CN103710150B - Tobacco flavor and preparation method thereof - Google Patents
Tobacco flavor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a tobacco flavor and a preparation method thereof. The preparation method comprises the following steps: (1) sequentially adding cellulase, pectinase, alpha-amylase and Serratia peptidase in an extraction process of compound Chinese herbal medicines, fully extracting active ingredients in the compound Chinese herbal medicines through a biological enzymolysis technology, adding 95% ethanol for inactivation and performing secondary extraction after the completion of enzymolysis, and filtering and concentrating after full extraction; (2) performing Maillard reaction on a concentrated solution obtained by preparation and compound amino acids; (3) performing staged treatment on a Maillard reaction solution obtained by preparation through a membrane separation technology according to molecular weight and functionality; (4) performing combination and compounding on membrane separation components obtained in various stages by smoking quality evaluation, and finally preparing the tobacco flavor provided by the invention. The flavor is added into cigarettes in an appropriate ratio and can further realize the effects of enhancing flavor, reducing irritation, covering mixed gas, coordinating smoke gas, reducing irritation of the oral cavity of the throat and improving the aftertaste in the oral cavity.
Description
Technical field
The present invention relates to technical field of tobacco, especially a kind of tobacco aromatics using and preparation method thereof.
Background technology
Progressively reduce cigarette products tar content, Development of Novel low-coke tar cigarette is the overall development trend of domestic and international tobacco.But facts have proved: while coke tar in cigarette reduces, the fragrance matter in cigarette is corresponding minimizing also, and cigarette sense organ comfort level is deteriorated.Flavoring and casing is the important means solved the problem at present, and therefore the functional tobacco aromatics using of development of new becomes the important technical keeping suction quality while tobacco industry reduces tar.
Herbal medicine is as China's tradition rarity, aboundresources, various in style.Through distilling, gasifying, volatilize or sublimation process after modern study shows the pharmacological component burning that herbal medicine contains, form particulate phase and gas phase composition, the drug particle of these different-grain diameters acts on human respiratory, or be deposited on mouth and nose, respiratory tract, or directly absorbed into blood by alveolar, thus performance effect, and then reduce negative sensory's effect that cigarette smoking brings human body, improve the comfort level of cigarette smoking.And the fragrant homology of medicine, in herbal medicine, a lot of pharmacological component is also important aroma component simultaneously, aroma component contained by many Chinese herbal medicines and tobacco aroma component have very large similarity, and therefore herbal medicine becomes tobacco aromatics using important source material source day by day.China's herbal medicine is theoretical of extensive knowledge and profound scholarship, and wherein compatibility of medicines in a prescription research history is long.Saying of its monarch shows specific function to occur between herbal medicine, and the extraction of this acting in conjunction to the overall curative effect of Chinese medicine and effective constituent all serves special role.With regard to its on extraction impact with regard to, summed up: side effect falls in synergistic effect, stripping promoter action and attenuation.
Current compound Chinese herb, as one of very important tobacco aromatics using source, has been widely used in cigarette composition in recent years.Chinese patent " CN 102499455 A " discloses and utilizes the compound Chinese medicine extract such as Unibract Fritillary Bulb, Loquat Leaf, Root of Upright Ladybell, Poria cocos, Pummelo Peel to improve cigarette to throat's comfortableness; Chinese patent " CN 103082403 A " discloses a kind of tobacco aromatics using utilizing ferment the tuber of dwarf lilyturf and preparation method thereof and application, the spices prepared except have the tuber of dwarf lilyturf itself fragrant and sweet except, add ester perfume (or spice), more coordinate with cigarette perfume (or spice), reduce and stimulate, reduce assorted gas.
According to technical study achievement, we have chosen has the asparagus fern of better effect, the tuber of dwarf lilyturf, Poria cocos and Root of Pubescent Holly to carry out compound extraction to cigarette compensating aroma, suction comfort level, up to the present, also do not utilize said herbal medicine assembly, use the report of modern separation and Extraction and purification technique exploitation cigarette perfume material.
Summary of the invention
The object of the invention is to provide a kind of functional tobacco aromatics using that can improve low-coke tar cigarette suction quality and preparation method thereof.
