CN106387987B - A kind of preparation method and applications of red tangerine extract - Google Patents
A kind of preparation method and applications of red tangerine extract Download PDFInfo
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- CN106387987B CN106387987B CN201610859549.5A CN201610859549A CN106387987B CN 106387987 B CN106387987 B CN 106387987B CN 201610859549 A CN201610859549 A CN 201610859549A CN 106387987 B CN106387987 B CN 106387987B
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- red tangerine
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- 241000675108 Citrus tangerina Species 0.000 title claims abstract description 52
- 239000000284 extract Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 46
- 229920005989 resin Polymers 0.000 claims abstract description 46
- 241000208125 Nicotiana Species 0.000 claims abstract description 25
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 25
- 241000207199 Citrus Species 0.000 claims abstract description 24
- 235000020971 citrus fruits Nutrition 0.000 claims abstract description 24
- 239000003205 fragrance Substances 0.000 claims abstract description 18
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 14
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003546 flue gas Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- MDYZKJNTKZIUSK-UHFFFAOYSA-N tyloxapol Chemical compound O=C.C1CO1.CC(C)(C)CC(C)(C)C1=CC=C(O)C=C1 MDYZKJNTKZIUSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002304 perfume Substances 0.000 claims abstract description 9
- 230000001737 promoting effect Effects 0.000 claims abstract description 9
- 235000019505 tobacco product Nutrition 0.000 claims abstract description 9
- 229920002678 cellulose Polymers 0.000 claims abstract description 8
- 239000001913 cellulose Substances 0.000 claims abstract description 8
- 150000004676 glycans Chemical class 0.000 claims abstract description 8
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 8
- 239000005017 polysaccharide Substances 0.000 claims abstract description 8
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 8
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 8
- 101710118538 Protease Proteins 0.000 claims abstract description 7
- 101000693530 Staphylococcus aureus Staphylokinase Proteins 0.000 claims abstract description 7
- 230000002708 enhancing effect Effects 0.000 claims abstract description 7
- 239000002932 luster Substances 0.000 claims abstract description 7
- 108010059892 Cellulase Proteins 0.000 claims abstract description 6
- 229940106157 cellulase Drugs 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 102000004190 Enzymes Human genes 0.000 claims description 17
- 108090000790 Enzymes Proteins 0.000 claims description 17
- 229940088598 enzyme Drugs 0.000 claims description 17
- 239000012141 concentrate Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000003795 desorption Methods 0.000 claims description 10
- 238000001179 sorption measurement Methods 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000009990 desizing Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 5
- 229920001277 pectin Polymers 0.000 claims description 5
- 239000001814 pectin Substances 0.000 claims description 5
- 235000010987 pectin Nutrition 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
- 235000013305 food Nutrition 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000000215 hyperchromic effect Effects 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000000855 fermentation Methods 0.000 abstract description 3
- 230000004151 fermentation Effects 0.000 abstract description 3
- 229920002521 macromolecule Polymers 0.000 abstract description 3
- 238000000638 solvent extraction Methods 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 239000002085 irritant Substances 0.000 description 2
- 231100000021 irritant Toxicity 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 206010036790 Productive cough Diseases 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 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 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 108010047754 beta-Glucosidase Proteins 0.000 description 1
- 102000006995 beta-Glucosidase Human genes 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000012505 colouration Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000014103 egg white Nutrition 0.000 description 1
- 210000000969 egg white Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 208000024794 sputum Diseases 0.000 description 1
- 210000003802 sputum Anatomy 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000000115 thoracic cavity Anatomy 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
- 239000013579 wash concentrate Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- 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
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
Abstract
The present invention provides a kind of preparation method and applications of red tangerine extract, using Citrus reticuiata Blano as raw material, after clean dry, crush, take cellulase, neutral proteinase, endo protease, the life of exoproteinase composite fermentation fragrant, then solvent extraction combination macroreticular resin purification techniques, remove the macromolecular substances such as protein, cellulose, polysaccharide, red tangerine extract is prepared, and is applied in reconstituted tobacco, makes its appearance luster more naturally uniform, and coordinate with flue gas, abundant fragrance, reducing stimulates and reduces miscellaneous gas, improves and inhales taste；And used in electrical heating novel tobacco product Alevaire, enrich fragrance and promoting or transferring cigarette perfume, enhancing throat comfortableness.
