CN107653064A - A kind of inoxidizability is strong, the preparation method and applications of high fragrance Rome yellow chamomile fermentation absolute oil - Google Patents
A kind of inoxidizability is strong, the preparation method and applications of high fragrance Rome yellow chamomile fermentation absolute oil Download PDFInfo
- Publication number
- CN107653064A CN107653064A CN201710889766.3A CN201710889766A CN107653064A CN 107653064 A CN107653064 A CN 107653064A CN 201710889766 A CN201710889766 A CN 201710889766A CN 107653064 A CN107653064 A CN 107653064A
- Authority
- CN
- China
- Prior art keywords
- rome
- yellow chamomile
- fermentation
- fragrance
- chamomile
- 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
- 240000008632 Cota tinctoria Species 0.000 title claims abstract description 75
- 238000000855 fermentation Methods 0.000 title claims abstract description 48
- 230000004151 fermentation Effects 0.000 title claims abstract description 48
- 239000003205 fragrance Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003921 oil Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 33
- 102000004190 Enzymes Human genes 0.000 claims abstract description 32
- 108090000790 Enzymes Proteins 0.000 claims abstract description 32
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 28
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims abstract description 13
- 239000002893 slag Substances 0.000 claims abstract description 12
- 238000000899 pressurised-fluid extraction Methods 0.000 claims abstract description 8
- 239000000341 volatile oil Substances 0.000 claims abstract description 8
- 238000001256 steam distillation Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 229940088598 enzyme Drugs 0.000 claims description 31
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- 241000208125 Nicotiana Species 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 230000000694 effects Effects 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 108010047754 beta-Glucosidase Proteins 0.000 claims description 10
- 102000006995 beta-Glucosidase Human genes 0.000 claims description 10
- 230000007062 hydrolysis Effects 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 10
- 108010059892 Cellulase Proteins 0.000 claims description 9
- 108010036940 Levansucrase Proteins 0.000 claims description 9
- 229940106157 cellulase Drugs 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 108091005508 Acid proteases Proteins 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 7
- -1 pectase Proteins 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 230000002195 synergetic effect Effects 0.000 claims description 5
- 230000033228 biological regulation Effects 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 102000004547 Glucosylceramidase Human genes 0.000 claims description 2
- 108010017544 Glucosylceramidase Proteins 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims 1
- 241000723353 Chrysanthemum Species 0.000 abstract description 27
- 235000007516 Chrysanthemum Nutrition 0.000 abstract description 27
- 150000001875 compounds Chemical class 0.000 abstract description 16
- 239000002304 perfume Substances 0.000 abstract description 15
- 239000001960 chamomile flower oil england Substances 0.000 abstract description 11
- 239000002253 acid Substances 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 7
- 239000000796 flavoring agent Substances 0.000 abstract description 6
- 235000019634 flavors Nutrition 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000000638 stimulation Effects 0.000 abstract description 3
- 244000061176 Nicotiana tabacum Species 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 15
- 239000004615 ingredient Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 10
- 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 9
- 239000000463 material Substances 0.000 description 9
- 230000031700 light absorption Effects 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 150000004676 glycans Chemical class 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 229940119217 chamomile extract Drugs 0.000 description 5
- 235000020221 chamomile extract Nutrition 0.000 description 5
- 239000000284 extract Substances 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 229930003935 flavonoid Natural products 0.000 description 5
- 150000002215 flavonoids Chemical class 0.000 description 5
- 235000017173 flavonoids Nutrition 0.000 description 5
- 239000003546 flue gas Substances 0.000 description 5
- 229920001282 polysaccharide Polymers 0.000 description 5
- 239000005017 polysaccharide Substances 0.000 description 5
- IRZWAJHUWGZMMT-UHFFFAOYSA-N 4,6,6-trimethylbicyclo[3.1.1]hept-3-en-7-ol Chemical group CC1=CCC2C(C)(C)C1C2O IRZWAJHUWGZMMT-UHFFFAOYSA-N 0.000 description 4
- 235000009508 confectionery Nutrition 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 230000001953 sensory effect Effects 0.000 description 4
- 150000003384 small molecules Chemical class 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- MBDOYVRWFFCFHM-SNAWJCMRSA-N (2E)-hexenal Chemical compound CCC\C=C\C=O MBDOYVRWFFCFHM-SNAWJCMRSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 241000510678 Falcaria vulgaris Species 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010835 comparative analysis Methods 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 238000001785 headspace extraction Methods 0.000 description 2
- 235000012907 honey Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- RUVINXPYWBROJD-ONEGZZNKSA-N trans-anethole Chemical compound COC1=CC=C(\C=C\C)C=C1 RUVINXPYWBROJD-ONEGZZNKSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- ITYNGVSTWVVPIC-DHGKCCLASA-N (-)-allo-Aromadendrene Chemical compound C([C@@H]1[C@H]2C1(C)C)CC(=C)[C@@H]1[C@H]2[C@H](C)CC1 ITYNGVSTWVVPIC-DHGKCCLASA-N 0.000 description 1
- 101800000263 Acidic protein Proteins 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- 241001558019 Euryops pectinatus Species 0.000 description 1
- 240000006927 Foeniculum vulgare Species 0.000 description 1
- 235000004204 Foeniculum vulgare Nutrition 0.000 description 1
- 229940123457 Free radical scavenger Drugs 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- YKVWPZJHENXDAJ-VOTSOKGWSA-N Megastigmatrienone Chemical compound CC1=CC(=O)CC(C)(C)C1\C=C\C=C YKVWPZJHENXDAJ-VOTSOKGWSA-N 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- 244000299461 Theobroma cacao Species 0.000 description 1
- 235000009470 Theobroma cacao Nutrition 0.000 description 1
- 241001505102 Valeriana fauriei Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 229940011037 anethole Drugs 0.000 description 1
- 230000003474 anti-emetic effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000002111 antiemetic agent Substances 0.000 description 1
- UIDUJXXQMGYOIN-UHFFFAOYSA-N aromadendrin Natural products CC1(C)C2C1CCC(C)C1C2C(C)CC1 UIDUJXXQMGYOIN-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 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