The present inventor, through exploring for many years, works out compound Chinese herb tobacco aromatics using of the present invention and preparation method thereof.The present invention is achieved by the following technical solutions:
1, asparagus fern, the tuber of dwarf lilyturf, Poria cocos, Root of Pubescent Holly are dried and pulverized, add water and multiple enzyme enzymolysis successively after mixing, the complete interpolation ethanol of enzymolysis carries out deactivation and second extraction, filters, concentrates;
2, concentrated solution step 1 obtained and aminoacids complex carry out Maillard reaction;
3, step 2 gained Maillard reaction liquid is carried out segmentation and retains according to molecular weight and cigarette with functional by membrane separation technique, it is 30 ° of B é that the different section constituent unit obtained are concentrated into solution degree Beaume;
4, by Chinese-style cigarette sensory evaluation and blending experience, step 3 obtained component unit is carried out combination by panel of experts composite, prepare functional tobacco aromatics using required for the present invention.
The preparation method of tobacco aromatics using of the present invention carries out according to the following steps:
(1) by weight part asparagus fern 40 ~ 60, the tuber of dwarf lilyturf 20 ~ 40, Poria cocos 10 ~ 25, Root of Pubescent Holly 5 ~ 10, total amount is after the herbal powder mixing of 100 parts, according to weight ratio powder: water=1:5 ~ 1:10 adds water, ultrasonic immersion 10 ~ 20 minutes at 25 DEG C;
(2) cellulase added and polygalacturonase prozyme carry out the first step enzymolysis, hydrolysis temperature 50 ~ 55 DEG C, enzymolysis pH value 3.5 ~ 4.5, reaction times 1-5 hour, and enzyme addition is 2 ‰ ~ 5 ‰ of herbal powder quality;
(3) add α-amylase and carry out second step enzymolysis, hydrolysis temperature 65 ~ 80 DEG C, enzymolysis pH value 7 ~ 7.5, reaction times 2-8 hour, enzyme addition is 0.5 ‰ ~ 2 ‰ of herbal powder quality;
(4) add serrapeptass and carry out the 3rd step enzymolysis, hydrolysis temperature 35-40 DEG C, enzymolysis pH value 7 ~ 7.5, reaction times 1-2 hour, enzyme addition is 0.5 ‰ ~ 1 ‰ of herbal powder quality;
(5) adding 95% ethanol to solution ethanol concentration is stir extraction 1 ~ 4 hour at 50% ~ 75%, 50 ~ 80 DEG C, and extract fully, filtering and concentrating to solution degree Beaume is 10 ° of B é ~ 25 ° B é;
(6) in step (5) concentrated solution, add amino acid and carry out Maillard reaction, add-on is 10% ~ 20% of concentrated solution quality; PH value of reaction system 6.5 ~ 8.0, temperature of reaction 60 ~ 80 DEG C, agitation condition lower seal reaction 6 ~ 10 hours, after sufficient reacting, filters after ultrasonic 15 minutes, obtains Maillard reaction liquid after removing filter residue;
(7) the Maillard reaction liquid that step (6) prepares is carried out membrane sepn, obtain tobacco flavor components unit, being finally concentrated into degree Beaume is that 30 ° of B é solution M1, M2 and M3 are in order to composite;
(8) by M1 5 ~ 9 parts, M2 45 ~ 65 parts, M3 10 ~ 20 parts, propylene glycol 20 ~ 35 parts, gross weight 100 parts is carried out composite, obtains tobacco aromatics using.
Described asparagus fern, the tuber of dwarf lilyturf, Poria cocos, Root of Pubescent Holly herbal powder mixture granularity < 100 order.
Described in step (2), the prozyme compositely proportional of cellulase and polygalacturonase is 10:1 ~ 6:1.
Step (6) described aminoacids complex comprises leucine, Isoleucine, α-amino-isovaleric acid and phenylalanine, and compositely proportional is leucine 15 ~ 24 parts, Isoleucine 12 ~ 17 parts, α-amino-isovaleric acid 3 ~ 11 parts, phenylalanine 50 ~ 65 parts, gross weight 100 weight part.