Description
Technical field
The present invention relates to cigarette additive technical field, specifically a kind of preparation method and applications of red tangerine extract.
Background technology
Reconstituted tobaccos, adhesive and other additives etc. are mainly added by offal, fragment, offal or discarded tobacco leaf and formed,
Relaxed and comfortable to spend, a certain amount of filling can reduce harmful ingredients in flue gas and adjustable nicotine tar content in cigarette, but there is also miscellaneous
The suction taste defects such as gas weight, excitant are big and mouthfeel is uncomfortable, have impact on using effect and addition of the reconstituted tobacco in cigarette product
Amount.Domestic common practice is improved using the method for additive, is increasingly strengthened with the consciousness of people's back to nature,
The mankind confirm that natural extract has irreplaceable important value as food additives.It is using more additive at present
Tobacco, natural plant kind extract, these extracts are typically obtained by water, alcohol extracting or molecular distillation, to cigarette after addition
The improvement limitation of quality, it is still irritant big, miscellaneous gas is more the defects of.
Tangerine is the character in popular form of tangerine, is the ripening fruits of a variety of tangerine classes such as rutaceae good fortune tangerine or Zhu tangerine, is often oblateness, skin
Color is orange red, bright red or orange.The most delicious flavour of red tangerine (Tangerine) fruit, rich in amino acid, vitamin, carbohydrate and ore deposit
Prime element etc., abroad very early by as important industrial crops, its ripe main colouration material of orange peel is carotenoid,
There are the less flavonoids of content and anthocyanin in addition.Contain aurantiamarin in the pericarp of red tangerine, be a kind of important natural
Flavonoids, there is important medical value, have regulating qi-flowing for strengthening spleen, the function for resolving sputum of drying, can treat thoracic cavity rise it is vexed, food
The diseases such as few vomiting and diarrhoea, cough ant phlegm.China has abundant red tangerine resource, and the pericarp for accounting for whole red tangerine weight 20% every year removes
It is a small amount of to be abandoned as outside Chinese medicine mostly as discarded object, the living resources of preciousness are not only wasted, can also seriously be polluted
Environment.Prepared by the extraction of the bioactive substance in Citrus reticuiata Blano, at present to have taken ethanol solution extraction method, water extraction method and second more
Ether extraction etc., the defects of weight in tobacco using irritant big, miscellaneous gas.
Using red tangerine (tangerine) skin as raw material, complex enzyme for hydrolyzing, solvent extraction combination macroreticular resin purification techniques are taken, is prepared red
Tangerine cigarette extract, and applied in reconstituted tobacco, its appearance luster more naturally uniformly, and coordinate with flue gas, is enriched perfume
Gas, reducing stimulates and reduces miscellaneous gas, improves and inhales taste, and is used in electrical heating novel tobacco product Alevaire, enrich fragrance and
Promoting or transferring cigarette perfume, enhancing throat comfortableness, has not been reported.
The content of the invention
It is an object of the invention to provide a kind of preparation method and applications of red tangerine extract, using Citrus reticuiata Blano as raw material, adopt
The fragrant pretreatment of mixed enzyme fermentation life is taken, decomposes, conversion macromolecular substances, discharges small molecule Aroma precursor material, then solvent extracts
Take and combine macroreticular resin purification techniques, remove protein, cellulose, the macromolecular substances such as polysaccharide, prepare red tangerine extract, and
Applied in reconstituted tobacco, its appearance luster more naturally uniformly, and coordinate with flue gas, is enriched fragrance, reducing stimulates and reduce
Miscellaneous gas, improve and inhale taste；And used in electrical heating novel tobacco product Alevaire, fragrance and promoting or transferring cigarette perfume are enriched, strengthens throat
Comfortableness.