- 239000011324 bead Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 108010051210 beta-Fructofuranosidase Proteins 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000001914 calming effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- JDPQWHLMBJZURR-UHFFFAOYSA-N decan-5-one Chemical compound CCCCCC(=O)CCCC JDPQWHLMBJZURR-UHFFFAOYSA-N 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005059 dormancy Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 206010016766 flatulence Diseases 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
- 239000001573 invertase Substances 0.000 description 1
- 235000011073 invertase Nutrition 0.000 description 1
- 229910000462 iron(III) oxide hydroxide Inorganic materials 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- ZAJNGDIORYACQU-UHFFFAOYSA-N methyl n-octyl ketone Natural products CCCCCCCCC(C)=O ZAJNGDIORYACQU-UHFFFAOYSA-N 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- RUVINXPYWBROJD-UHFFFAOYSA-N para-methoxyphenyl Natural products COC1=CC=C(C=CC)C=C1 RUVINXPYWBROJD-UHFFFAOYSA-N 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229960003424 phenylacetic acid Drugs 0.000 description 1
- 239000003279 phenylacetic acid Substances 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 229930004725 sesquiterpene Natural products 0.000 description 1
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 210000002460 smooth muscle Anatomy 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003204 tranquilizing agent Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/305—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances of undetermined constitution characterised by their preparation
- A24B15/307—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances of undetermined constitution characterised by their preparation using microorganisms or enzymes as catalysts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Microbiology (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- General Chemical & Material Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Botany (AREA)
- Biochemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
It is strong that the present invention provides a kind of inoxidizability, the preparation method of high fragrance Rome yellow chamomile fermentation absolute oil, steam distillation is extracted to the Rome yellow chamomile slag after volatile oil to air-dry, low-temperature submicron powder is broken, add a certain amount of acid, oxidant and complex enzyme are well mixed in aqueous, fermentation is incubated under the synergy of three, with reference to super-pressure Accelerated solvent extraction technology, improve the recovery rate and flavouring essence quality of Rome chamomile absolute, except there is the characteristic flavor compounds of chrysanthemum, the more rich nature of fragrance, it is fragrant with chrysanthemum, the compound natural style such as happy fragrance, inoxidizability is strong, excitant is low, flavouring essence quality improves；Applied in cigarette composition pipe tobacco, reconstituted tobacco, stem, cigarette perfume is clear, there is chrysanthemum feature note, fragrance to enrich pure, pleasant impression totally carries sweetness sense, overcomes excessively strong chrysanthemum characteristic perfume, increase stimulation, slightly has the defects of miscellaneous gas, pleasant impression slightly bitter.
Description
Technical field
The present invention relates to cigarette additive technical field, and in particular to a kind of inoxidizability is strong, high fragrance Rome yellow chamomile
The preparation method and applications of fermentation absolute oil.
Background technology
With the raising of people's health consciousness, tobacco factory reduces tar content in cigarette in solution and and can keeps or met cigarette
The difficulty faced in terms of sucking availability becomes increasingly conspicuous.Cigarette has fragrance faint, deficient rich with the gradual reduction of tar
The defects of full, flue gas drying, sweet degree are not enough, comfort level is poor, in order to promote and improve the flue gas concentration of cigarette and fragrance, it is
Promote and improve the flue gas concentration and fragrance of cigarette, flavoring and casing technology is an effective way.The system of tobacco aromaticss at present
Making method mainly has two, and natural perfume material or fragrant using traditional chemical industry method synthesis is extracted from tobacco or other plants
Material.The defects of recovery rate is low, production cost is high, purity is relatively low, impurity is more still be present in plant extract natural perfume material.
Rome yellow chamomile (Euryopspectinatus), also known as golden chrysanthemum, category herbaceous plant, perennial herb flowers, one
Year is raw or herbaceos perennial, pinnate leaf have checking, flower yellow, yellow fickle in love, golden chrysanthemum summer-flowering；Complete stool has fragrance,
The fragrance of leaf slightly hay-scented and apple.Rome yellow chamomile has wind and heat dispersing, and flat liver improving eyesight, avoiding heat, it is tired to disappear, and clearing away heart-fire detoxification eliminates head
Bitterly, antiemetic, promotion scabs, profit digests, soft skin and can alleviate courbature and physical pain caused by flu, tool is releived effect；
Make us loosening, set the mind at rest, also be adapted for for improving insomnia.It is natural tranquillizer, relaxation, calming nerves effect are particularly good；It is right
Smooth muscle has calm effect, can loosen overwrought muscle, reaches sufficient rest, has and sets the mind at rest, prevents to lose
The excellent effect of dormancy.Li Shui, control tympanites.
A kind of patent " preparation method of cigarette chamomile extract " (application number：201610896432.4), take yellow chamomile
Flower water extraction obtains chamomile extract A, is fermented by fixing lactic acid bacteria bead, alcohol precipitation, is concentrated to give chamomile extract, assigns volume
Cigarette characteristic acid fragrant breeze lattice；Patent " preparation method of cigarette yellow chamomile medicinal extract " (grant number ZL201410729542.2) will flower, stem
Portion and leaf mixing carry out SCF-CO 2, add propane diols, are isolated and purified, be eventually adding again using molecular distillation technique
Honey, being applied in cigarette plays the role of to increase the sweet sense of flue gas and improvement pleasant impression；A kind of patent " the system of cigarette yellow chamomile spices
Preparation Method and application " (application number：201410699209.1) yellow chrysanthemum dried flower is soaked and distilled with water and extracted, collect volatile oil A；
It will be extracted and filtered with ethanol after distillating liquid and residue filter, obtained filter residue and filtrate, obtain B after filtrate concentration, filter residue is done
Yellow chamomile Thick many candies powder is obtained after dry, purifying, hydrolysis, Maillard reaction obtain yellow chamomile spices C.