Membrane sepn described in step (7) comprises the following steps:
A, to be filtered by molecular weight cut-off 1000dalton ultra-filtration membrane, ultra-filtration membrane working pressure: 0.1-0.2MPa, operating temperature: 25 ~ 35 DEG C;
B, above-mentioned ultra-filtration membrane filtrate through molecular weight cut-off 400dalton nanofiltration membrane, working pressure: 1.5-2.0MPa, operating temperature: 40 ~ 50 DEG C;
C above-mentioned nanofiltration membrane gained filtrate again through molecular weight cut-off 200dalton nanofiltration membrane, working pressure: 0.5-1.0MPa, operating temperature: 40 ~ 50 DEG C;
D, above-mentioned 400dalton nanofiltration membrane trapped substance, 200dalton nanofiltration membrane trapped substance and 200dalton permeate are carried out vacuum concentration respectively, thickening temperature 45 ~ 55 DEG C, being finally concentrated into degree Beaume is that solution M1, M2 and M3 of 30 ° of B é are in order to composite.
Mentality of designing of the present invention is: first carry out broken wall treatment with cellulase and polygalacturonase to vegetable cell, improves the stripping of active substance and promotes the carrying out of follow-up enzyme digestion reaction; Then adopt α-amylase to be degrade for the more starch component contained asparagus fern, the tuber of dwarf lilyturf, the small molecules sugar of gained is one of important sugared source of follow-up Maillard reaction; Serrapeptass, obtained through fermented extracted by subtilis, belong to a kind of restriction endonuclease, can be used for various proteolysis process, vegeto-animal macro-molecular protein can be hydrolyzed into small-molecular peptides or amino acid, its hydrolyzed solution degree of hydrolysis is high, and local flavor is good, has been widely used in and has produced senior seasonings and food enrichment.Utilize the broad spectrum that it is applied in the present invention, proteolysis all kinds of in compound Chinese herb is become small molecules amino acid, using as follow-up Maillard reaction nitrogenous source.
Described Maillard reaction mentality of designing is through data check and detection, in whole formula extracting solution, carbohydrate content will more than aminoacids content, in order to make Maillard reaction abundant, have chosen good four seed amino acids of effect in several cigarette Maillard reaction spices preparation in early stage additional, thus produce the aroma component that more multipair cigarette has significant contribution.After reacting completely, have part melanoidin by hydrogen bond can adsorb a part we needed for aroma component separate out together.Therefore there is the melanoidin of negative effect to retain required aroma component to remove to cigarette smoking simultaneously, adopt supersound process, utilize the hydrogen bond of hyperacoustic energy damages melanoidin, the aroma component making it adsorb is again molten to be got back in the middle of solution, then by filtering the part melanoidin removed and separate out.
Membrane sepn step of the present invention designs with functional carrying out according to the molecular weight of chemical composition in solution after above-mentioned Maillard reaction and cigarette.After Maillard reaction, solution is still containing high molecular polymers such as the melanoidins produced in the macromole product such as promising reactive protein, Mierocrystalline cellulose and Maillard reaction, and these materials can bring assorted gas, stimulation bring negative mouthfeel to cigarette smoking.And Chinese medicine grass effective component required for the present invention and aroma component molecular weight are all less than 1000, molecular weight cut-off 1000dalton ultra-filtration membrane is therefore adopted to remove the macromolecular substance affecting cigarette smoking; The asparagus fern chosen in the present invention, the tuber of dwarf lilyturf and Poria cocos are all containing a large amount of triterpenoid saponin compounds, these type of goods and materials have the pharmacologically actives such as promoting production of body fluid and nourishing the lung, cough-relieving apophlegmatic, dry sensation and throat's sense of discomfort that flue gas brings can be alleviated, thus promote cigarette smoking comfort level, and effectively can reduce free radical harmful in flue gas.It is because containing bitter principle and irritates nucous membrane simultaneously, once measure slightly stool can bring stimulation and sensory issues to cigarette smoking.This segment components is both advantageous and disadvantageous to cigarette smoking quality, needs to carry out preferably its consumption with sensory evaluation by experiment.The triterpenoid saponin contained in the present invention as asparagus fern furan sterol oligosaccharides glucoside, methyl Protodioscin, the tuber