Above-mentioned purpose is achieved through the following technical solutions：
A kind of preparation method of red tangerine extract, comprises the following steps：
1) after Citrus reticuiata Blano is cleaned after room temperature ventilation drying to constant weight, 60~120 are crushed to high speed Universal pulverizer
Mesh, it is in mass ratio 1:20~50 add water, and add complex enzyme by the 0.1~0.3% of Citrus reticuiata Blano quality, stir,
40~55 DEG C, under pH natural conditions, ferment 2~8h, 2~5min enzyme-deactivatings at 100 DEG C, obtains Citrus reticuiata Blano zymotic fluid；
The complex enzyme is：Cellulase, neutral proteinase, endo protease, exoproteinase (be food-grade, enzyme
20,000~100,000 u/g living), according to mass ratio 1~2:1:1:1 mixes；
2) solvent refluxing extracts：40~100% second for accounting in step 1) and adding water quality is added in Citrus reticuiata Blano zymotic fluid
Alcohol, 3~5h of refluxing extraction, filter, retain filtrate, less than 60 DEG C are concentrated under reduced pressure into the 1/8~1/15 of original volume for purifying；
3) macroreticular resin refines：
A. resin pre-processes：Net, repetition 3~4 times is put after 2~4h of ethanol immersion resin, then is fully eluted to not with clear water
It is aobvious muddy, without ethanol smell untill, and with filter paper suck dry moisture；
B. macroreticular resin Static Adsorption：By 1L above-mentioned steps 2) amounts of concentrate proportioning 50g~100g macroreticular resins, will be big
Macroporous adsorbent resin is put into bottle, add above-mentioned steps 2) concentrate, adjust pH3~6, at 25~50 DEG C, rotating speed 110~
18~48h is shaken under the conditions of 250rpm, further except big molecular impurities such as desizing, protein, pectin, cellulose, polysaccharide；
C. macroreticular resin desorption：By the resin of above-mentioned steps (b) adsorption saturation, surface remaining is removed with distillation water wash
Concentrate, be then placed in conical flask, add mass percent concentration be 30~90% ethanol stripping liquid, 25~55
DEG C, 16~48h of vibration desorption under the conditions of 100~250rpm of rotating speed, then 50-60 DEG C of the stripping liquid is concentrated under reduced pressure into relatively close
Spend the medicinal extract for 1.0~1.2, as red tangerine extract.
Further, ethanol is food-grade in the step (2), 95% ethanol.
Further, the macroreticular resin is one kind in D072, D401, D-301, GD-101.
The present invention also provides a kind of application of red tangerine extract prepared by above method, it is characterised in that：By the red tangerine
Extract in mass ratio 0.01~0.1% is added in reconstituted tobacco, makes its appearance luster more naturally uniform, is assisted with flue gas
Adjust, enrich fragrance, reducing stimulates and reduce miscellaneous gas, improves and inhales taste.
The present invention also provides a kind of application of red tangerine extract prepared by above method, it is characterised in that：By the red tangerine
Extract in mass ratio 0.01~0.05%, which is added in electrical heating novel tobacco product Alevaire, to be used, and enriches fragrance, promoting or transferring
Cigarette perfume, enhancing throat comfortableness.
Red tangerine extract provided by the present invention, through beta-glucosidase, neutral proteinase, endo protease, circumscribed egg
White enzyme mixed fermentation life is fragrant, then is extracted through certain ethanol solution, and macroporous resin adsorption-desorption purification enrichment refines, and removes not
Beneficial to fragrance, irritating macromolecular components such as protein, cellulose, polysaccharide etc. of suction taste, degraded, conversion macromolecular are small point
Sub- Volatile infochemicals, fragrance is enriched, improve flavouring essence quality.Make an addition in reconstituted tobacco coating fluid, make reconstituted tobacco outward appearance
Color and luster is more naturally uniform；Coordinate simultaneously with flue gas, enrich fragrance, reducing stimulates and reduce miscellaneous gas, promoting or transferring flavouring essence quality, improves
Taste is inhaled, so as to improve the defects of reconstituted tobacco excitant is big, miscellaneous gas is more；Applied in electrical heating novel tobacco product Alevaire,
It can coordinate with flue gas, enrich fragrance, promoting or transferring cigarette perfume, enhancing throat comfortableness.
Present invention process condition is simple, and product yield is high, and with short production cycle, cost is low, and raw material used have amount it is big,
The advantages that natural environmental-protective is harmless, the application and economic value of Citrus reticuiata Blano are widened and improved, there is larger commercial Application
Prospect.
