CN106433987A - Preparation method of refined sweet-orange spice and application thereof - Google Patents
Preparation method of refined sweet-orange spice and application thereof Download PDFInfo
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- CN106433987A CN106433987A CN201610933810.1A CN201610933810A CN106433987A CN 106433987 A CN106433987 A CN 106433987A CN 201610933810 A CN201610933810 A CN 201610933810A CN 106433987 A CN106433987 A CN 106433987A
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- spice
- pericarpium citri
- sinensiss
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- fructus citri
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- 235000013599 spices Nutrition 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 235000005976 Citrus sinensis Nutrition 0.000 title abstract 7
- 240000002319 Citrus sinensis Species 0.000 title abstract 7
- 239000011347 resin Substances 0.000 claims abstract description 46
- 229920005989 resin Polymers 0.000 claims abstract description 46
- 239000003205 fragrance Substances 0.000 claims abstract description 23
- 241000208125 Nicotiana Species 0.000 claims abstract description 20
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 20
- 102000006995 beta-Glucosidase Human genes 0.000 claims abstract description 14
- 108010047754 beta-Glucosidase Proteins 0.000 claims abstract description 14
- 238000000746 purification Methods 0.000 claims abstract description 14
- 238000000855 fermentation Methods 0.000 claims abstract description 13
- 230000004151 fermentation Effects 0.000 claims abstract description 13
- 235000019505 tobacco product Nutrition 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 58
- 239000007788 liquid Substances 0.000 claims description 21
- 235000019504 cigarettes Nutrition 0.000 claims description 17
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 16
- 239000003546 flue gas Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 235000009508 confectionery Nutrition 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 13
- 235000013305 food Nutrition 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 239000002304 perfume Substances 0.000 claims description 9
- 230000001737 promoting effect Effects 0.000 claims description 8
- 239000003380 propellant Substances 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- 102000004190 Enzymes Human genes 0.000 claims description 5
- 108090000790 Enzymes Proteins 0.000 claims description 5
- 230000002159 abnormal effect Effects 0.000 claims description 5
- 238000003795 desorption Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 230000035943 smell Effects 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- 239000002932 luster Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000007789 gas Substances 0.000 abstract description 4
- 239000000779 smoke Substances 0.000 abstract description 3
- 238000000638 solvent extraction Methods 0.000 abstract description 3
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- 230000000638 stimulation Effects 0.000 abstract description 2
- 206010013911 Dysgeusia Diseases 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000000796 flavoring agent Substances 0.000 abstract 1
- 235000019634 flavors Nutrition 0.000 abstract 1
- 229930003944 flavone Natural products 0.000 description 5
- 235000011949 flavones Nutrition 0.000 description 5
- 229930003935 flavonoid Natural products 0.000 description 5
- 235000017173 flavonoids Nutrition 0.000 description 5
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- -1 flavonoid compound Chemical class 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
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- 230000007547 defect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 description 3
- 239000001100 (2S)-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chroman-4-one Substances 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 2
- QUQPHWDTPGMPEX-UHFFFAOYSA-N Hesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(COC4C(C(O)C(O)C(C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-UHFFFAOYSA-N 0.000 description 2
- QUQPHWDTPGMPEX-UTWYECKDSA-N aurantiamarin Natural products COc1ccc(cc1O)[C@H]1CC(=O)c2c(O)cc(O[C@@H]3O[C@H](CO[C@@H]4O[C@@H](C)[C@H](O)[C@@H](O)[C@H]4O)[C@@H](O)[C@H](O)[C@H]3O)cc2O1 QUQPHWDTPGMPEX-UTWYECKDSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- APSNPMVGBGZYAJ-GLOOOPAXSA-N clematine Natural products COc1cc(ccc1O)[C@@H]2CC(=O)c3c(O)cc(O[C@@H]4O[C@H](CO[C@H]5O[C@@H](C)[C@H](O)[C@@H](O)[C@H]5O)[C@@H](O)[C@H](O)[C@H]4O)cc3O2 APSNPMVGBGZYAJ-GLOOOPAXSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
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- 238000011156 evaluation Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- VUYDGVRIQRPHFX-UHFFFAOYSA-N hesperidin Natural products COc1cc(ccc1O)C2CC(=O)c3c(O)cc(OC4OC(COC5OC(O)C(O)C(O)C5O)C(O)C(O)C4O)cc3O2 VUYDGVRIQRPHFX-UHFFFAOYSA-N 0.000 description 2