of dwarf lilyturf saponin, pachymic acid, soil not sour equimolecular quantity in the scope of 400-1000, therefore we adopt molecular weight cut-off 400dalton nanofiltration membrane to collect this type of chemical composition, consider interpolation as a functional plate in follow-up composite step; Molecular weight cut-off 200dalton nanofiltration membrane object is the aroma component such as flavonoid, sesquiterpenoids, small molecules glucosides, Amadori compound of collection molecular weight 200-400 or causes fragrant precursor.These aroma components will form cigarette main body note with this perfume of tobacco, also be improved flue gas concentration, will improve flue gas texture, and improve the effects such as oral cavity pleasant impression.Wherein flavonoid compound also has and covers bitter taste, promotes the production of body fluid, moisturizes, reduces the effects such as free radical objectionable constituent in cigarette.Therefore this section of membrane sepn component will as follow-up composite main body; Molecular weight cut-off 200dalton nanofiltration membrane permeate then contain molecular weight lower than 200 Pyrazine, pyridines, the small molecules Mei Lade product such as pyroles and pyrrones; the aromatic style of these compounds to tobacco has material impact; as methylpyrazine has puffed rice and cocoa smell; pyrrole derivatives has tobacco perfume (or spice); it is fragrant that acetyl furan has grape fermented glutinous rice, and Furanones has the fragrance such as strawberry, apple.Therefore select this appropriate compounds to add cigarette to, cigarette perfume (or spice) can be enriched, modify cigarette flavor style, promote flavouring essence quality.
The M of gained
1, M
2the composite effect can played flavouring and fall thorn, cover assorted gas, coordinate flue gas, alleviate throat and oral stimulation, improve oral cavity pleasant impression is carried out with M3.
Compared with developing with existing tobacco aromatics using, tobacco aromatics using preparation method of the present invention is integrated with the several theory and technologies such as Chinese medicine preparation theory, biological enzymolysis, Maillard reaction, membrane sepn, Chinese-style cigarette sensory evaluation and blending method and has the following advantages:
1, for compound Chinese herb plant physiology structure and chemical composition composition, the preferred particular organisms enzyme of biological enzymolysis technology is utilized to carry out enzymolysis and extraction to compound Chinese herb successively according to a definite sequence, add between herbal medicine under stripping promoter action, in compound Chinese herb, the more traditional extraction method efficiency of functional ingredient improves 50% ~ 80%;
2, carbohydrate content contained by compound Chinese herb of the present invention self and amino acid enrich, and utilize Maillard reaction to make it change into a large amount of tobacco flavor composition, make up the loss of aroma that cigarette brings because reducing tar;
3, utilize membrane separation technique to have the chemical composition of difference in functionality to carry out segmentation to cigarette smoking targetedly to retain, abandon useless, unwanted component, obtain three sections and there is constituent unit cigarette being had to different efficacies, then determine according to its chemical composition composition and effect the relative merits that each constituent unit is smoked panel test to cigarette.Then according to cigarette product demand, compounded combination is carried out to each section of constituent unit, has both given full play to effect of each constituent unit, also reduced the negative effect that it brings cigarette smoking, make combination formula be better than each constituent unit and simply add and, embody the synergism of organic compatibility.Thus a kind of comprehensive tobacco aromatics using can all indexs such as cigarette flavor quality, flue gas mass, Harmony, suction comfort level, stimulation, assorted gas with good action can be obtained, expand its range of application, improve its using value.
4, tcm prescription traditional theory has been used for reference, the synergistic effect utilizing it mutual, stripping promoter action and attenuation fall side effect and fully extract pharmacology contained by it and aroma component, reduce unwanted contributions to the negative impact of cigarette smoking, and significantly reduce toxic ingredient introducing.
5, present invention process clear process, equipment requirements is simple, and cheaper starting materials is easy to get, and is convenient to application and promotes.
Embodiment
For ease of understanding the present invention better, be illustrated by following examples.But protection scope of the present invention is not limited to these embodiments.