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 red tangerine extract, comprises the following steps：
1) after Citrus reticuiata Blano is cleaned after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 60 mesh, by matter
Amount is than being 1:20 add water, and add complex enzyme by the 0.1% of Citrus reticuiata Blano quality, stir, in 40 DEG C, pH natural conditions
Under, ferment 6h, 5min enzyme-deactivatings at 100 DEG C, obtains Citrus reticuiata Blano zymotic fluid；
The complex enzyme is：Cellulase, neutral proteinase, endo protease, exoproteinase (be food-grade, enzyme
20,000 u/g living), according to mass ratio 2:1:1:1 mixes；
2) solvent refluxing extracts：60% ethanol for accounting in step 1) and adding water quality is added in Citrus reticuiata Blano zymotic fluid, is returned
Stream extraction 3h, is filtered, and retains filtrate, and 60 DEG C are concentrated under reduced pressure into the 1/8 of original volume for purifying, and are red tangerine concentrate；
Ethanol is food-grade in the step (2), 95% ethanol.
3) macroreticular resin refines：
A. resin pre-processes：Put net after ethanol immersion resin 3h, be repeated 3 times, then fully eluted with clear water to it is not aobvious it is muddy,
Untill without ethanol smell, and with filter paper suck dry moisture；
B. macroreticular resin Static Adsorption：By 1L above-mentioned steps 2) concentrate proportioning 50g macroreticular resins amount, by macroporous absorption
Resin D072 is put into bottle, add above-mentioned steps 2) concentrate, adjust pH 4, at 25 DEG C, shaken under the conditions of rotating speed 110rpm
18h is swung, further except big molecular impurities such as desizing, protein, pectin, cellulose, polysaccharide；
C. macroreticular resin desorption：By the resin of above-mentioned steps 2 (b) adsorption saturation, it is residual to remove surface with distillation water wash
The concentrate deposited, is then placed in conical flask, adds the ethanol stripping liquid that mass percent concentration is 40%, at 25 DEG C, is turning
Vibration desorption 16h under the conditions of fast 100rpm, then 50 DEG C of the stripping liquid is concentrated under reduced pressure into the medicinal extract that relative density is 1.08, it is
Red tangerine extract.
The red tangerine extract in mass ratio 0.01% is added in reconstituted tobacco, can be coordinated with flue gas, reduces flue gas
PH value, fragrance is enriched, reducing stimulates and reduce miscellaneous gas, improves and inhales taste.
Embodiment 2
A kind of preparation method of red tangerine extract, comprises the following steps：
1) after Citrus reticuiata Blano is cleaned after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 80 mesh, by matter
Amount is than being 1:30 add water, and add complex enzyme by the 0.2% of Citrus reticuiata Blano quality, stir, in 45 DEG C, pH natural conditions
Under, ferment 7h, 4min enzyme-deactivatings at 100 DEG C, obtains Citrus reticuiata Blano zymotic fluid；
The complex enzyme is：Cellulase, neutral proteinase, endo protease, exoproteinase (be food-grade, enzyme
50,000 u/g living), according to mass ratio 1.5:1:1:1 mixes；
2) solvent refluxing extracts：70% ethanol for accounting in step 1) and adding water quality is added in Citrus reticuiata Blano zymotic fluid, is returned
Stream extraction 4h, is filtered, and retains filtrate, and 60 DEG C are concentrated under reduced pressure into the 1/10 of original volume for purifying, and are red tangerine concentrate；
Ethanol is food-grade in the step (2), 95% ethanol.
