
Remaining distilled water after oil of badian, the volatile component of Chinese anise is dissolved in this water, and main component is anise
Fragrant aldehyde, anise ketone musk and anisic acid；Wherein collected after the brown color muddiness waste liquid re-distillation in Chinese anise oil extractor
Water phase distillate be colourless or micro-strip light yellow liquid, the volatile component of Chinese anise is dissolved in this water, mainly at
Divide also is anisic aldehyde, anise ketone musk and anisic acid；
(2) sodium chloride or potassium chloride are added into water phase distillate acquired by step (1), wherein sodium chloride or chlorine is added
Change the amount of potassium are as follows: the 50% of concentration when making the concentration saturation solubility of sodium chloride or Klorvess Liquid；Make in water phase distillate
Anisic aldehyde, anise ketone musk and anisic acid be precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is
Methylene chloride or petroleum ether or n-hexane or acetone or ethyl acetate, organic solvent are with the water phase distillate volume ratio taken
1/10, organic solvent phase is taken after extraction；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, is being evaporated under reduced pressure specifically: be in temperature
It is evaporated under reduced pressure under conditions of 55 DEG C~85 DEG C by Rotary Evaporators；Pale yellow oily liquid is obtained after vacuum distillation；
(5) cryogenic freezing is carried out to pale yellow oily liquid acquired by step (4), the temperature of cryogenic freezing is -10 DEG C
~-30 DEG C, cooling time is 5~10 hours, and wait which crystallization is precipitated after cryogenic freezing, rapid filtration under suction is up to anisic aldehyde, anise
Ketone musk and anisic acid mixture, in mixture the content of anisic aldehyde be 56~67%, the content of anise ketone musk be 17~
20%, the content of anisic acid is 5~8%；
B. prepared anisic aldehyde, anise ketone musk and the anisic acid mixture obtained of above-mentioned steps a, has stronger antibacterial
Antioxidant activity, it was proved that anisic aldehyde, anise ketone musk and anisic acid mixture are to staphylococcus aureus, large intestine
Bacillus, hay bacillus, aspergillus niger, aspergillus flavus and Penicillium citrinum have bacteriostatic activity, have scavenging effect to DPPH free radical, make
Anisic aldehyde, anise ketone musk and the anisic acid mixture obtained prepared by above-mentioned steps a is used as food preservative.
1. proposing the suppression of the anisic aldehyde extracted in oily waste liquid, anise ketone musk and anisic acid mixture from oil of badian
Bacterium experiment
1.1 experimental method
1.1.1 for trying strain
Aspergillus flavus (Aspergillus flavus), aspergillus niger (Aspergillus niger), Penicillium citrinum
(Penicillium citrinum), Escherichia coli (Escherichia coli), staphylococcus aureus
(Staphylococus aureus), bacillus subtilis (Bacillus subtilis).
1.1.2 culture medium
PDA culture medium (mould use) (g/L): peeled potatoes 200g, glucose 20g, agar 15g, natural ph.
Nutrient agar (bacterium use) (g/L): peptone 10g, beef extract powder 3g, sodium chloride 5g, agar powder 15g,
pH7.3±0.1。
Nutrient broth medium (bacterial liquid culture use) (g/L): peptone 10g, beef extract powder 3g, sodium chloride 5g,
pH7.3±0.1。
Culture medium containing candidate drug (bacterium, mould use): nutrient agar (bacterium) or PDA culture medium (mould),
Tween 80, candidate drug.
1.1.3 related solution
Physiological saline, streptomycin sulphate for injection solution (1.35mg/mL), clotrimazole solution (3mg/mL).
1.1.4 the preparation of culture medium
Firstly, doing 50 bottles of nutrient agar, 2% Tween-80 is added, shakes up, wraps up, moist heat sterilization at 121 DEG C
20min；Then, on superclean bench, anisic aldehyde, anise ketone musk and anisic acid is added by the concentration gradient of following table 1
Mixture (or star anise oil, streptomycin sulphate, clotrimazole), jog to inverted plate after even, every bottle is fallen 3 wares, on plate
Corresponding label is sticked, is laid flat to solidifying.Three groups are finished to doing three groups of antibacterial tests to mould after the antibacterial tests of bacterium again.Battalion
It supports agar to replace for PDA culture medium, the moist heat sterilization 30min at 115 DEG C.