- QUQPHWDTPGMPEX-QJBIFVCTSA-N hesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]4[C@@H]([C@H](O)[C@@H](O)[C@H](C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-QJBIFVCTSA-N 0.000 description 2
- 229940025878 hesperidin Drugs 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- ULSUXBXHSYSGDT-UHFFFAOYSA-N tangeretin Chemical compound C1=CC(OC)=CC=C1C1=CC(=O)C2=C(OC)C(OC)=C(OC)C(OC)=C2O1 ULSUXBXHSYSGDT-UHFFFAOYSA-N 0.000 description 2
- 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
- 206010013789 Dry throat Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- OBIOZWXPDBWYHB-UHFFFAOYSA-N Nobiletin Natural products C1=CC(OC)=CC=C1C1=C(OC)C(=O)C2=C(OC)C(OC)=C(OC)C(OC)=C2O1 OBIOZWXPDBWYHB-UHFFFAOYSA-N 0.000 description 1
- IECRXMSGDFIOEY-UHFFFAOYSA-N Tangeretin Natural products COC=1C(OC)=C(OC)C(OC)=C(C(C=2)=O)C=1OC=2C1=CC=C(O)C=C1 IECRXMSGDFIOEY-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
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- 230000003064 anti-oxidating effect Effects 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- QGGZBXOADPVUPN-UHFFFAOYSA-N dihydrochalcone Chemical compound C=1C=CC=CC=1C(=O)CCC1=CC=CC=C1 QGGZBXOADPVUPN-UHFFFAOYSA-N 0.000 description 1
- PXLWOFBAEVGBOA-UHFFFAOYSA-N dihydrochalcone Natural products OC1C(O)C(O)C(CO)OC1C1=C(O)C=CC(C(=O)CC(O)C=2C=CC(O)=CC=2)=C1O PXLWOFBAEVGBOA-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 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
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000019261 food antioxidant Nutrition 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 230000036449 good health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000000937 inactivator Effects 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- ARGKVCXINMKCAZ-UZRWAPQLSA-N neohesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O[C@H]3[C@@H]([C@H](O)[C@@H](O)[C@H](C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UZRWAPQLSA-N 0.000 description 1
- MRIAQLRQZPPODS-UHFFFAOYSA-N nobiletin Chemical compound C1=C(OC)C(OC)=CC=C1C1=CC(=O)C2=C(OC)C(OC)=C(OC)C(OC)=C2O1 MRIAQLRQZPPODS-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 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
- 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
- 230000035807 sensation Effects 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229940089401 xylon Drugs 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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- 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
- A24B15/20—Biochemical treatment
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- 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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
Abstract
The invention aims at providing a preparation method of refined sweet-orange spice and an application thereof. The refined sweet-orange spice is obtained by using sweet-orange peel as a raw material, and adopting a technology combining beta-glucosidase fermentation, solvent extraction and macroporous resin purification. The refined sweet-orange spice is richer in fragrance, the quality is improved and the stimulating components are reduced. After the refined sweet-orange spice is applied to reconstituted tobaccos, the coordination with smoke is achieved, the fragrance is rich, the aftertaste of sweetness is increased, the smoke is soft, and stimulation and foreign gases are reduced; and after the refined sweet-orange spice is applied to an atomizing agent for novel tobacco products, the fragrance of the novel tobacco products is enriched, the flavor of the tobacco is improved and the sweetness is increased.
Description
Technical field
The present invention relates to cigarette additive technical field, the preparation method of specifically a kind of refined Fructus Citri sinensiss spice and its should
With.
Background technology
Discarded tobacco leaf, thin slice and stem product are the important source material in cigarette product, but because these raw materials have elder generation
Nature defect, including lacking Medicated cigarette characteristic perfume or tobacco aroma is light, miscellaneous QI, xylon gas are heavier, throat's dry sensation and tongue thorn
Peppery sense is obvious, thus these raw materials intervention tobacco leaf formulation will significantly reduce Medicated cigarette grade.Improve discarded tobacco leaf, thin slice and stem cigarette
Hay-scented, solves the negative effect to sense organ, will have far-reaching influence to improving Medicated cigarette integral suction quality.Most important of which
Means are exactly that outside flavoring and casing is processed.