3) macroreticular resin refines：
A. resin pre-processes：Put net after ethanol immersion resin 2h, be repeated 4 times, then fully eluted with clear water to it is not aobvious it is muddy,
Untill without ethanol smell, and with filter paper suck dry moisture；
B. macroreticular resin Static Adsorption：By 1L above-mentioned steps 2) concentrate proportioning 65g macroreticular resins amount, by macroporous absorption
Resin D401 is put into bottle, add above-mentioned steps 2) concentrate, adjust pH5, at 30 DEG C, shaken under the conditions of rotating speed 150rpm
24h, further except big molecular impurities such as desizing, protein, pectin, cellulose, polysaccharide；
C. macroreticular resin desorption：By the resin of above-mentioned steps 2 (b) adsorption saturation, it is residual to remove surface with distillation water wash
The concentrate deposited, is then placed in conical flask, adds the ethanol stripping liquid that mass percent concentration is 70%, at 35 DEG C, is turning
Vibration desorption 24h under the conditions of fast 150rpm, then 55 DEG C of the stripping liquid is concentrated under reduced pressure into the medicinal extract that relative density is 1.12, it is
Red tangerine extract.
The red tangerine extract in mass ratio 0.05% is added in reconstituted tobacco, makes appearance luster more naturally equal
It is even, coordinate with flue gas, enrich fragrance, improve and inhale taste, drop thorn subtracts miscellaneous.
Embodiment 3
A kind of preparation method of red tangerine extract, comprises the following steps：
1) after Citrus reticuiata Blano is cleaned after room temperature ventilation drying to constant weight, high speed Universal pulverizer is crushed to 100 mesh, by matter
Amount is than being 1:45 add water, and add complex enzyme by the 0.25% of Citrus reticuiata Blano quality, stir, in 50 DEG C, pH natural conditions
Under, ferment 8h, 5min enzyme-deactivatings at 100 DEG C, obtains Citrus reticuiata Blano zymotic fluid；
The complex enzyme is：Cellulase, neutral proteinase, endo protease, exoproteinase (be food-grade, enzyme
100,000 u/g living), according to mass ratio 1:1:1:1 mixes；
2) solvent refluxing extracts：90% ethanol for accounting in step 1) and adding water quality is added in Citrus reticuiata Blano zymotic fluid, is returned
Stream extraction 3h, is filtered, and retains filtrate, and 60 DEG C are concentrated under reduced pressure into the 1/10 of original volume for purifying, and are red tangerine concentrate；
Ethanol is food-grade in the step (2), 95% ethanol.
3) macroreticular resin refines：
A. resin pre-processes：Put net after ethanol immersion resin 3h, be repeated 3 times, then fully eluted with clear water to it is not aobvious it is muddy,
Untill without ethanol smell, and with filter paper suck dry moisture；
B. macroreticular resin Static Adsorption：By 1L above-mentioned steps 2) concentrate proportioning 100g macroreticular resins amount, macropore is inhaled
Attached resin D301 is put into bottle, add above-mentioned steps 2) concentrate, adjust pH6, at 40 DEG C, shaken under the conditions of rotating speed 180rpm
32h is swung, further except big molecular impurities such as desizing, protein, pectin, cellulose, polysaccharide；
C. macroreticular resin desorption：By the resin of above-mentioned steps 2 (b) adsorption saturation, it is residual to remove surface with distillation water wash
The concentrate deposited, is then placed in conical flask, adds the ethanol stripping liquid that mass percent concentration is 80%, at 40 DEG C, is turning
Vibration desorption 32h under the conditions of fast 180rpm, then 55 DEG C of the stripping liquid is concentrated under reduced pressure into the medicinal extract that relative density is 1.15, it is
Red tangerine extract.
Above-mentioned red tangerine cigarette extract in mass ratio 0.01%, which is added in electrical heating novel tobacco product Alevaire, to be made
With abundant fragrance, promoting or transferring cigarette perfume, enhancing throat comfortableness.
Test example 1：Sensorial effects are tested
Red tangerine extract in mass ratio 0.01%, 0.03%, 0.05% prepared by embodiment 1-2 is added to reconstituted tobacco
In (B classes).Then reconstituted tobacco is loaded into hermetic bag, places 80 DEG C of constant temperature 30min in an oven, closed to reconstituted tobacco moisture
It is suitable, cigarette is rolled into, (22 DEG C+1, relative humidity 60%+2%) smooth 48h is put into climatic chamber, asks expert to smoke panel test small
Group is smoked panel test.
As a result (being shown in Table 1) is shown, red tangerine extract in mass ratio 0.01% and 0.03% is added in reconstituted tobacco, can be with
Flue gas is coordinated, and reduces smoke pH, enriches fragrance, improves and inhales taste, and reducing stimulates, reduces miscellaneous gas, overcome reconstituted tobacco miscellaneous gas weight,
Stimulate the defects of big.