Table 1: contained anisic aldehyde, anise ketone musk and anisic acid mixture, star anise oil and the positive in culture medium
The concentration of reference substance
1.1.5 the preparation of bacteria suspension
(1) preparation of bacterium bacteria suspension
A. the preparation of liquid is planted
Strain picks them separately a ring lawn in nutrient broth medium after slant activation 2~3 times, with oese, mixes
Even (every kind of strain prepares 3 bottles), is placed in shaking table, 37 DEG C of temperature control, revolving speed 130rpm, culture is for 24 hours, spare as strain liquid.
B. the extension rate of strain liquid is determined
9mL physiological saline is accurately drawn respectively with 10mL pipette in numbered sterile test tube.It first shakes to be diluted
Meat soup bacterium solution to uniform, then with 1 sterile pipette pipe, for several times, then the accurate 1mL that draws is in 10 for pressure-vaccum back and forth in bacterium solution-1Examination
(note: the tip of pipette cannot contact 10 in pipe-1Bacterium solution) concussion is uniform.The sterile pipette pipe of 1 1mL is taken, separately with same
Mode, 10-1Bacterium solution in purge back and forth for several times, accurate 1mL bacterium solution of drawing is to 10-2Guan Zhong, and so on.10 are taken respectively-5、10-6、10-7、10-8Bacteria suspension 0.1mL is coated in 37 DEG C of cultures for 24 hours.Original bacteria liquid concentration is calculated according to flat-plate bacterial colony number.
Total bacteria count cfu/mL=average colony number × extension rate × 10
According to count of bacteria as a result, dilute the strain liquid of each bacterium, it is made into final concentration of 108The Escherichia coli of cfu/mL,
Staphylococcus aureus suspension and 106The hay bacillus suspension of cfu/mL.
C. bacteria suspension is prepared
9mL physiological saline is accurately drawn respectively with 10mL pipette in numbered sterile test tube.It first shakes to be diluted
Bacterium solution to uniform, then with 1 sterile pipette pipe, for several times, then the accurate 1mL that draws is in 10 for pressure-vaccum back and forth in bacterium solution-1Test tube
In (note: the tip of pipette cannot contact 10-1Bacterium solution).The sterile pipette pipe of 1 1mL is separately taken, in the same way,
10-1Bacterium solution in purge back and forth for several times, accurate 1mL bacterium solution of drawing is to 10-2Guan Zhong, and so on, until what is determined in (2) is dilute
Until degree of releasing.
(2) preparation of mycotic spore suspension
After strain is carried out slant activation 2~3 times, 48h is cultivated, it is spare.
The mycotic spore on inclined-plane is eluted with physiological saline, after vibrating so that spore is fully dispersed, as mould
The spore suspension of bacterium.The counting of spore suspension is carried out with blood counting chamber.Take spore suspension, the appropriate dilution of progress.Take drying
Clean blood counting chamber covered, spore suspension is dripped a droplet by coverslip edge with sterile dropper (should not mistake
It is more), it allows spore suspension voluntarily to penetrate into, pays attention to cannot thering is bubble generation.5min is stood, blood counting chamber is placed in microscope and is carried
On object platform, several bacterium are carried out.The specification for the blood counting chamber that this experiment uses is 25 × 16, total bacteria count in every milliliter of bacterium solution are as follows:
Total bacteria count
Note: X indicates the spore count per small lattice
According to mycotic spore count as a result, dilute the strain liquid of each mould, be made into final concentration of 106The spore of cfu/mL
Suspension.
1.1.6 the measurement of inhibition zone
Using filter paper enzyme measurement anisic aldehyde, anise ketone musk and anisic acid mixture inhibition zone, and with octagonal fennel
Essential oil, anisic aldehyde, anise ketone musk experimental result compare, with streptomycin sulphate for injection (to bacterium) and clotrimazole
(to mould) makees positive control, and process is as follows:
Prepare filter paper: with the stronger and homogeneous double-layer filter paper of water absorbing force, breaking into the circle that diameter is 6mm with punch
Shape filter paper, sets in the culture dish of clean dried, 1~2h of hot air sterilization at 150~170 DEG C.