Fructus Citri sinensiss are that distribution in China is widest in area, cultivation amount at most, most important juice kind processed in production.Flavonoid in its peel
Compounds content is high, such as Hesperidin, neohesperidin, Tangeretin, Nobiletin etc..In Pericarpium Citri junoris, how flavone is with the larger glucosides of polarity
Form exists.Natural flavonoid compound toxic and side effects are little, and the non-oxidizability of some Flavonoid substances can be compared favourably with BHT,
It is very potential as the development of food antioxidant.Flavonoid substances Hesperidin in Pericarpium Citri junoriss, has similar medicine to rutin
Reason acts on, and is the important source material for the treatment of cardiovascular disease treating medicine, or synthesizes high sugariness, novel sweetener dihydrochalcone low in calories
The primary raw material of (suitable diabetes patient and overweight people eat).Abroad report relatively containing Flavonoid substances function in Pericarpium Citri junoris
Many, mainly include anti-inflammation, antiallergic, analgesia, prevention and cure of cardiovascular disease and antiviral, antioxidation, anticancer etc. act on, and have
Good health function.Flavone compound also has various pharmacology and health-care effect, but can not synthesize in human body, and in body
Intracellular metabolite it is therefore desirable to find the source of more flavone compounds to meet human intake's level, reaches effectively quickly
Intake.Pericarpium Citri junoriss are the extremely general low-cost resources being easy to get containing flavone compound, and wherein flavones content is higher, if to every
Pericarpium Citri junoriss resource in terms of dry ten thousand tons for the year is used, and its benefit is considerable.China is No.1 big as Orange Producing in the world
By-product Pericarpium Citri junoriss are often abandoned in Citrus procession, not only waste of resource, and cause environmental pollution, therefore it opened by state
Send out using significant.
With Pericarpium Citri junoris as raw material, take beta-glucosidase enzyme fermentation, solvent extraction to combine purification by macroporous resin technology, obtain
Refined Fructus Citri sinensiss spice, fragrance is more rich, and quality improves, and stimulating component reduces.This refined Fructus Citri sinensiss spice should in reconstituted tobacco
With coordinating with flue gas, abundant fragrance, increasing back sweet sense, soft flue gas, reduce and stimulate and reduce miscellaneous QI；In novel tobacco product
Apply in propellant, the fragrance of abundant novel tobacco product, promoting or transferring cigarette perfume, the sweet sense of increase, have not been reported.
Content of the invention
It is an object of the invention to provide a kind of preparation method and applications of refined Fructus Citri sinensiss spice, with Pericarpium Citri junoris as raw material,
Take beta-glucosidase enzyme fermentation raw fragrant, decompose, convert macromolecular substances, discharge small molecule Aroma precursor material, solvent extraction
In conjunction with purification by macroporous resin technology, remove the macromolecular substances such as the big protein of zest, cellulose, polysaccharide further, obtain
Refined Fructus Citri sinensiss spice, and apply in reconstituted tobacco, coordinate with flue gas, abundant fragrance, increase back sweet sense, soft flue gas, reduce
Stimulate and reduce miscellaneous QI；Novel tobacco product propellant is applied, the fragrance of abundant novel tobacco product, promoting or transferring cigarette perfume, increasing
Sweeten sense.