Steam distillation is extracted to the Rome yellow chamomile slag after volatile oil to air-dry, low-temperature submicron powder is broken, adds certain
Acid, oxidant and the complex enzyme of amount are well mixed in aqueous, fermentation are incubated under the synergy of three, with reference to super-pressure
Accelerated solvent extraction technology, improve Rome chamomile absolute recovery rate and flavouring essence quality, except have the characteristic perfume of chrysanthemum into
Point, fragrance is more rich naturally, with compound natural styles such as fragrant, the happy fragrance of chrysanthemum, and inoxidizability is strong, and excitant is low, fragrance
Quality improves, and there is not been reported.
The content of the invention
It is an object of the invention to provide a kind of inoxidizability is strong, the preparation method of high fragrance Rome yellow chamomile fermentation absolute oil,
Steam distillation is extracted to the Rome yellow chamomile slag after volatile oil to air-dry, low-temperature submicron powder is broken, adds a certain amount of acid, oxygen
Agent and complex enzyme are well mixed in aqueous, fermentation are incubated under the synergy of three, with reference to super-pressure fast solvent
Extractive technique, the recovery rate and flavouring essence quality of Rome chamomile absolute are improved, except having the characteristic flavor compounds of chrysanthemum, fragrance
It is more rich naturally, with compound natural styles such as fragrant, the happy fragrance of chrysanthemum, inoxidizability is strong, and excitant is low, and flavouring essence quality carries
It is high；Applied in cigarette composition pipe tobacco, reconstituted tobacco, stem, cigarette perfume is clear, have chrysanthemum feature note, fragrance enrich it is pure,
Pleasant impression overcomes that chrysanthemum characteristic perfume is excessively strong, increase stimulates, slightly miscellaneous gas, pleasant impression slightly bitter lacks totally with happy sense
Fall into.
The present invention is achieved through the following technical solutions：
A kind of inoxidizability is strong, the preparation method of high fragrance Rome yellow chamomile fermentation absolute oil, comprises the following steps：
(1) low-temperature submicron powder is broken：Steam distillation is extracted to the Rome yellow chamomile slag after volatile oil to air-dry, is put into liquid nitrogen
Ultra-micro powder is ground into freezing micronizer；
(2) synergetic hydrolysis ferments：By Rome yellow chamomile ultra-micro powder and water in mass ratio 1:5~30 mixing, add acetic acid,
PH 4.0~6.0 is adjusted, oxidant is added, adds a certain amount of complex enzyme and be well mixed, is added in fermentation tank, starts stirring
Motor, is heated to 35~55 DEG C, incubates 2~12h of fermentation, filtrate in fermentation tank is released and continued to employ, filter residue pour out it is stand-by, it is described
Complex enzyme is the mixing of acid protease, levansucrase, acidic cellulase, pectase, beta-glucosidase；
(3) super-pressure Accelerated solvent extraction：Filter residue is poured into ultra high pressure extraction tank, adds 6~20 times of 10~50% second
Alcoholic solution, 50M~99MPa is pressurized to, 2~6min of pressurize, release immediately, filtering, filtrate and the zymotic fluid of above-mentioned steps (2) close
And 4 DEG C of low-temperature centrifugations take supernatant, are concentrated under reduced pressure, obtain as Rome yellow chamomile fermentation absolute oil, relative density 1.1~1.3.
Further, the ethanol is the ethanol of food-grade 95%, and the acetic acid is pure to analyze.
Further, the temperature of step (1) the liquid nitrogen frozen ultramicro grinding is -2~4 DEG C, and the mesh number of ultra-micro powder is
250~300 mesh.
Further, the oxidant is H2O2With the mixing of Na2Fe04, Rome yellow chamomile ultra-micro powder quality is accounted for
0.01~0.05%, H2O2Mass ratio with Na2Fe04 is 1:0.5~2.
Further, described complex enzyme is food-grade, and the enzyme activity of acid β-glucosidase is 100~10000u/
G, levansucrase, acidic cellulase, pectase, the enzyme activity of beta-glucosidase are 10,000-20 ten thousand u/g, acidic protein
Enzyme, levansucrase, acidic cellulase, pectase, the proportioning of beta-glucosidase are 1 in mass ratio:0.5~2:0.5~
2：0.5~2：1~2.
Further, described complex enzyme accounts for Rome yellow chamomile ultra-micro powder mass ratio as 0.01~0.2%.