Culture medium: bacterium uses nutrient agar, and mould uses PDA culture medium.
Specific experiment process: prepared bacteria suspension is shaken uniformly, on ultrapurification aseptic working platform, with sterile liquid relief
Rifle draw bacterium solution 0.1mL, it is equably coated on to planar surface, just setting incubator 1h (37 DEG C of bacteriological incubator temperature, it is mould
28 DEG C of bacterium incubator temperature).It is got after 1h on ultrapurification aseptic working platform, is put into 3 filter papers in positive triangle in each plate,
Then various sample to be tested 10ul are drawn with sterile liquid-transfering gun again to be vertically added drop-wise on filter paper.Bacterium is just setting training in 37 DEG C of constant temperature
Culture is inverted for 24 hours after supporting 1h, and mould is inverted culture 48h after 28 DEG C of constant temperature are just setting culture 1h, observes antibacterial situation, and measure suppression
Bacterium loop diameter, is averaged, and evaluates its fungistatic effect with this.
1.1.7 the measurement of minimal inhibitory concentration (MIC)
Using the minimal inhibitory concentration (MIC) of plate dilution assay method trans-cinnamaldehyde and cortex cinnamomi acid blend, and and meat
Osmanthus essential oil, trans-cinnamaldehyde, cinnamic acid experimental result compare, experimental method is as follows:
On clean work station, bacterium bacteria suspension or spore suspension 0.1mL are drawn with sterile liquid-transfering gun, is injected according to label
In the culture medium containing candidate drug solidified, it is equably coated on planar surface, it is (37 DEG C of bacterium, mould to set certain temperature
28 DEG C of bacterium) under, after culture certain time (Bacteria Culture for 24 hours, mycotic culture 48h), the growing state of observation test bacterium.With complete
Minimal inhibitory concentration MIC of the Cmin for not having bacterium to grow as every kind of medicine to different bacterium.Blank pair is set up during test
According to.
1.1.8 the measurement of minimum bactericidal concentration (MBC)
Anti-microbial property is studied, it is also necessary to which bactericidal properties size is judged by the minimum bactericidal concentration (MBC) of measurement.Its
Process are as follows: not having the plate of long bacterium to continue to cultivate in 1.1.7, bacterium is further cultured for for 24 hours, and mould is further cultured for 48h, takes out observation knot
Fruit.Originally there may be long bacterium phenomenon without the plate of long bacterium, and be that minimum bactericidal is dense with the minimum concentration that absolutely not bacterium grows
Spend MBC.
1.2 experimental result
1.2.1 anisic aldehyde, anise ketone musk and the suppression of anisic acid mixture extracted from Chinese anise oil extract waste liquid
Bacterium determination of activity
The anisic aldehyde, anise ketone musk and anise extracted from Chinese anise oil extract waste liquid is determined using filter paper enzyme
Fragrant acid blend, star anise oil and anisic aldehyde, anise one monomers are to for trying bacterium staphylococcus aureus, large intestine bar
Bacterium, hay bacillus, aspergillus niger, aspergillus flavus and Penicillium citrinum bacteriostatic activity, and with streptomycin sulphate for injection (to bacterium) and gram
Mould azoles (to mould) makees positive control, is as a result listed in following table 2.
Table 2: the fungistatic effect (unit: millimeter) of anisic aldehyde, anise ketone musk and anisic acid mixture
Note :-indicate not doing corresponding test, no data.
From table 2 it can be seen that anisic aldehyde, anise ketone musk and anisic acid mixture are to golden yellow grape bacillus, large intestine
Bacillus, hay bacillus, aspergillus niger, Penicillium citrinum, aspergillus flavus have good inhibiting effect.Anisic aldehyde, anise ketone musk and anise
Fragrant acid blend to golden yellow grape bacillus, Escherichia coli, hay bacillus, aspergillus niger, Penicillium citrinum, aspergillus flavus antibacterial circle diameter
Size respectively be 13.5mm, 13.8mm, 18.5mm, 30.9mm, 33.3mm, 29.9mm；Star anise oil is to above-mentioned
Size for trying bacterium antibacterial circle diameter respectively is 9.2mm, 9.2mm, 11.8mm, 14.8mm, 17.8mm, 13.6mm.