Above-mentioned purpose is achieved through the following technical solutions：
A kind of preparation method of refined Fructus Citri sinensiss spice, comprises the following steps：
1) ferment：Pericarpium Citri junoris clean after after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 60～
120 mesh, in mass ratio for 1:20～50 addition water, and press 0.05～0.3% addition beta-glucosidase of Pericarpium Citri junoris quality, stir
Mix uniformly, under 40～55 DEG C, pH natural conditions, ferment 3～12h, and 5～10min enzyme-deactivating at 100 DEG C obtains Pericarpium Citri junoris and sends out
Zymotic fluid；
Described beta-glucosidase is food stage, enzyme activity 100～10000u/g；
2) reflux, extract,：Food stage 95% ethanol, food stage 95% ethanol and Fructus Citri sinensiss cortex is added in Pericarpium Citri junoris fermentation liquid
Amount ratio is 1:10～25,60～70 DEG C of reflux, extract, 1～3 time, 3～5h every time, sucking filtration, merging filtrate, 50～70 DEG C of decompressions are dense
It is reduced to the 1/5～1/10 of original volume for purification, referred to as Pericarpium Citri junoris concentrated solution；
3) purification by macroporous resin：
A. resin pretreatment：Ethanol is put net after soaking macroporous resin 2～4h, repeat 3～4 times, then with the abundant drip washing of clear water
To not showing muddy, no ethanol abnormal smells from the patient, be sufficiently absorbed through moisture with filter paper；
B. macroporous resin static adsorption：By 1L above-mentioned steps 2) Pericarpium Citri junoris concentrated solution proportioning 40g～120g macroporous resin
Amount, macroporous adsorbent resin is put in bottle, add above-mentioned steps 2) concentrated solution, adjust pH4～6, at 25～45 DEG C, turn
12～48h is shaken under the conditions of fast 100～240rpm；
C. macroporous resin desorption：By the resin of above-mentioned steps (b) adsorption saturation, remove surface remaining with distillation water wash
Concentrated solution, be then placed in conical flask, add mass percent concentration be 35～85% ethanol stripping liquid, 25～45
DEG C, vibrate desorbing 12～48h under the conditions of rotating speed 100～240rpm, then 50-60 DEG C of this stripping liquid is evaporated to relatively close
Spend the extractum for 1.0～1.2, as refine Fructus Citri sinensiss spice.
Further, described macroporous resin is AB-8, X-5, D101, DS401, HP-20, HPD400 one kind therein.
The present invention also provide a kind of refined Fructus Citri sinensiss spice of said method preparation application it is characterised in that：By described essence
Fructus Citri sinensiss spice in mass ratio 0.001～0.01% processed is added in reconstituted tobacco so as to appearance luster is more naturally uniform, and with
Flue gas is coordinated, abundant fragrance, increases back sweet sense, soft flue gas, reduces and stimulates and reduce miscellaneous QI.
The present invention also provide a kind of refined Fructus Citri sinensiss spice of said method preparation application it is characterised in that：By described essence
Fructus Citri sinensiss spice in mass ratio 0.001～0.01% processed is added to use, abundant novel tobacco system in novel tobacco product propellant
The fragrance of product, promoting or transferring cigarette perfume, the sweet sense of increase.
Beneficial effects of the present invention：
Refined Fructus Citri sinensiss spice provided by the present invention, raw fragrant through beta-glucosidase enzyme fermentation, then return through certain ethanol solution
Stream extract, macroporous resin adsorption-desorption purification enrichment, remove be unfavorable for fragrance, inhale taste irritating macromolecular components such as
Protein, cellulose, polysaccharide etc., degraded, conversion macromole are small molecule volatile aroma substance, and abundant fragrance improves fragrance
Quality, reduces stimulating component.This refined Fructus Citri sinensiss fragrance applications, in reconstituted tobacco coating fluid, is coordinated with flue gas, abundant fragrance,
Increase back sweet sense, soft flue gas, reduce and stimulate and reduce miscellaneous QI, thus improve that reconstituted tobacco zest is big, the defect more than miscellaneous QI；
It is applied in novel tobacco product propellant, can coordinate with flue gas, abundant fragrance, promoting or transferring cigarette perfume, the sweet sense of increase.
Present invention process condition is simple, and product yield is high, with short production cycle, low cost, and the raw material amount of having used big,
The advantages of natural environmental-protective is harmless, widens and improves range of application and the economic worth of Pericarpium Citri junoris, have larger commercial Application
Prospect.
Specific embodiment
Below in conjunction with specific embodiment, the technical scheme in the present invention is clearly and completely described.
