CN109171004A - A kind of compounding maple extract Maillard reaction fragrance, preparation method and the application in papermaking-method reconstituted tobaccos - Google Patents

A kind of compounding maple extract Maillard reaction fragrance, preparation method and the application in papermaking-method reconstituted tobaccos Download PDF

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CN109171004A
CN109171004A CN201810824840.8A CN201810824840A CN109171004A CN 109171004 A CN109171004 A CN 109171004A CN 201810824840 A CN201810824840 A CN 201810824840A CN 109171004 A CN109171004 A CN 109171004A
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maple extract
compounding
maillard reaction
maple
acid
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CN109171004B (en
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席高磊
陈芝飞
蔡莉莉
刘前进
楚文娟
冯颖杰
王鹏飞
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China Tobacco Henan Industrial Co Ltd
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China Tobacco Henan Industrial Co Ltd
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/14Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/26Use of organic solvents for extraction
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/0003Compounds of unspecified constitution defined by the chemical reaction for their preparation
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials

Abstract

The present invention relates to a kind of preparation methods for compounding maple extract Maillard reaction fragrance: 1) composition analysis result according to traditional maple extract, reject component pectin, cellulose, protein, tartaric acid, shikimic acid, 2 ethyl hexanoic acid, caproic acid, furfural, furfuryl alcohol, 2,3- dimethyl pyrazine, 2,5- dimethyl pyrazine, 2,6- dimethyl pyrazine, syringaldehyde and 2, after 6- syringol, as simulated formula;2) each raw material component is prepared by simulated formula, obtains compounding maple extract;3) it after compounding maple extract being diluted with water, is mixed with amino acid, and adjust pH to 8~10, then obtains Maillard reaction maple extract solution in atmosphere of inert gases high temperature reaction under high pressure;PH is adjusted to 5~7, after vacuum freeze drying to obtain the final product.The fragrance product quality is stablized, and is added in papermaking-method reconstituted tobaccos, has well solved the problems such as perfume quantity present in existing papermaking-method reconstituted tobaccos is less, fragrance is flat, xylon gas are heavy, the hot sense of flue gas is heavier.

Description

A kind of compounding maple extract Maillard reaction fragrance, preparation method and in paper process Application in reconstituted tobacco
Technical field
The invention belongs to tobacco addition fragrance technical fields, and in particular to a kind of compounding maple extract Maillard reaction is fragrant Material, preparation method and the application in papermaking-method reconstituted tobaccos.
Background technique
Currently, papermaking-method reconstituted tobaccos using very extensive, China's cigarette is using accounting up to 10% or so, and state is additional The pipe tobacco of the hot cigarette that do not burn is made by papermaking-method reconstituted tobaccos entirely.The utilization of papermaking-method reconstituted tobaccos avoids raw materials for production Waste, has saved manufacturing cost, has improved the quality of cigarette.But about half is all offal to papermaking-method reconstituted tobaccos raw material, due to Aroma substance contained by offal itself is few, and preparation process is produced using paper process, and flavor component loss is serious, leads to paper process again Make tobacco leaf there are perfume quantities the problems such as less, fragrance is flat, xylon gas are heavy, the hot sense of flue gas is heavier.Therefore, how to increase papermaking The fragrance content of method reconstituted tobacco reduces miscellaneous gas, optimization mouthfeel, always is that the technology of the highly desirable solution of tobacco enterprise is asked Topic.
Currently, improving papermaking-method reconstituted tobaccos aesthetic quality by addition foreign substance is an important technological means, Mostly use addition enzyme or with peat-reek, substance of sweet taste etc..Wherein, addition adventitious plant extract, which can use it, has Peat-reek, sweet taste cover the miscellaneous gas of papermaking-method reconstituted tobaccos raw material itself, increase fragrance and sweet sense, to reach preferable Suction quality.But plant extracts is influenced by factors such as plant growth environment temperature, moisture, soil, illumination, leads to not the same year The product quality fluctuation of part, batch and producer is big, stability is poor, to affect it to a certain extent in paper-making method reconstructed cigarette Application in leaf.Therefore, how to guarantee natural extract stable product quality, become the class of tobacco enterprise and food service industry concern Topic.