The Rome yellow chamomile fermentation absolute oil that the present invention also provides strong, the high fragrance of inoxidizability prepared by a kind of above method exists
Perfumed applications in cigarette composition pipe tobacco, reconstituted tobacco, stem, addition be pipe tobacco, reconstituted tobacco, stem quality 0.1~
1ppm。
The beneficial effects of the invention are as follows：
(1) the broken Rome yellow chamomile of low-temperature submicron powder is in order that Rome yellow chamomile slag raw material exists to 250~300 mesh
Breaking-wall cell under lower temperature, while aroma component extraction efficiency improves, its natural fragrance component is protected not by high temperature；
(2) acetic acid is added, regulation pH value to 4.0-6.0, is because of polysaccharide key easy fracture in acid condition, makes polysaccharide big
Molecule sour water solution, while add oxidant H2O2And Na2Fe04, it is because the active group of oxidant can make polysaccharide C-O-C keys
It is broken, acid and oxidant combined effect can improve the polysaccharide hydrolysis efficiency in the yellow chamomile of Rome, make more more sugars
Solve as the compound compared with small molecule, beneficial to the enzyme hydrolysis in later stage；
(3) complex enzyme (acid protease, levansucrase, acidic cellulase, pectase, beta-glucosidase are used
Enzyme) hydrolysed ferment Rome yellow chamomile residues ultramicro powder end, further make Rome yellow chamomile slag breaking-wall cell degree increase, will be thin
Cell wall substance such as cellulose, protein, pectin etc., and polysaccharide macro-molecular material are the small-molecule substances such as glucose, amino acid,
Aroma component recovery rate is improved, while flavor precursors are hydrolyzed to aroma substance；And acid and oxidant can cooperate with promotion more
The hydrolysis of the macromoleculars such as sugar, make fermented by biological enzyme hydrolysis degree bigger, therefore in the broken breaking-wall cell of low-temperature submicron powder, acid, oxidation
Under agent, the potent effect of the collaboration of complex enzyme for hydrolyzing, Rome yellow chamomile aroma component is set to keep more natural, in ultra micro amidin
The flavor matter species and content of incubation increase, and the Rome yellow chamomile slag after extraction volatile oil is passed through these compound pre- places
After reason, then purify through solvent extraction, go the removal of impurity, soft chrysanthemum feature note and other enrich happy fragrance, have compound
Naturally abundant fragrance.
(4) super-pressure Accelerated solvent extraction technology is combined, Extracting temperature is low, the time is short, anti-oxidant active ingredient activity is high,
Aroma component retains naturally, product purity is high, environment friendly and pollution-free.
The inventive method improves the recovery rate and flavouring essence quality of Rome chamomile absolute, except there is the characteristic perfume of chrysanthemum
Composition, fragrance is more rich, and naturally, with compound natural styles such as fragrant, the happy fragrance of chrysanthemum, inoxidizability is strong, and excitant is low, fragrant
Gas quality improves；Applied in cigarette composition pipe tobacco, reconstituted tobacco, stem, cigarette perfume is clear, has chrysanthemum feature note, fragrance
Enrich pure, pleasant impression and totally carry sweetness sense, overcome excessively strong chrysanthemum characteristic perfume, increase stimulation, slightly have miscellaneous gas, pleasant impression
The defects of slightly bitter.The raw materials used wide material sources of this method are cheap, green, and process conditions are gentle, have industrialization prospect.
Brief description of the drawings
Fig. 1 is the DPPH. clearance rates of Rome yellow chamomile fermentation absolute oil prepared by the present invention；
Fig. 2 is the total ion chromatogram of Rome yellow chamomile reference extract volatile ingredient；
Fig. 3 is the total ion chromatogram of Rome yellow chamomile fermentation absolute oil volatile ingredient of the present invention.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
A kind of inoxidizability is strong, the preparation of high fragrance Rome yellow chamomile fermentation absolute oil：
(1) low-temperature submicron powder is broken：Steam distillation is extracted to the Rome yellow chamomile after volatile oil and air-dries flower slag, is put into liquid nitrogen
Ultra-micro powder is ground into freezing micronizer, the temperature of the liquid nitrogen frozen ultramicro grinding is -2 DEG C, the mesh of ultra-micro powder
Number is 250 mesh；
(2) synergetic hydrolysis ferments：By Rome yellow chamomile ultra-micro powder and water in mass ratio 1:8 mixing, acetic acid is added, it is described
Acetic acid is pure to analyze, and adjusts pH 4.0, adds oxidant H2O2, Na2Fe04 (analyze pure, mass ratio 1:0.5) the Rome spring, is accounted for
The 0.01% of yellow chrysanthemum flower residues ultramicro powder end quality, adds a certain amount of complex enzyme (acid protease, levansucrase, fibre
Tie up plain enzyme, pectase, beta-glucosidase) it is well mixed, add in fermentation tank, start stirring motor, be heated to 35 DEG C, incubate
Ferment 10h, and complex enzyme is food-grade, and enzyme activity is respectively 10,000,50,000,100,000,50,000,1000 u/g, the proportioning between various enzymes
It is 1 in mass ratio:0.5:0.5：0.5：1, described complex enzyme accounts for Rome yellow chamomile ultra-micro powder mass ratio as 0.2%；
(3) super-pressure Accelerated solvent extraction：Filter residue is poured into ultra high pressure extraction tank, 6 times of 50% ethanol solution is added, adds
Be pressed onto 90MPa, pressurize 2min, release immediately, filtering, filtrate and above-mentioned steps 2) zymotic fluid merge, refrigerated centrifuge takes supernatant
Liquid, it is concentrated under reduced pressure, obtains as Rome yellow chamomile fermentation absolute oil, relative density 1.10；Wherein ethanol is the ethanol of food-grade 95%,.
The Rome yellow chamomile fermentation absolute oil that the present invention also provides strong, the high fragrance of inoxidizability prepared by a kind of above method exists
The application of perfuming in cigarette composition pipe tobacco, addition account for the 0.1ppm for the quality that cuts filler.