Embodiment 1
A kind of preparation method of refined Fructus Citri sinensiss spice, comprises the following steps：
1) ferment：After Pericarpium Citri junoris are clean after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 80 mesh,
It is 1 in mass ratio:20 addition water, and press Pericarpium Citri junoris quality 0.05% add beta-glucosidase, stir, 45 DEG C,
Under pH natural conditions, ferment 6h, and 5min enzyme-deactivating at 100 DEG C obtains Pericarpium Citri junoris fermentation liquid；
Described beta-glucosidase is food stage, enzyme activity 10000u/g；
2) reflux, extract,：Add ethanol in Pericarpium Citri junoris fermentation liquid, be 1 with Pericarpium Citri junoris mass ratio:10,60 DEG C of reflux, extract, 2
Secondary, each 4h, sucking filtration, merging filtrate, 55 DEG C are evaporated to the 1/5 of original volume for purification, referred to as Pericarpium Citri junoris concentrated solution；
Further, in described step (2), ethanol is food stage, 95% ethanol.
3) purification by macroporous resin：
A. resin pretreatment：Ethanol is put only after soaking macroporous adsorbent resin AB-8 2h, is repeated 3 times, is more fully drenched with clear water
Cannot not be washed till aobviously muddy, no till ethanol abnormal smells from the patient, be sufficiently absorbed through moisture with filter paper；
B. macroporous resin static adsorption：By 1L above-mentioned steps 2) Pericarpium Citri junoris concentrated solution proportioning 50g macroporous resin AB-8
Amount, macroporous adsorbent resin AB-8 is put in bottle, add above-mentioned steps 2) concentrated solution, adjust pH4, at 28 DEG C, rotating speed
12h is shaken under the conditions of 120rpm；
C. macroporous resin desorption：By the resin of above-mentioned steps (b) adsorption saturation, remove surface remaining with distillation water wash
Concentrated solution, be then placed in conical flask, add mass percent concentration be 45% ethanol stripping liquid, at 28 DEG C, in rotating speed
Under the conditions of 120rpm vibrate desorbing 12h, then by this stripping liquid 50 DEG C be evaporated to the extractum that relative density is 1.15, as essence
Fructus Citri sinensiss spice processed.
Described refined Fructus Citri sinensiss spice in mass ratio 0.005% is added in reconstituted tobacco, can coordinate with flue gas, reduce cigarette
Gas pH value, abundant fragrance, increase back sweet sense, soft flue gas, pleasant impression is clean.
Embodiment 2
A kind of preparation method of refined Fructus Citri sinensiss spice, comprises the following steps：
1) ferment：After Pericarpium Citri junoris are clean after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 80 mesh,
It is 1 in mass ratio:30 addition water, and press 0.1% addition beta-glucosidase of Pericarpium Citri junoris quality, stir, in 50 DEG C, pH
Under natural conditions, ferment 10h, and 100 DEG C of 6min inactivators obtain Pericarpium Citri junoris fermentation liquid；
Described beta-glucosidase is food stage, enzyme activity 5000u/g；
2) reflux, extract,：Add ethanol in Pericarpium Citri junoris fermentation liquid, be 1 with Pericarpium Citri junoris mass ratio:15,65 DEG C of reflux, extract, 2
Secondary, each 3.5h, sucking filtration, merging filtrate, 60 DEG C are evaporated to the 1/8 of original volume for purification, referred to as Pericarpium Citri junoris concentrated solution；
Further, in described step (2), ethanol is food stage, 95% ethanol.
3) purification by macroporous resin：
A. resin pretreatment：Ethanol is put only after soaking macroporous adsorption resin X-5 3h, is repeated 3 times, is more fully drenched with clear water
Cannot not be washed till aobviously muddy, no till ethanol abnormal smells from the patient, be sufficiently absorbed through moisture with filter paper；
B. macroporous resin static adsorption：By 1L above-mentioned steps 2) Pericarpium Citri junoris concentrated solution proportioning 80g macroporous adsorption resin X-5
Amount, macroporous adsorption resin X-5 is put in bottle, add above-mentioned steps 2) concentrated solution, adjust pH4.5, at 30 DEG C, in rotating speed
20h is shaken under the conditions of 130rpm；
C. macroporous resin desorption：By the resin of above-mentioned steps (b) adsorption saturation, remove surface remaining with distillation water wash
Concentrated solution, be then placed in conical flask, add mass percent concentration be 60% ethanol stripping liquid, at 30 DEG C, in rotating speed
Under the conditions of 130rpm vibrate desorbing 20h, then by this stripping liquid 55 DEG C be evaporated to the extractum that relative density is 1.06, as essence
Fructus Citri sinensiss spice processed.