Anisic aldehyde, anise ketone musk and anisic acid mixture are both greater than Chinese anise to each antibacterial circle diameter for trying bacterium
Essential oil illustrates to extract the anisic aldehyde, anise ketone musk and the anisic acid mixture that extract in waste liquid from star anise oil to institute
There is the fungistatic effect for trying bacterium to be all higher than star anise oil.
Anisic aldehyde, anise ketone musk and anisic acid mixture are all significantly greater than anise to each antibacterial circle diameter for trying bacterium
Fragrant aldehyde, anise one monomers illustrate to extract anisic aldehyde, anise ketone musk and the anise extracted in waste liquid from star anise oil
Acid blend is apparently higher than anisic aldehyde monomer and anise one monomers to all fungistatic effects for trying bacterium.
1.1.2 anisic aldehyde, anise ketone musk and the anisic acid mixture extracted from Chinese anise oil extract waste liquid
Minimal inhibitory concentration
Using anisic aldehyde, the anise ketone musk and big extracted from Chinese anise oil extract waste liquid with plate dilution assay method
Fennel acid blend, star anise oil and anisic aldehyde, anise one monomers are to staphylococcus aureus, Escherichia coli, withered
Straw bacterium, aspergillus niger, aspergillus flavus and Penicillium citrinum minimal inhibitory concentration, be as a result listed in following table 3.
Table 3: anisic aldehyde, anise ketone musk and anisic acid mixture and star anise oil are to the various minimums for trying bacterium
Mlc (MIC)
Note :-: indicate not long bacterium；+: indicate thallus dotted (bulk) growth；++: it is small that thalli growth area accounts for platen area
In 25%；+++: thalli growth area accounts for platen area 25%~50%；++++: thalli growth area account for platen area 50%~
75%；+++ ++: thalli growth area accounts for platen area 75%~100%
From table 3 it can be seen that anisic aldehyde, anise ketone musk and anisic acid mixture are to Escherichia coli, golden yellow grape
Coccus, hay bacillus, Penicillium citrinum, aspergillus niger, aspergillus flavus have certain inhibiting effect, to Escherichia coli, Staphylococcus aureus
Bacterium, three kinds of the hay bacillus minimal inhibitory concentrations for trying bacterium are 5~20mL/L；To Penicillium citrinum, aspergillus niger and three kinds of aspergillus flavus
Minimal inhibitory concentration for trying mould is 1.25~2.5mL/L.
Anisic aldehyde, anise ketone musk and anisic acid mixture are below Chinese anise to the minimal inhibitory concentration of test bacterium
The minimal inhibitory concentration of essential oil, anisic aldehyde monomer, anise one monomers to test bacterium, anisic aldehyde, anise ketone musk and anise
The bacteriostatic activity of fragrant acid blend is better than star anise oil, anisic aldehyde monomer, anise one monomers.
1.2.3 anisic aldehyde, anise ketone musk and the anisic acid mixture extracted from Chinese anise oil extract waste liquid
Minimum bactericidal concentration (MBC)
Minimum bactericidal concentration can accurately reflect the anti-microbial property of bacteriostatic agent, not have long bacterium after measuring minimal inhibitory concentration
Plate continue to cultivate the corresponding time (bacterium is further cultured for for 24 hours, and mould is further cultured for 48h), record is useless from Chinese anise oil extract
The minimum bactericidal concentration of the anisic aldehyde, anise ketone musk and anisic acid mixture that extract in liquid, is as a result listed in following table 4.