Embodiment 2
A kind of preparation for the Roman chamomille oil for improving flavouring essence quality：
(1) low-temperature submicron powder is broken：Rome yellow chamomile is air-dried into flower slag and is put into crushing (0 in liquid nitrogen frozen micronizer
DEG C), the mesh of particle diameter 280；
(2) synergetic hydrolysis ferments：Rome yellow chamomile ultra-micro powder and water are first pressed 1:12 mixing, acetic acid is added (for analysis
It is pure), regulation pH value to 5.0, add the oxidant H for accounting for Rome yellow chamomile residues ultramicro powder end quality 0.015%2O2And ferric acid
Sodium (analyzes pure, mass ratio 1:0.8), add account for chrysanthemum residues ultramicro powder end quality 0.15% complex enzyme (acid protease,
Levansucrase, cellulase, pectase, beta-glucosidase, mass ratio 1：1：0.8：1：1) it is well mixed, adds hair
In fermentation tank, start stirring motor, be heated to 38 DEG C, incubate fermentation 8h, complex enzyme is food-grade, enzyme activity is respectively 20,000,80,000,
150000,150,000,2000u/g；
(3) super-pressure Accelerated solvent extraction：Filter residue is poured into ultra high pressure extraction tank, adds 8 times of 40% ethanol solution (second
Alcohol is the ethanol of food-grade 95%), be pressurized to 80MPa, pressurize 3min, release immediately, filtering, filtrate and above-mentioned steps 2) hair
Zymotic fluid merges, and refrigerated centrifuge takes supernatant, is concentrated under reduced pressure, and obtains as Rome yellow chamomile fermentation absolute oil, relative density 1.11.
The Rome yellow chamomile fermentation absolute oil that the present invention also provides strong, the high fragrance of inoxidizability prepared by a kind of above method exists
The application of perfuming in reconstituted tobacco, addition account for the 0.3ppm of reconstituted tobacco quality.
Embodiment 3
A kind of preparation of the Rome yellow chamomile fermentation absolute oil of strong, the high fragrance of inoxidizability：
(1) low-temperature submicron powder is broken：Rome yellow chamomile is air-dried into flower slag and is put into crushing (2 in liquid nitrogen frozen micronizer
DEG C), the mesh of particle diameter 300；
(2) synergetic hydrolysis ferments：Rome yellow chamomile ultra-micro powder and water are first pressed 1:15 mixing, acetic acid is added (for analysis
It is pure), regulation pH value to 5.5, add the oxidant H for accounting for Rome yellow chamomile residues ultramicro powder end quality 0.02%2O2And Na2Fe04
(analyze pure, mass ratio 1:1.2) complex enzyme (acid protease, the fruit for accounting for chrysanthemum residues ultramicro powder end quality 0.18%, are added
Glycan invertase, cellulase, pectase, beta-glucosidase, mass ratio 1：1.2：1.2：1.5：1, it is food-grade, enzyme
Living is respectively 100,000,100,000,200,000,100,000,10,000 u/g) it is well mixed, add in fermentation tank, start stirring motor, be heated to
38 DEG C, incubate fermentation 8h；
(3) super-pressure Accelerated solvent extraction：Filter residue is poured into ultra high pressure extraction tank, adds 12 times of 10% ethanol solution
(ethanol is the ethanol of food-grade 95%), it is pressurized to 50MPa, pressurize 5min, immediately release, filtering, filtrate and above-mentioned steps 2)
Zymotic fluid merges, and refrigerated centrifuge takes supernatant, is concentrated under reduced pressure, and obtains as Rome yellow chamomile fermentation absolute oil, relative density 1.15.
The Rome yellow chamomile fermentation absolute oil that the present invention also provides strong, the high fragrance of inoxidizability prepared by a kind of above method exists
The application of perfuming in stem, addition account for the 0.2ppm of stem quality.
Test example 1：The sensory effects evaluation of application
Rome yellow chamomile fermentation absolute oil prepared by embodiment 1-3 is being cut filler, felt in reconstituted tobacco and stem
Official's quality evaluation, sample be applied with yellow chamomile of the present invention fermentation absolute oil it is corresponding cut filler, reconstituted tobacco and stem, control
Group for apply yellow chamomile slag ethanol extract it is corresponding cut filler, reconstituted tobacco and stem, blank group are matching somebody with somebody for non-perfuming
Square pipe tobacco, reconstituted tobacco and stem.
As a result show：The inventive method improves the recovery rate and flavouring essence quality of Rome chamomile absolute, except there is chrysanthemum
Characteristic flavor compounds, fragrance is more rich, and naturally, with compound natural styles such as fragrant, the happy fragrance of chrysanthemum, inoxidizability is strong, thorn
It is low to swash property, flavouring essence quality improves；Applied in cigarette composition pipe tobacco, reconstituted tobacco, stem, cigarette perfume is clear, has chrysanthemum feature
Note, fragrance enrich pure, pleasant impression and totally carry sweetness sense, overcome excessively strong chrysanthemum characteristic perfume, increase stimulation, slightly have
The defects of miscellaneous gas, pleasant impression slightly bitter.
Sensory evaluation of the Rome yellow chamomile fermentation absolute oil of strong, the high fragrance of the inoxidizability of table 1. in cutting filler
Sensory evaluation of the Rome yellow chamomile fermentation absolute oil of strong, the high fragrance of the inoxidizability of table 2. in reconstituted tobacco
Sensory evaluation of the Rome yellow chamomile fermentation absolute oil of strong, the high fragrance of the inoxidizability of table 3. in stem
Test example 2：The inoxidizability of Rome yellow chamomile fermentation absolute oil of the present invention
The content of the Flavonoid substances of Rome yellow chamomile fermentation absolute oil prepared by 2.1 present invention
Measure after the light absorption value of Rome chamomile absolute by regression equation calculation institute value, be its institute through concentration conversion
Content containing Flavonoid substances.Standard curve is done with rutin standard items.Rome chamomile absolute 1g is taken, adds 30% ethanol constant volume to arrive
500mL, then 0.2mL constant volumes are therefrom taken to the ethanol systems of 25mL 30%, it is through ultraviolet spectrometry range meter detection light absorption value
0.1425, its Flavonoid substances concentration is 0.6256mg/mL, quality 866.5mg, content 86.65%；Equally calculate it
It is 0.1239 to compare extract solution light absorption value, and Flavonoid substances concentration is 0.4121, quality 503mg, content 50.30%；This
Its purifying control sample that do not ferment of the Flavonoid substances content balance of Rome yellow chamomile fermentation absolute oil prepared by invention, is improved
72.27%.