Embodiment 1:
(1) first enzymolysis and second extraction are carried out to compound Chinese herb powder: after 40 grams of asparagus ferns, 40 grams of tubers of dwarf lilyturf, 15 grams of Poria cocos and 5 grams of Root of Pubescent Holly herbal powders (granularity < 100 order) are mixed and 500 grams of water add in extraction vessel, to be first placed under ultrasound environments soak at room temperature 10 minutes.Then carry out the first step enzymolysis, enzyme used is the prozyme of cellulase and polygalacturonase combination, and the weight ratio of cellulase and polygalacturonase is 8:1, hydrolysis temperature 50 DEG C, with citric acid regulating solution pH value to 3.5, enzymolysis time 5 hours, enzyme dosage is 2 ‰ of compound Chinese herb powder weight; Second step enzymolysis enzyme used is α-amylase, hydrolysis temperature 65 DEG C, and with salt of wormwood regulator solution pH value to 7.0, enzymolysis time 6 hours, enzyme dosage is 1 ‰ of compound Chinese herb powder weight; 3rd step enzymolysis enzyme used is serrapeptass, hydrolysis temperature 35 DEG C, and solution ph remains 7.0, enzymolysis time 1 hour, and enzyme dosage is 0.5 ‰ of compound Chinese herb powder weight.
After enzymolysis, adding 95% ethanol to extracting solution alcohol concn is 50% carry out second extraction and simultaneously deactivation, Extracting temperature 50 DEG C, 1 hour extraction time, extracts fully, crosses to filter filter residue final vacuum to be concentrated into solution degree Beaume be 10 ° of B é.
(2) extract concentrated solution for reactive agent with above-mentioned steps (1) gained, add aminoacids complex and carry out Maillard reaction: regulate pH value of reaction system to 7.5, temperature of reaction is 60 DEG C, react 10 hours under agitation condition; After sufficient reacting, filter after ultrasonic 15 minutes, after removing filter residue, obtain Maillard reaction liquid.Described aminoacids complex comprises leucine, Isoleucine, α-amino-isovaleric acid and phenylalanine, and compositely proportional is leucine 15 parts, Isoleucine 15 parts, α-amino-isovaleric acid 7 parts, phenylalanine 63 parts, total amount 100 parts, and aminoacids complex add-on is extract concentrated solution quality 10%;
(3) Mei Lade product reaction solution above-mentioned steps (2) prepared first filters with molecular weight cut-off 1000dalton ultra-filtration membrane, working pressure: 0.1MPa, operating temperature: 25 DEG C; Ultra-filtration membrane filtrate again through molecular weight cut-off 400dalton nanofiltration membrane, working pressure: 1.5MPa, temperature: 40 DEG C; Gained filtrate is filtered through molecular weight cut-off 200dalton nanofiltration membrane again, working pressure: 0.5MPa, temperature: 40 DEG C, then obtains by vacuum concentration the 400dalton nanofiltration membrane trapped substance solution M that degree Beaume is 30 ° of B é
1, 200dalton nanofiltration membrane trapped substance solution M
2with 200dalton nanofiltration membrane permeate concentrated solution M
3,, vacuum concentration temperature 50 C.
(4) the professional blending personnel of tissue are to the M of step 3 gained
1, M
2chinese-style cigarette sensory evaluation is carried out with M3, formula combination is carried out according to evaluation result and blending experience, again according to screening formulation by the spices allocated be sprayed on tobacco leaf according to Conventional feed introduction processing sequence, then in climatic chamber, balance 18 hours, then roll into cigarette evaluation.According to effect determination tobacco flavor components of the present invention, gross weight 100 parts: M
19 parts, M
250 parts, M
315 parts, propylene glycol 26 parts.