Table 4: anisic aldehyde, anise ketone musk and anisic acid mixture and star anise oil to it is various for examination bacterium most
Small bacteriocidal concentration (MBC)
From table 4, it can be seen that anisic aldehyde, anise ketone musk and anisic acid mixture are to Escherichia coli, golden yellow grape
Coccus, hay bacillus, Penicillium citrinum, aspergillus niger and aspergillus flavus bacteriocidal concentration be respectively 20ml/L, 40ml/L, 10ml/L, 5ml/
L,2.5ml/L,2.5ml/L；Anisic aldehyde, anise ketone musk and anisic acid mixture are greater than illiciumverum to the bactericidal activity for trying bacterium
Fennel essential oil, anisic aldehyde monomer, anise one monomers.
2. the antioxygen of the anisic aldehyde extracted in Chinese anise oil extract waste liquid, anise ketone musk and anisic acid mixture
Change experiment
The antioxygenic property of method evaluation anisic aldehyde, anise ketone musk and anisic acid mixture is removed using DPPH, and
It is compared with the antioxygenic property of star anise oil.
2.1 experimental method
The anisic aldehyde, anise ketone musk and anisic acid mixture, illiciumverum that will be extracted in Chinese anise oil extract waste liquid
Fennel essential oil, anisic aldehyde monomer, anise one monomers, respectively using dehydrated alcohol as solvent be configured to various concentration (20~
Solution 800mg/mL).Precise DPPH solid, and being made into concentration is 2 × 10-2The ethanol solution of mg/mL,
Pay attention to being kept in dark place.2mLDPPH solution is sequentially added into 5.0mL tool plug test tube, adds a certain amount of different volumes
Sample is added with dehydrated alcohol to 4.0mL scale, is sufficiently mixed uniformly.Timing is started simultaneously at, reference is made with dehydrated alcohol,
(maximum absorption wave strong point) measures different sample solutions in the absorbance of various time points, preferably to reflect change at 517nm
The concentration of change trend experimental selection is determined substantially according to double dilution method, and absorbance is surveyed 3 times and is averaged, when determining hybrid reaction
Between be 1h.
Defining sample antioxidant is the clearance rate to DPPH free radical are as follows:
S%=[1- (Ai-Aj)/Ac] × 100
Wherein: Ai=2mLDPPH solution+each sample absorbance；
Aj=each sample solution does not add background absorbance when DPPH solution in system；
The absorbance of Ac=2mLDPPH solution+2mL dehydrated alcohol.
This experiment makees positive control with tert-butyl hydroquinone (TBHQ) and butylated hydroxy anisole (BHA).
2.2 experimental result
Fig. 1 is that anisic aldehyde, anise ketone musk and anisic acid mixture change feelings with concentration to the scavenging effect of DPPH
Condition, Fig. 2 be star anise oil to the scavenging effect of DPPH with concentration situation of change, Fig. 3 is anisic aldehyde to DPPH's
Scavenging effect with concentration situation of change, Fig. 4 be anise ketone musk to the scavenging effect of DPPH with concentration situation of change, can be clear
Ground finds out under experimental conditions, anisic aldehyde, anise ketone musk and anisic acid mixture, star anise oil, anisic aldehyde list
Body, anise one monomers all have certain Scavenging activity to DPPH free radical, and with the increase of concentration, clearance rate
It gradually increases.
Anisic aldehyde, anise ketone musk and anisic acid mixture, star anise oil, anisic aldehyde monomer, anise ketone musk
Monomer is to there is a certain amount to imitate relationship between the clearance rate and concentration of DPPH, when usually with the clearance rate of DPPH up to 50%,
Concentration (the IC of antioxidant sample50) Scavenging activity of the Lai Hengliang sample to DPPH, IC50It is worth smaller, shows that its is right
The Scavenging activity of DPPH is stronger.From the available anisic aldehyde of FIG. 1 to FIG. 4, anise ketone musk and anisic acid mixture, illiciumverum
Fennel essential oil, anisic aldehyde monomer, anise one monomers IC50Value, is listed in following table 5.
Table 5: anisic aldehyde, anise ketone musk and anisic acid mixture remove the ability (IC of DPPH50)
| Antioxidant sample | IC50(mg/mL) |
| Anisic aldehyde, anise ketone musk and anisic acid mixture | 4.34 |
| Star anise oil | 19.03 |
| Anisic aldehyde | 38.13 |
| Anise ketone musk | 12.35 |
| TBHQ | 3.90×10-4 |
| BHA | 3.13×10-3 |
As can be seen from Table 5, the antioxidant activity of anisic aldehyde, anise ketone musk and anisic acid mixture is better than octagonal fennel
Essential oil, anisic aldehyde monomer, anise one monomers.