2.2 remove the experiment of DPPH. free radicals
DPPH. it is a kind of free radical of stabilization in organic solvent, its ethanol solution (aobvious darkviolet) has at 516nm
Maximum absorption band.When being acted on anti-oxidizing activities material, its lone pair electrons is paired, thus is absorbed and disappeared or weaken, and is led to
Cross measure and absorb the degree weakened, the activity of free radical scavenger can be evaluated.
Accurately weighing 2.5mg DPPH. is dissolved in 100mL methanol, is formulated as concentration .025mg/mLDPPH. purple solutions.Point
Not Pei Zhi Rome yellow chamomile extract solution be 0.04,0.2,0.35,0.50,0.70,0.85,1.00mg/mL concentration, be loaded 0.1mL
Sample liquid and 3.9mL DPPH. solution detect light absorption value at 516nm in cuvette after mixing 5 minutes.
It is A0 that 0.1mL distilled water and 3.9mL DPPH. solution, which mix and light absorption value surveyed at 516nm in 5 minutes,.
It is A1 that 0.1mL samples and 3.9mL DPPH. solution, which mix and light absorption value surveyed at 516nm in 5 minutes,.
Using 0.1mL samples and 3.9mL methanol solutions mix 5 minutes at 516nm survey light absorption value as blank.
Clearance rate (%)=(1-A1/A0) × 100%
Take 2 Duplicate Samples every time, replication is averaged for 2 times.
Light absorption value of the various concentrations Rome chamomile absolute dilution of table 4 in DPPH. systems
The Rome chamomile absolute dilution of the present invention has stronger inoxidizability, right in 0.70mg/mL concentration
DPPH. 51.52% is reached during the clearance rate of free radical, and the concentration added is proportionate within the specific limits with clearance rate,
There is 7.77% scavenging action during 0.04mg/mL concentration, 82.40% is up in 1.00 mg/mL, have stronger anti-oxidant
Ability (as shown in Figure 1).
Test example 3：SPME gaseous mass spectrum (the HS- of the Rome yellow chamomile fermentation absolute oil volatile ingredient of the present invention
SPME-GC/MS) analyze
The Rome yellow chamomile fermentation absolute oil strong to inoxidizability of the present invention compares with it carries out volatility aroma component progress
SPME-gaseous mass spectrum (HS-SPME-GC/MS) comparative analysis.
(1) Rome yellow chamomile fermentation absolute oil or its control sample 1g are weighed, is placed in the special headspace extraction sample bottles of 15mL,
250 DEG C of aging PDMS extracting heads, 30min, insert in headspace extraction sample bottle, balance is incubated 10 minutes at 60 DEG C, then at 60 DEG C
Lower extraction 40min；
(2) chromatographic condition：50 DEG C of post initial temperature, 2min is kept, is warming up to 180 DEG C with 8 DEG C/min speed, keeps 1min,
280 DEG C are warming up to 18 DEG C/min speed again, keeps 30min；Carrier gas is helium (He, purity 99.99%), constant current mode,
Flow velocity is 1.0mL/min；Split sampling mode, split ratio 1：10, solvent-free delay；250 DEG C of injector temperature.
(3) Mass Spectrometry Conditions：Ionization mode：EI sources；Electron energy:70eV；Multiplier voltage：1.2kV；Ion source temperature：
230℃；Level Four bar temperature:150℃；Interface temperature：280 DEG C, 280 DEG C of transmission line；Scanning range：33-350m/z.Use
NIST standard spectrums storehouse carries out retrieval analysis, and compound percentage contents are calculated by areas of peak normalization method.Rome yellow chamomile pair
According to the total ion chromatogram of extract volatile ingredient and Rome yellow chamomile of the present invention fermentation absolute oil volatile ingredient respectively such as
Shown in Fig. 2 and Fig. 3.
(4) volatile ingredient comparative analysis
GC/MS analysis results (table 5) show：
The Rome yellow chamomile fermentation absolute oil volatile ingredient GC/MS analyses of strong, the high fragrance of the inoxidizability of table 5
As shown in Table 5, Rome chamomile extract control identifies 78 kinds of volatile ingredients, wherein 24 kinds of ketone, relatively
Percentage composition accounts for 42.74%, 13 kinds of alcohols, and percentage contents account for 13.76%, esters 5 kinds (4.35%), 5 kinds of alkane
(3.58%), aromatic hydrocarbon 5 kinds (3.78%), alkenes 5 kinds (3.01%), aldehydes 4 kinds (4.9%), 15 kinds of other heterocyclic compounds
(12.83%)；And Rome chamomile absolute prepared by the present invention identifies 86 kinds of volatile ingredients, wherein 22 kinds of ketone, relatively
Percentage composition accounts for 22.27%, 20 kinds of alcohols, percentage contents 22.69%, alkenes 9 kinds (5.02%), 7 kinds of esters
(6.12%), hydro carbons 6 kinds (4.77%), aldehydes 3 kinds (7.24%), acids 3 kinds (3.7%), phenols 3 kinds (3.31%).
For the volatile ingredient of Rome chamomile absolute prepared by the present invention compared with its extract compares, there occurs larger
Change：
(1) emerging volatile ingredient has 49 kinds；
(2) volatile ingredient identical has 35 kinds, and wherein percentage contents are increased 20 kinds, and constant has 4 kinds, phase
There are 11 kinds to what percentage composition reduced；
(3) volatile ingredient to disappear has 39 kinds.