embodiment 2:
(1) first enzymolysis and second extraction are carried out to compound Chinese herb powder: after 50 grams of asparagus ferns, 25 grams of tubers of dwarf lilyturf, 18 grams of Poria cocos and 7 grams of Root of Pubescent Holly herbal powders (granularity < 100 order) are mixed and 1000 grams of water add in extraction vessel, to be first placed under ultrasound environments soak at room temperature 20 minutes.Then carry out the first step enzymolysis, enzyme used is the prozyme of cellulase and polygalacturonase combination, and the weight ratio of cellulase and polygalacturonase is 6:1, hydrolysis temperature 55 DEG C, by citric acid regulating solution pH value to 4, enzymolysis time 1 hour, enzyme dosage is 5 ‰ of compound Chinese herb powder weight; Second step enzymolysis enzyme used is α-amylase, hydrolysis temperature 80 DEG C, and with salt of wormwood regulator solution pH value to 7.5, enzymolysis time 5 hours, enzyme dosage is 2 ‰ of compound Chinese herb powder weight; 3rd step enzymolysis enzyme used is serrapeptass, hydrolysis temperature 40 DEG C, and solution ph remains 7.5, enzymolysis time 2 hours, and enzyme dosage is 1 ‰ of compound Chinese herb powder weight.
After enzymolysis, adding 95% ethanol to extracting solution alcohol concn is 75% carry out second extraction and simultaneously deactivation, Extracting temperature 80 DEG C, 4 hours extraction times, extracts fully, crosses to filter filter residue final vacuum to be concentrated into solution degree Beaume be 25 ° of B é.
(2) extract concentrated solution for reactive agent with above-mentioned steps (1) gained, add aminoacids complex and carry out Maillard reaction: regulate pH value of reaction system to 8.0, temperature of reaction is 80 DEG C, react 6 hours under agitation condition; After sufficient reacting, filter after ultrasonic 15 minutes, after removing filter residue, obtain Maillard reaction liquid.Described aminoacids complex comprises leucine, Isoleucine, α-amino-isovaleric acid and phenylalanine, and compositely proportional is leucine 22 parts, Isoleucine 16 parts, α-amino-isovaleric acid 11 parts, phenylalanine 51 parts, gross weight 100 parts.Aminoacids complex add-on is extract concentrated solution quality 15%.
(3) Mei Lade product reaction solution above-mentioned steps (2) prepared first filters with molecular weight cut-off 1000dalton ultra-filtration membrane, working pressure: 0.2MPa, operating temperature: 35 DEG C; Ultra-filtration membrane filtrate again through molecular weight cut-off 400dalton nanofiltration membrane, working pressure: 2.0MPa, temperature: 50 DEG C; Gained filtrate is filtered through molecular weight cut-off 200dalton nanofiltration membrane again, working pressure: 1.0MPa, temperature: 50 DEG C, finally obtains by vacuum concentration the 400dalton nanofiltration membrane trapped substance solution M that degree Beaume is 30 ° of B é again
1, 200dalton nanofiltration membrane trapped substance solution M
2with 200dalton nanofiltration membrane filtrate concentrated solution M
3.Vacuum concentration temperature 45 C.
(4) the professional blending personnel of tissue are to the M of step 3 gained
1, M
2chinese-style cigarette sensory evaluation is carried out with M3, formula combination is carried out according to evaluation result and blending experience, again according to screening formulation by the spices allocated be sprayed on tobacco leaf according to Conventional feed introduction processing sequence, then in climatic chamber, balance 12 hours, then roll into cigarette evaluation.According to effect determination tobacco flavor components of the present invention, gross weight 100 parts: M
15 parts, M
265 parts, M
310 parts, propylene glycol 20 parts.
embodiment 3:
(1) first enzymolysis and second extraction are carried out to compound Chinese herb powder: after 60 grams of asparagus ferns, 20 grams of tubers of dwarf lilyturf, 20 grams of Poria cocos and 10 grams of Root of Pubescent Holly herbal powders (granularity < 100 order) are mixed and 800 grams of water add in extraction vessel, to be first placed under ultrasound environments soak at room temperature 15 minutes.Then carry out the first step enzymolysis, enzyme used is the prozyme of cellulase and polygalacturonase combination, and the weight ratio of cellulase and polygalacturonase is 10:1, hydrolysis temperature 53 DEG C, by citric acid regulating solution pH value to 4, enzymolysis time 3 hours, enzyme dosage is 1.5 ‰ of compound Chinese herb powder weight; Second step enzymolysis enzyme used is α-amylase, hydrolysis temperature 70 DEG C, and with salt of wormwood regulator solution pH value to 7.2, enzymolysis time 2 hours, enzyme dosage is 0.5 ‰ of compound Chinese herb powder weight; 3rd step enzymolysis enzyme used is serrapeptass, hydrolysis temperature 37 DEG C, and solution ph remains 7.2, enzymolysis time 1.5 hours, and enzyme dosage is 0.8 ‰ of compound Chinese herb powder weight.