The red tangerine extract of table 1. is added to the sensory evaluation in reconstituted tobacco
Red tangerine extract in mass ratio 0.01%, 0.03% prepared by embodiment 3 is added to electrical heating novel tobacco system
In product Alevaire, abundant fragrance, promoting or transferring cigarette perfume, enhancing throat's comfortableness (being shown in Table 2) can be played a part of.
The red tangerine extract of table 2. is added to the sensory evaluation in electrical heating novel tobacco product Alevaire
Claims (4)
1. a kind of preparation method of red tangerine extract, it is characterised in that the red tangerine extract is used to be added to reconstituted tobacco or add
It is added in electrical heating novel tobacco Alevaire, is used for hyperchromic flavouring when being used in reconstituted tobacco, makes appearance luster more natural
It is even, and coordinate with flue gas, fragrance is enriched, reducing stimulates and reduce miscellaneous gas, improves and inhales taste；It is atomized in electrical heating novel tobacco product
It is used to enrich fragrance and promoting or transferring cigarette perfume, enhancing throat comfortableness when using in agent, the preparation method comprises the following steps：
1) after Citrus reticuiata Blano is cleaned after room temperature ventilation drying to constant weight, 60~120 mesh is crushed to high speed Universal pulverizer, are pressed
Mass ratio is 1:20~50 add water, and add complex enzyme by the 0.1~0.3% of Citrus reticuiata Blano quality, stir, 40~55
DEG C, under pH natural conditions, ferment 2~8h, 2~5min enzyme-deactivatings at 100 DEG C, obtains Citrus reticuiata Blano zymotic fluid；
The complex enzyme is：Cellulase, neutral proteinase, endo protease, exoproteinase, according to mass ratio 1~2:1:
1:1 mixes；
2) solvent refluxing extracts：40~100% ethanol for accounting in step 1) and adding water quality is added in Citrus reticuiata Blano zymotic fluid, is returned
Stream 3~5h of extraction, is filtered, and retains filtrate, and less than 60 DEG C are concentrated under reduced pressure into the 1/8~1/15 of original volume for purifying；
3) macroreticular resin refines：
A. resin pre-processes：Net, repetition 3~4 times is put after 2~4h of ethanol immersion resin, then is fully eluted to not aobvious muddy with clear water
It is turbid, without ethanol smell untill, and with filter paper suck dry moisture；
B. macroreticular resin Static Adsorption：By 1L above-mentioned steps 2) concentrate proportioning 50g~100g macroreticular resins amount, macropore is inhaled
Attached resin is put into bottle, add above-mentioned steps 2) concentrate, adjust pH3~6, at 25~50 DEG C, in 110~250rpm of rotating speed
Under the conditions of shake 18~48h, further except desizing, protein, pectin, cellulose, polysaccharide, the macroreticular resin be D072,
One kind in D401, D-301, GD-101；
C. macroreticular resin desorption：By the resin of above-mentioned steps (b) adsorption saturation, the dense of surface remaining is removed with distillation water wash
Contracting liquid, is then placed in conical flask, adds the ethanol stripping liquid that mass percent concentration is 30~90%, at 25~55 DEG C,
16~48h of vibration desorption under the conditions of 100~250rpm of rotating speed, then 50-60 DEG C of the stripping liquid is concentrated under reduced pressure into relative density and is
1.0~1.2 medicinal extract, as red tangerine extract.
2. the preparation method of red tangerine extract as claimed in claim 1, it is characterised in that：Ethanol is food in the step (2)
Grade, 95% ethanol.
A kind of 3. application of red tangerine extract prepared by method as any one of claim 1-2, it is characterised in that：By institute
Red tangerine extract in mass ratio 0.01~0.1% is stated to be added in reconstituted tobacco.
A kind of 4. application of red tangerine extract prepared by method as any one of claim 1-2, it is characterised in that：By institute
Red tangerine extract in mass ratio 0.01~0.05% is stated to be added in electrical heating novel tobacco product Alevaire.
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