Many macromolecular substances disappear in the yellow chamomile control of Rome or percentage contents reduce, single percentage contents
Highest material is 1,8- dimethyl -8,9- epoxy -4- isopropyls-spiral shell [4.5] decanone, 24.52%, it is pure through present invention fermentation
Change, drop to 3.51%, it may be possible to it is decomposed, converts, has been oxidized to other small molecule flavor matters or fragrance precursor material, its
Secondary is cis- chrysanthenol, is reduced to 4.74% from 5.47%, fragrant citrus olefinic oxide (2) 4.72%, long leaf aldehyde increases to from 4.50%
6.63%.In the volatile ingredient of Rome yellow chamomile fermentation absolute oil, single percentage composition highest material is different aromadendrene epoxy
Compound 7.51%, it is emerging fragrance component, next to that long leaf aldehyde 6.63%, 47.33%, 2,3,4 are increased compared to control,
5,6- mellityl alcohols 5.07%, followed by cis- chrysanthenol 4.74%, acetic acid Valeriana Fauriei Briq alcohol ester 3.93% etc..These are waved
Hair property composition has the compound fragrance of nature, and wherein phenylacetic acid is with a kind of smell of picture honey；Anethole band is pleasantly sweet, has fennel
Special aroma；Megastigmatrienone has cocoa aroma, can increase the comfortable mouthfeel of flue gas, improves side-stream smoke fragrance；Extensively suddenly
Aromatic tricyclic sesquiterpene class compound；Excitant macromolecular substances content reduces, and small molecule volatile substance classes increase, and make sieve
Horse yellow chamomile ferments absolute oil except with chrysanthemum characteristic perfume, also more having the compound breath of nature, fragrance is more rich, adds in cigarette
Perfume (or spice), fragrance is fresh and clean, harmony is more preferable, and excitant is reduced, miscellaneous gas is reduced, and has happy breath and with chrysanthemum feature perfume
Gas.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Belong to those skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (7)
1. a kind of inoxidizability is strong, the preparation method of high fragrance Rome yellow chamomile fermentation absolute oil, it is characterised in that including following step
Suddenly：
(1) low-temperature submicron powder is broken：Steam distillation is extracted to the Rome yellow chamomile slag after volatile oil to air-dry, is put into liquid nitrogen frozen
Ultra-micro powder is ground into micronizer；
(2) synergetic hydrolysis ferments：By Rome yellow chamomile ultra-micro powder and water in mass ratio 1:5~30 mixing, add acetic acid, regulation
PH 4.0~6.0, oxidant is added, a certain amount of complex enzyme is added and is well mixed, added in fermentation tank, start stirring electricity
Machine, is heated to 35~55 DEG C, incubates 2~12h of fermentation, filtrate in fermentation tank is released and continued to employ, and filter residue is poured out stand-by, and described answers
Synthase is the mixing of acid protease, levansucrase, acidic cellulase, pectase, beta-glucosidase；
(3) super-pressure Accelerated solvent extraction：Filter residue is poured into ultra high pressure extraction tank, it is molten to add 6~20 times of 10~50% ethanol
Liquid, 50M~99MPa being pressurized to, 2~6min of pressurize, release immediately, is filtered, filtrate merges with the zymotic fluid of above-mentioned steps (2), and 4
DEG C low-temperature centrifugation takes supernatant, is concentrated under reduced pressure, and obtains fermenting absolute oil for Rome yellow chamomile, relative density 1.1~1.3.
2. the method as described in claim 1, it is characterised in that：The ethanol is the ethanol of food-grade 95%, and the acetic acid is point
Analyse pure.
3. the method as described in claim 1, it is characterised in that：In the step (1) temperature of liquid nitrogen frozen ultramicro grinding for-
2~4 DEG C, the mesh number of ultra-micro powder is 250~300 mesh.
4. the method as described in claim 1, it is characterised in that：The oxidant is H2O2With the mixing of Na2Fe04, Rome is accounted for
0.01~0.05%, H of yellow chamomile ultra-micro powder quality2O2Mass ratio with Na2Fe04 is 1:0.5~2.
5. the method as described in claim 1, it is characterised in that：Described complex enzyme is food-grade, acid beta-glucosidase
The enzyme activity of enzyme is 100~10000u/g, and levansucrase, acidic cellulase, pectase, the enzyme activity of beta-glucosidase are equal
For 10,000-20 ten thousand u/g, acid protease, levansucrase, acidic cellulase, pectase, the proportioning of beta-glucosidase are pressed
Mass ratio is 1:0.5~2:0.5~2：0.5~2：1~2.
6. the method as described in claim 1, it is characterised in that：Described complex enzyme accounts for Rome yellow chamomile ultra-micro powder mass ratio
For 0.01~0.2%.