Described refined Fructus Citri sinensiss spice in mass ratio 0.003% is added in the propellant of electronics tobacco product, with flue gas association
Adjust, fragrance is more rich, has back sweet sense, promoting or transferring cigarette perfume.
Embodiment 3
A kind of preparation method of refined Fructus Citri sinensiss spice, comprises the following steps：
1) ferment：After Pericarpium Citri junoris are clean after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 120
Mesh, in mass ratio for 1:40 addition water, and press 0.3% addition beta-glucosidase of Pericarpium Citri junoris quality, stir, 55
DEG C, under pH natural conditions, ferment 12h, and 10min enzyme-deactivating at 100 DEG C obtains Pericarpium Citri junoris fermentation liquid；
Described beta-glucosidase is food stage, enzyme activity 1000u/g；
2) reflux, extract,：Add ethanol in Pericarpium Citri junoris fermentation liquid, be 1 with Pericarpium Citri junoris mass ratio:25,65 DEG C of reflux, extract, 3
Secondary, each 3h, sucking filtration, merging filtrate, 60 DEG C are evaporated to the 1/10 of original volume for purification, referred to as Pericarpium Citri junoris concentrated solution；
Further, in described step (2), ethanol is food stage, 95% ethanol.
3) purification by macroporous resin：
A. resin pretreatment：Ethanol is put only after soaking macroporous adsorbent resin D101 3h, is repeated 3 times, is more fully drenched with clear water
Cannot not be washed till aobviously muddy, no till ethanol abnormal smells from the patient, be sufficiently absorbed through moisture with filter paper；
B. macroporous resin static adsorption：By 1L above-mentioned steps 2) Pericarpium Citri junoris concentrated solution proportioning 120g macroporous adsorbent resin
The amount of D101, macroporous adsorbent resin D101 is put in bottle, add above-mentioned steps 2) concentrated solution, adjust pH5.5, at 40 DEG C,
12h is shaken under the conditions of rotating speed 200rpm；
C. macroporous resin desorption：By the resin of above-mentioned steps (b) adsorption saturation, remove surface remaining with distillation water wash
Concentrated solution, be then placed in conical flask, add mass percent concentration be 75% ethanol stripping liquid, at 40 DEG C, in rotating speed
Under the conditions of 200rpm vibrate desorbing 12h, then by this stripping liquid 52 DEG C be evaporated to the extractum that relative density is 1.10, as essence
Fructus Citri sinensiss spice processed.
Above-mentioned refined Fructus Citri sinensiss spice in mass ratio 0.001% is added in electrical heating novel tobacco product propellant to be made
With, abundant fragrance, increase back sweet sense, promoting or transferring cigarette perfume.
Test example 1：Sensorial effects are tested
Refined Fructus Citri sinensiss spice in mass ratio 0.001%, 0.005%, 0.01% prepared by embodiment 1 is added to and reproduces cigarette
In leaf (B class).Then reconstituted tobacco is loaded hermetic bag, place 80 DEG C of constant temperature 30min in an oven, close to reconstituted tobacco moisture
Suitable, roll into cigarette, put in climatic chamber (22 DEG C+1, relative humidity be 60%+2%) and smooth 48h, ask expert to smoke panel test little
Group is smoked panel test.
Result shows (being shown in Table 1), and refined Fructus Citri sinensiss spice in mass ratio 0.001% and 0.005% is added in reconstituted tobacco,
Can coordinate with flue gas, fragrance is more rich, there is back sweet sense, soft flue gas, reduce and stimulate, reduce miscellaneous QI, overcome reconstituted tobacco miscellaneous
The big defect of gas weight, stimulation.
The refined Fructus Citri sinensiss spice in mass ratio 0.003%, 0.001% of embodiment 2,3 preparation is added to electronic cigarette, electricity adds
In hot novel tobacco product propellant, abundant fragrance, promoting or transferring cigarette perfume can be played, increase back the effect (being shown in Table 2) of sweet sense.