Claims (5)
1. a kind of method for preparing food preservative using Chinese anise oil extract waste liquid, it is characterised in that: include the following steps:
A. anisic aldehyde, anise ketone musk and anisic acid mixture, including following step are extracted from Chinese anise oil extract waste liquid
It is rapid:
(1) water phase distillate is collected, water phase distillate is the water phase flowed out from the oil water separator of oil of badian extractor
Distillate, or the water phase distillate that will be collected after the brown color muddiness waste liquid re-distillation in oil of badian extractor；
(2) sodium chloride or potassium chloride are added into water phase distillate acquired by step (1), makes the anise in water phase distillate
Aldehyde, anise ketone musk and anisic acid are precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is dichloro
Methane or petroleum ether or n-hexane or acetone or ethyl acetate, organic solvent are 1/ with the water phase distillate volume ratio taken
10, organic solvent phase is taken after extraction；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, obtains pale yellow oily liquid；
(5) cryogenic freezing is carried out to pale yellow oily liquid acquired by step (4), wait which crystallization is precipitated, rapid filtration under suction is obtained
Anisic aldehyde, anise ketone musk and anisic acid mixture, the content of anisic aldehyde is containing for 56 ~ 67%, anise ketone musk in mixture
Amount is that the content of 17 ~ 20%, anisic acid is 5 ~ 8%；
B. the preparation-obtained anisic aldehyde of above-mentioned steps a, anise ketone musk and anisic acid mixture have stronger antibacterial anti-
Oxidation activity can be used as food using the preparation-obtained anisic aldehyde of above-mentioned steps a, anise ketone musk and anisic acid mixture
Preservative.
2. the method according to claim 1 for preparing food preservative using Chinese anise oil extract waste liquid, feature exist
In: the amount of sodium chloride or potassium chloride is added in the step (2) are as follows: make the saturation dissolution of the concentration of sodium chloride or Klorvess Liquid
The 30 ~ 70% of concentration when spending.
3. the method according to claim 1 for preparing food preservative using Chinese anise oil extract waste liquid, feature exist
In: the vacuum distillation in the step (4) are as follows: depressurized under conditions of being 55 DEG C ~ 85 DEG C in temperature by Rotary Evaporators
Distillation.
4. the method according to claim 1 for preparing food preservative using Chinese anise oil extract waste liquid, feature exist
In: the temperature of the cryogenic freezing in the step (5) is -10 DEG C ~ -30 DEG C, and cooling time is 5~10 hours.
5. preparing food preservative using Chinese anise oil extract waste liquid described in any claim according to claim 1 ~ 4
Method, it is characterised in that: anisic aldehyde, anise ketone musk and anisic acid mixture are to staphylococcus aureus, Escherichia coli, withered
Straw bacterium, aspergillus niger, aspergillus flavus and Penicillium citrinum have bacteriostatic activity, have scavenging effect to DPPH free radical, can be used as food
Savor preservative.
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Citations (2)
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|---|---|---|---|---|
| CN101411365A (en) * | 2008-11-14 | 2009-04-22 | 广东工业大学 | Recombinant aromatic condiment essential oil with oxidation resistance function and use method thereof |
| CN105124716A (en) * | 2015-07-23 | 2015-12-09 | 广西科技大学 | Method of preparing food preservative through extraction waste liquid of cinnamon oil |
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- 2019-07-16 CN CN201910642507.XA patent/CN110301572A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101411365A (en) * | 2008-11-14 | 2009-04-22 | 广东工业大学 | Recombinant aromatic condiment essential oil with oxidation resistance function and use method thereof |
| CN105124716A (en) * | 2015-07-23 | 2015-12-09 | 广西科技大学 | Method of preparing food preservative through extraction waste liquid of cinnamon oil |
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| 王同禹，等: "八角茴香水溶性挥发成分的抑菌活性研究", 《中国调味品》 * |
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