The present invention chooses traditional tobacco aromaticss maple extract as research object, with the separation point of maple extract key component Analysis result is reference, is compounded to maple extract, by macromolecular compound and and papermaking-method reconstituted tobaccos unfavorable in medicinal extract The perfume monomer of style and features conflict is rejected, and remaining perfume monomer and solvent are carried out mixed dissolution by different proportion, answered With maple extract (compounding maple extract stable components, do not influenced by external factor such as temperature, moisture, soil, illumination);Then Maillard reaction is occurred into amino acid in it, promotes the conversion of maple extract reducing sugar, a kind of and paper-making method reconstructed cigarette is made The novel maple extract that leaf is coordinated, maple extract glucide after reaction reduce, and aroma substance increases, fragrance is more abundant, Coordinate, can be preferably applied in papermaking-method reconstituted tobaccos, can play improvement and modification thin slice fragrance, increase it is sweet Feel, cover miscellaneous gas, reduce irritation, improve aroma quality and perfume quantity, coordinate cigarette perfume, increase sense organ comfort level, improve inhale taste and The effect of pleasant impression.
Summary of the invention
Present invention aims to overcome that prior art defect, provides a kind of compounding maple extract Maillard reaction fragrance, Analysis result is separated as reference, by macromolecular compound and and paper process unfavorable in medicinal extract using traditional maple extract key component Perfume monomer of reconstituted tobacco style and features conflict etc. is rejected, and is added amino acid and carried out Maillard reaction and obtain;The fragrance Stable product quality is added in papermaking-method reconstituted tobaccos, has well solved perfume present in existing papermaking-method reconstituted tobaccos The problems such as tolerance is less, fragrance is flat, xylon gas are heavy, the hot sense of flue gas is heavier, has important practical value.
The present invention also provides the preparation method of above-mentioned compounding maple extract Maillard reaction fragrance and its paper process again Make the application in tobacco leaf.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method compounding maple extract Maillard reaction fragrance, specifically includes the following steps:
1) composition analysis result according to traditional maple extract, rejects component pectin, cellulose, protein, tartaric acid, thick grass Acid, 2 ethyl hexanoic acid, caproic acid, furfural, furfuryl alcohol, 2,3- dimethyl pyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, fourth Fragrant aldehyde and 2, after 6- syringol, as simulated formula;
2) each raw material component is prepared by simulated formula, obtains compounding maple extract;Specifically, can by perfume monomer ethyl alcohol, Propylene glycol or water dissolution, then mix in proportion, then are diluted to traditional maple extract concentration and soak to get to compounding maple maple Cream;Wherein, carbohydrate and acids use water to dissolve as solvent, and vanillic aldehyde, fenugreck lactone are solvent dissolution, residual monomer with ethyl alcohol Raw material is solvent dissolution with propylene glycol;
Traditional maple extract is by glucose, fructose, sucrose, maltose, pectin, cellulose, protein, malic acid, fumaric acid, lemon Lemon acid, lactic acid, acetic acid, tartaric acid, shikimic acid, 2 ethyl hexanoic acid, caproic acid, proline, aspartic acid, vanillic aldehyde, dehydrogenation pine and cypress Alcohol, fenugreck lactone, 5 methyl furfural, furfural, maltol, formylpyrrole, benzyl carbinol, benzyl alcohol, furfuryl alcohol, 5- methylol dihydro Furans -2- ketone, methyl cyclopentenyl ketone, acetyl pyrrole, methylpyrazine, 2,3- dimethyl pyrazine, 2,5-dimethyl pyrazine, 2,6- Dimethyl pyrazine, ethyl pyrazine, 3-Hydroxybutanone, 3- hydroxyl -2- pyranone, 2- hydroxyl -2- cyclopentene-1-one, 3- hydroxyl fourth Ketone, 4- hydroxyl -2,5- dimethyl -3(2H) furanone (pineapple ketone), 2,3- dehydrogenation -3,5- dihydroxy -6- methyl (4H)-pyrans - The organic compounds such as 4- ketone (DDMP), 3- methyl 3- butene-2 -one, 2- ethyl-1- hexanol, syringaldehyde, 2,6- syringol Object composition;
Maple extract is compounded by glucose, fructose, sucrose, maltose, malic acid, fumaric acid, citric acid, lactic acid, acetic acid, chinese cymbidium Element, dehydrogenation coniferyl alcohol, fenugreck lactone, 5 methyl furfural, maltol, formylpyrrole, benzyl carbinol, benzyl alcohol, 5- methylol two Hydrogen furans -2- ketone, methyl cyclopentenyl ketone, acetyl pyrrole, methylpyrazine, ethyl pyrazine, 3-Hydroxybutanone, 3- hydroxyl -2- pyrrole Mutter ketone, 2- hydroxyl -2- cyclopentene-1-one, 3-Hydroxybutanone, 4- hydroxyl -2,5- dimethyl -3(2H) furanone (pineapple ketone), 2, 3- dehydrogenation-3,5- dihydroxy-6- methyl (4H)-pyrans-4- ketone (DDMP), 3- methyl 3- butene-2 -one, 2- ethyl-1- hexanol Composition.That is, eliminate macromolecular compound pectin, cellulose, protein in compounding maple extract, and with paper-making method reconstructed cigarette Perfume monomer tartaric acid, shikimic acid, 2 ethyl hexanoic acid, caproic acid, furfural, furfuryl alcohol, the 2,3- dimethyl pyrazole of leaf style and features conflict The substances such as piperazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, syringaldehyde and 2,6- syringol;
3) will compounding maple extract be diluted with water after, be added pressure autoclave type reactor in (additional amount be reactor volume 1/4~ 1/2) amino acid mixing, is added, pH to 8~10 is adjusted with lye, then in atmosphere of inert gases, in temperature 200~300 DEG C, 2~4 h are reacted under the conditions of 0.6~3.0 MPa of pressure, obtain Maillard reaction maple extract solution;
4) pH of Maillard reaction maple extract solution is adjusted to 5~7, then after vacuum freeze drying to obtain the final product.