Table 1. refines Fructus Citri sinensiss spice and is added to the sensory evaluation in reconstituted tobacco
Table 2. refines Fructus Citri sinensiss spice and is added to the sensory evaluation in electronic cigarette liquid
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and any
Belong to those skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in, all answer
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 (4)
1. a kind of preparation method of refined Fructus Citri sinensiss spice is it is characterised in that comprise the following steps：
1) ferment：After Pericarpium Citri junoris are clean after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 60～120
Mesh, in mass ratio for 1:20～50 addition water, and press 0.05～0.3% addition beta-glucosidase of Pericarpium Citri junoris quality, stirring
Uniformly, under 40～55 DEG C, pH natural conditions, ferment 3～12h, 5～10min enzyme-deactivating at 100 DEG C, obtains Pericarpium Citri junoris fermentation
Liquid；
Described beta-glucosidase is food stage, enzyme activity 100～10000u/g；
2) reflux, extract,：Food stage 95% ethanol, food stage 95% ethanol and Pericarpium Citri junoris mass ratio is added in Pericarpium Citri junoris fermentation liquid
For 1:10～25,60～70 DEG C of reflux, extract, 1～3 time, 3～5h every time, sucking filtration, merging filtrate, 50～70 DEG C are evaporated to
The 1/5～1/10 of original volume is for purification, referred to as Pericarpium Citri junoris concentrated solution；
3) purification by macroporous resin：
A. resin pretreatment：Ethanol puts net, repetition 3～4 times after soaking macroporous resin 2～4h, then with the abundant drip washing of clear water to not
Till aobvious muddiness, no ethanol abnormal smells from the patient, it is sufficiently absorbed through moisture with filter paper；
B. macroporous resin static adsorption：By 1L above-mentioned steps 2) Pericarpium Citri junoris concentrated solution proportioning 40g～120g macroporous resin amount,
Macroporous adsorbent resin is put in bottle, add above-mentioned steps 2) concentrated solution, adjust pH4～6, at 25～45 DEG C, in rotating speed 100
12～48h is shaken under the conditions of～240rpm；
C. macroporous resin desorption：By the resin of above-mentioned steps (b) adsorption saturation, remove the dense of surface remaining with distillation water wash
Contracting liquid, is then placed in conical flask, adds the ethanol stripping liquid that mass percent concentration is 35～85%, at 25～45 DEG C,
Vibrate desorbing 12～48h under the conditions of rotating speed 100～240rpm, then 50-60 DEG C of this stripping liquid is evaporated to relative density and be
1.0～1.2 extractum, as refines Fructus Citri sinensiss spice.
2. as claimed in claim 1 refine Fructus Citri sinensiss spice preparation method it is characterised in that：Described macroporous resin be AB-8,
X-5, D101, DS401, HP-20, HPD400 one kind therein.
3. a kind of application of the refined Fructus Citri sinensiss spice of method as claimed in claim 1 or 2 preparation it is characterised in that：By described essence
Fructus Citri sinensiss spice in mass ratio 0.001～0.01% processed is added in reconstituted tobacco so as to appearance luster is more naturally uniform, and with
Flue gas is coordinated, abundant fragrance, increases back sweet sense, soft flue gas, reduces and stimulates and reduce miscellaneous QI.
4. a kind of application of the refined Fructus Citri sinensiss spice of method as claimed in claim 1 or 2 preparation it is characterised in that：By described essence
Fructus Citri sinensiss spice in mass ratio 0.001～0.01% processed is added to use, abundant novel tobacco system in novel tobacco product propellant
The fragrance of product, promoting or transferring cigarette perfume, the sweet sense of increase.
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| CN106954767A (en) * | 2017-03-28 | 2017-07-18 | 西南大学 | A kind of sweet orange beverage and preparation method thereof |
| CN109953364A (en) * | 2019-01-21 | 2019-07-02 | 河南中烟工业有限责任公司 | A kind of natural vegetable powder and its preparation method and application for increasing saliva moisture feeling and returning sweet tea sense |
| CN111979049A (en) * | 2020-08-26 | 2020-11-24 | 云南中烟工业有限责任公司 | Component directional preparation method |
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