After enzymolysis, adding 95% ethanol to extracting solution alcohol concn is 60% carry out second extraction and simultaneously deactivation, Extracting temperature 65 DEG C, 2 hours extraction times.Extract fully, cross and filter filter residue final vacuum to be concentrated into solution degree Beaume be 18 ° of B é.
(2) extract concentrated solution for reactive agent with above-mentioned steps (1) gained, add aminoacids complex and carry out Maillard reaction: regulate pH value of reaction system to 7.0, temperature of reaction is 70 DEG C, react 8 hours under agitation condition; After sufficient reacting, filter after ultrasonic 15 minutes, after removing filter residue, obtain Maillard reaction liquid.Described aminoacids complex comprises leucine, Isoleucine, α-amino-isovaleric acid and phenylalanine, and compositely proportional is leucine 24 parts, Isoleucine 17 parts, α-amino-isovaleric acid 3 parts, phenylalanine 56 parts, gross weight 100 parts.Aminoacids complex add-on is extract concentrated solution quality 15%.
(3) Mei Lade product reaction solution above-mentioned steps (2) prepared first filters with molecular weight cut-off 1000dalton ultra-filtration membrane, working pressure: 0.15MPa, operating temperature: 30 DEG C; Ultra-filtration membrane filtrate again through molecular weight cut-off 400dalton nanofiltration membrane, working pressure: 1.8MPa, temperature: 45 DEG C; Gained filtrate is filtered through molecular weight cut-off 200dalton nanofiltration membrane again, working pressure: 0.7MPa, temperature: 45 DEG C, finally obtains by vacuum concentration the 400dalton nanofiltration membrane trapped substance solution M that degree Beaume is 30 ° of B é again
1, 200dalton nanofiltration membrane trapped substance solution M
2with 200dalton nanofiltration membrane filtrate concentrated solution M
3.Vacuum concentration temperature 55 DEG C.
(4) the professional blending personnel of tissue are to the M of step 3 gained
1, M
2chinese-style cigarette sensory evaluation is carried out with M3, formula combination is carried out according to evaluation result and blending experience, again according to screening formulation by the spices allocated be sprayed on tobacco leaf according to Conventional feed introduction processing sequence, then in climatic chamber, balance 24 hours, then roll into cigarette evaluation.According to effect determination tobacco flavor components of the present invention, gross weight 100 parts: M
18 parts, M
245 parts, M
312 parts, propylene glycol 35 parts.
In above-described embodiment 1,2,3, preparation-obtained tobacco aromatics using adds in cigarette, can fall thorn, covers assorted gas, coordinates flue gas, alleviate throat's oral stimulation and improve oral cavity pleasant impression by flavouring.Details of smokeing panel test see the following form:
Note :+represent that this index is micro-to be improved, ++ represent this index and be improved, +++ represent this index and have clear improvement.As unchanged in then represented this index for space.