Specifically, the additional amount of water is 1~5 times for compounding maple extract quality in step 3);The amino acid is dried meat ammonia One or more of acid, histidine, leucine and tryptophan, amino acid additive amount are compound maple extract quality 5% ~20%.PH value is adjusted to 8~10 using the sodium hydrate aqueous solution or potassium hydroxide aqueous solution of 1~5 mol/L of concentration.It selects Inert gas be nitrogen.
Specifically, adjusting pH to 5~7 using organic acid soln, the organic acid soln is that citric acid is water-soluble in step 4) One or more of liquid, aqueous solution of malic acid and aqueous tartaric acid solution.
Specifically, in step 4), cryogenic temperature is -200~-120 DEG C when vacuum freeze drying, vacuum pressure is 10~ 100Pa。
The present invention provides the compounding maple extract Maillard reaction fragrance being prepared using above-mentioned preparation method.
The present invention also provides application of the above-mentioned compounding maple extract Maillard reaction fragrance in papermaking-method reconstituted tobaccos, Specifically, compounding maple extract Maillard reaction fragrance broiler diets be papermaking-method reconstituted tobaccos weight 0.5 ‰~ 2.5‰。
In order to solve, traditional maple extract ingredient easily changes, stability is poor, different manufacturers difference is big, is unfavorable for making The problems such as paper method reconstituted tobacco is applied, the present invention provide a kind of preparation side of Maillard reaction fragrance based on compounding maple extract Method.Novel maple extract ingredient is fixed made from this method, performance is stable, contents of saccharide is low, flavor component is more, is applied to papermaking In method reconstituted tobacco, it is able to solve the problems such as papermaking-method reconstituted tobaccos perfume quantity is less, fragrance is flat, the hot sense of flue gas is heavier, It can improve and modify papermaking-method reconstituted tobaccos fragrance well, increase sweet sense, cover miscellaneous gas, reduce irritation, improve perfume Gas quality and quantity coordinates cigarette perfume, increases sense organ comfort level, improving and inhale taste and pleasant impression, is suitable for papermaking-method reconstituted tobaccos application.
Compared with prior art, remarkable advantage of the invention has:
1) present invention simulation compounding maple extract by macromolecular compound unfavorable in former maple extract and with paper-making method reconstructed cigarette The perfume monomer of leaf style and features conflict is directly rejected, and avoids outer perfuming bring insufficient;Meanwhile the maple extract of compounding It studies a point type and content to fix, not influenced by external factor such as temperature, moisture, soil, illumination, so that performance is stablized, no The variation of quality can be generated;
2) under high-temperature and high-pressure conditions, the Maillard reaction of carbohydrate and amino acid can be accelerated, carry out reaction more thorough;Inertia Gas shield, can prevent under the active perfume compound of maple extract and volatile perfume compound hot conditions oxidation deterioration and Volatilization reduces fragrance matter loss, improves maple extract product quality;
3) Maillard reaction is carried out under the maple extract and different aminoacids high-temperature and high-pressure conditions that the present invention compounds, generates aldehyde ketone The perfume compounds such as class, alcohols, acids, esters, heterocyclic increase flavor component type and content in maple extract, make maple The odor characteristic of maple medicinal extract is more abundant, coordinates.Existing for these perfume compound very good solutions papermaking-method reconstituted tobaccos The problems such as perfume quantity is less, fragrance is flat, the hot sense of flue gas is heavier, increases the flue gas concentration and fragrance of papermaking-method reconstituted tobaccos Amount, raising cigarette perfume is rich, improves pleasant impression, reduces miscellaneous gas and irritation, plays to papermaking-method reconstituted tobaccos organoleptic quality is improved Important role;
4) alkali used in the present invention is potassium hydroxide etc., and acid is citric acid etc., and potassium citrate etc. is generated after acid-base neutralization, is fine Combustion adjuvant, the flammability of papermaking-method reconstituted tobaccos can be improved, after so that papermaking-method reconstituted tobaccos is burnt cigarette ash is snow-white, tar Content reduces, and plays an important role to papermaking-method reconstituted tobaccos quality is improved.