A kind of 7. Rome yellow chamomile hair of strong, the high fragrance of inoxidizability prepared by method as any one of claim 1-6
Perfumed applications of the ferment absolute oil in cigarette composition pipe tobacco, reconstituted tobacco, stem, addition are pipe tobacco, reconstituted tobacco, stem quality
0.1~1ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710889766.3A CN107653064A (en) | 2017-09-27 | 2017-09-27 | A kind of inoxidizability is strong, the preparation method and applications of high fragrance Rome yellow chamomile fermentation absolute oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710889766.3A CN107653064A (en) | 2017-09-27 | 2017-09-27 | A kind of inoxidizability is strong, the preparation method and applications of high fragrance Rome yellow chamomile fermentation absolute oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107653064A true CN107653064A (en) | 2018-02-02 |
Family
ID=61116137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710889766.3A Pending CN107653064A (en) | 2017-09-27 | 2017-09-27 | A kind of inoxidizability is strong, the preparation method and applications of high fragrance Rome yellow chamomile fermentation absolute oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107653064A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109730350A (en) * | 2019-03-05 | 2019-05-10 | 湖北中烟工业有限责任公司 | Use Fe-CA/H2O2The method that imitative enzyme system promotes papermaking-method reconstituted tobaccos quality |
| CN110373269A (en) * | 2019-07-05 | 2019-10-25 | 福建省农业科学院作物研究所 | A method of cape jasmine flower essential oil is prepared with waste liquid |
| CN111035054A (en) * | 2019-11-27 | 2020-04-21 | 内蒙古昆明卷烟有限责任公司 | Method for preparing tar extract with aroma characteristics from waste cigarette butts and application of tar extract in cigarettes |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86102952A (en) * | 1985-04-26 | 1987-11-04 | 纳比斯科商标公司 | Remove the method for assorted peculiar smell hot puckery in the volatile oil |
| US20130239981A1 (en) * | 2010-11-29 | 2013-09-19 | Shanghai Tobacco Group Co., Ltd. | Method for supercritical extraction of characteristic fragrant substances in different fragrant tobacco leaves |
| CN106418663A (en) * | 2016-10-31 | 2017-02-22 | 湖北中烟工业有限责任公司 | Biochemical joint preparation method and application of absolute rose oil |
| CN106497906A (en) * | 2016-10-13 | 2017-03-15 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette chamomile extract |
-
2017
- 2017-09-27 CN CN201710889766.3A patent/CN107653064A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86102952A (en) * | 1985-04-26 | 1987-11-04 | 纳比斯科商标公司 | Remove the method for assorted peculiar smell hot puckery in the volatile oil |
| US20130239981A1 (en) * | 2010-11-29 | 2013-09-19 | Shanghai Tobacco Group Co., Ltd. | Method for supercritical extraction of characteristic fragrant substances in different fragrant tobacco leaves |
| CN106497906A (en) * | 2016-10-13 | 2017-03-15 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette chamomile extract |
| CN106418663A (en) * | 2016-10-31 | 2017-02-22 | 湖北中烟工业有限责任公司 | Biochemical joint preparation method and application of absolute rose oil |
Non-Patent Citations (1)
| Title |
|---|
| 吴梧桐主编: "《生物化学》", 31 August 2015, 中国医药科技出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109730350A (en) * | 2019-03-05 | 2019-05-10 | 湖北中烟工业有限责任公司 | Use Fe-CA/H2O2The method that imitative enzyme system promotes papermaking-method reconstituted tobaccos quality |
| CN110373269A (en) * | 2019-07-05 | 2019-10-25 | 福建省农业科学院作物研究所 | A method of cape jasmine flower essential oil is prepared with waste liquid |
| CN111035054A (en) * | 2019-11-27 | 2020-04-21 | 内蒙古昆明卷烟有限责任公司 | Method for preparing tar extract with aroma characteristics from waste cigarette butts and application of tar extract in cigarettes |
| CN111035054B (en) * | 2019-11-27 | 2022-07-05 | 内蒙古昆明卷烟有限责任公司 | Method for preparing tar extract with aroma characteristics from waste cigarette butts and application of tar extract in cigarettes |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105754722B (en) | A kind of preparation method and applications of the cigarette perfume object for reconstituted tobacoo | |
| CN106418663B (en) | A kind of biochemistry combined preparation process of rose extrait and its application | |
| CN110786534B (en) | Method for improving aroma of tobacco extract by using carotenoid-producing microorganism | |
| CN101570717A (en) | Method for preparing tobacco extract and application thereof | |
| CN107723092A (en) | A kind of preparation method and applications with fragrant and sweet fermentation angelica extract | |
| CN107653064A (en) | A kind of inoxidizability is strong, the preparation method and applications of high fragrance Rome yellow chamomile fermentation absolute oil | |
| CN107118848A (en) | A kind of fine processing method of coconut oil and its application | |
| CN107232638A (en) | A kind of upgrading purification process of raisin extract and its application | |
| Gnekow et al. | Methanol in wines and musts: source and amounts | |
| CN102732381B (en) | Preparation method of fermented tobacco Dendranthema indicum essential oil | |
| CN109762664A (en) | A kind of quick-fried pearl tea essence of persistent form cigarette and preparation method thereof | |
| CN107287031B (en) | Method for preparing tobacco additive by separating aroma-developing components of Maillard reactant of aromatic tobacco and application | |
| CN108851173A (en) | A kind of cigarette preparation method of mango fragrance and the application in cigarette | |
| CN103070475A (en) | Cigar tobacco leaf additive and production method thereof | |
| CN106978258A (en) | Enzymatic flavouring improves the preparation method and application of the FLOS CHRYSANTHEMI ALBA from Haizhou of China volatile oil of flavouring essence quality | |
| CN107699352A (en) | A kind of method and its application for improving Roman chamomille oil flavouring essence quality | |
| CN102344853A (en) | Preparation method of meratia praecox extract for improving aroma and application thereof | |
| CN108165371A (en) | A kind of preparation method and applications of iris extract | |
| CN107997228A (en) | A kind of preparation method and applications of the fragrant angelica extract of band baking | |
| CN103881815A (en) | Black plum extract, preparation method for same and application of extract to cigarette | |
| CN115011410B (en) | Schisandra chinensis branch spice, preparation method thereof and cigarette | |
| CN109536283B (en) | Preparation method and application of storax oil for improving quality | |
| CN115644494B (en) | Preparation method and application of mixed tobacco recombinant essence | |
| CN108264965B (en) | Preparation method of artemisia scoparia enzymolysis extract and application of artemisia scoparia enzymolysis extract in cigarettes | |
| CN108142988B (en) | Preparation method of momordica grosvenori extract for increasing aroma and keeping moisture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180202 |
|
| RJ01 | Rejection of invention patent application after publication |