Claims (5)
1. a preparation method for tobacco aromatics using, is characterized in that carrying out according to the following steps:
(1) by weight part asparagus fern 40 ~ 60, the tuber of dwarf lilyturf 20 ~ 40, Poria cocos 10 ~ 25, Root of Pubescent Holly 5 ~ 10, total amount is after the herbal powder mixing of 100 parts, according to weight ratio powder: water=1:5 ~ 1:10 adds water, ultrasonic immersion 10 ~ 20 minutes at 25 DEG C;
(2) cellulase added and polygalacturonase prozyme carry out the first step enzymolysis, hydrolysis temperature 50 ~ 55 DEG C, enzymolysis pH value 3.5 ~ 4.5, reaction times 1-5 hour, and enzyme addition is 2 ‰ ~ 5 ‰ of herbal powder quality;
(3) add α-amylase and carry out second step enzymolysis, hydrolysis temperature 65 ~ 80 DEG C, enzymolysis pH value 7 ~ 7.5, reaction times 2-8 hour, enzyme addition is 0.5 ‰ ~ 2 ‰ of herbal powder quality;
(4) add serrapeptass and carry out the 3rd step enzymolysis, hydrolysis temperature 35-40 DEG C, enzymolysis pH value 7 ~ 7.5, reaction times 1-2 hour, enzyme addition is 0.5 ‰ ~ 1 ‰ of herbal powder quality;
(5) adding 95% ethanol to solution ethanol concentration is stir extraction 1 ~ 4 hour at 50% ~ 75%, 50 ~ 80 DEG C, and extract fully, filtering and concentrating to solution degree Beaume is 10 ° of B é ~ 25 ° B é;
(6) in step (5) concentrated solution, add amino acid and carry out Maillard reaction, add-on is 10% ~ 20% of concentrated solution quality; PH value of reaction system 6.5 ~ 8.0, temperature of reaction 60 ~ 80 DEG C, agitation condition lower seal reaction 6 ~ 10 hours, after sufficient reacting, filters after ultrasonic 15 minutes, obtains Maillard reaction liquid after removing filter residue;
(7) the Maillard reaction liquid that step (6) prepares is carried out membrane sepn, obtain tobacco flavor components unit, being finally concentrated into degree Beaume is that solution M1, M2 and M3 of 30 ° of B é are in order to composite;
Described membrane sepn comprises the following steps:
A, to be filtered by molecular weight cut-off 1000dalton ultra-filtration membrane, ultra-filtration membrane working pressure: 0.1-0.2MPa, operating temperature: 25 ~ 35 DEG C;
B, above-mentioned ultra-filtration membrane filtrate through molecular weight cut-off 400dalton nanofiltration membrane, working pressure: 1.5-2.0MPa, operating temperature: 40 ~ 50 DEG C;
C above-mentioned nanofiltration membrane gained filtrate again through molecular weight cut-off 200dalton nanofiltration membrane, working pressure: 0.5-1.0MPa, operating temperature: 40 ~ 50 DEG C;
D, above-mentioned 400dalton nanofiltration membrane trapped substance, 200dalton nanofiltration membrane trapped substance and 200dalton permeate are carried out vacuum concentration respectively, thickening temperature 45 ~ 55 DEG C, be finally concentrated into solution M1, M2 and M3 that degree Beaume is 30 ° of B é;
(8) by M1 5 ~ 9 parts, M2 45 ~ 65 parts, M3 10 ~ 20 parts, propylene glycol 20 ~ 35 parts, gross weight 100 parts is carried out composite, obtains tobacco aromatics using.
2. the preparation method of tobacco aromatics using according to claim 1, is characterized in that described asparagus fern, the tuber of dwarf lilyturf, Poria cocos, Root of Pubescent Holly herbal powder mixture granularity < 100 order.
3. the preparation method of tobacco aromatics using according to claim 1, is characterized in that the prozyme compositely proportional of cellulase and polygalacturonase described in step (2) is 10:1 ~ 6:1.
4. the preparation method of tobacco aromatics using according to claim 1, it is characterized in that step (6) described aminoacids complex comprises leucine, Isoleucine, α-amino-isovaleric acid and phenylalanine, compositely proportional is leucine 15 ~ 24 parts, Isoleucine 12 ~ 17 parts, α-amino-isovaleric acid 3 ~ 11 parts, phenylalanine 50 ~ 65 parts, gross weight 100 weight part.
5. the tobacco aromatics using prepared of the preparation method of a tobacco aromatics using as claimed in claim 1.
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Address after: 653100 Hongta Road, Yunnan, Yuxi, No. 118 Patentee after: Hongta Tobacco (Group) Co., Ltd. Patentee after: Yunnan Tianhong essence Co. Ltd. Address before: 653100 Hongta Road, Yunnan, Yuxi, No. 118 Patentee before: Hongta Tobacco (Group) Co., Ltd. Patentee before: Yunnan Tianhong Essence and Spice Co., Ltd. |