The disadvantages of contents of saccharide that the present invention not only overcomes traditional maple extract is higher, fragrance component is on the low side, but also solve Its material quality when preparing Maillard reaction fragrance using natural products of having determined fluctuates the problems such as big, stability is poor, obtained new Type maple extract can be preferably suitable for cigarette industry and food service industry.Novel built maple extract beauty prepared by the present invention Maillard reaction fragrance can coordinate with flue gas of papermaking-method reconstituted tobaccos, improves and modify well thin slice fragrance, improve aroma quality With perfume quantity, increase sweet sense, improve flue gas concentration, cover miscellaneous gas, reduce irritation, coordinate cigarette perfume, increase sense organ comfort level, Improve and inhales taste and pleasant impression, meanwhile, also reduce the burnt bitter breath of traditional maple extract bring and sweet sense.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention It is not limited thereto.
In following embodiments, compounding maple extract used is obtained through following step:
1) by traditional maple extract, with Agilent7890A-5975C type makings chromatograph-mass spectrometer, (U.S.'s Agilent Technologies have Limit company), II type liquid chromatography mass combined instrument (Anjelen Sci. & Tech. Inc of the U.S.) of Agilent1290-micrOTOF Q Constituent analysis is carried out with 400 nuclear magnetic resonance chemical analysers (VARIAN Oncology Systems), obtains the content analysis result of key component;
Wherein, the preparation method of traditional maple extract are as follows: evaporating dish is added in maple maple juice, and (maple maple juice additional amount is to steam Send out the 1/3~1/2 of ware volume) in, under 200~300 DEG C of high temperature heating conditions, reaction concentration obtains maple maple (to remove moisture) Syrup uses propylene glycol dissolved dilution up to (propylene glycol additional amount is the 1.5~3.5 of maple maple syrup quality) after cooling.The present invention In, maple maple juice is obtained using this field routine techniques, e.g., the trunk of mature maple maple can be scratched with knife or in trunk The juice oozed out at cut, as maple maple juice are collected in upper drilling;
2) composition analysis result according to traditional maple extract, rejects component pectin, cellulose, protein, tartaric acid, thick grass Acid, 2 ethyl hexanoic acid, caproic acid, furfural, furfuryl alcohol, 2,3- dimethyl pyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, fourth Fragrant aldehyde and 2, after 6- syringol, as simulated formula;
Traditional maple extract is by glucose, fructose, sucrose, maltose, pectin, cellulose, protein, malic acid, fumaric acid, lemon Lemon acid, lactic acid, acetic acid, tartaric acid, shikimic acid, 2 ethyl hexanoic acid, caproic acid, proline, aspartic acid, vanillic aldehyde, dehydrogenation pine and cypress Alcohol, fenugreck lactone, 5 methyl furfural, furfural, maltol, formylpyrrole, benzyl carbinol, benzyl alcohol, furfuryl alcohol, 5- methylol dihydro Furans -2- ketone, methyl cyclopentenyl ketone, acetyl pyrrole, methylpyrazine, 2,3- dimethyl pyrazine, 2,5-dimethyl pyrazine, 2,6- Dimethyl pyrazine, ethyl pyrazine, 3-Hydroxybutanone, 3- hydroxyl -2- pyranone, 2- hydroxyl -2- cyclopentene-1-one, 3- hydroxyl fourth Ketone, 4- hydroxyl -2,5- dimethyl -3(2H) furanone (pineapple ketone), 2,3- dehydrogenation -3,5- dihydroxy -6- methyl (4H)-pyrans - The organic compounds such as 4- ketone (DDMP), 3- methyl 3- butene-2 -one, 2- ethyl-1- hexanol, syringaldehyde, 2,6- syringol Object composition;
Maple extract is compounded by glucose, fructose, sucrose, maltose, malic acid, fumaric acid, citric acid, lactic acid, acetic acid, chinese cymbidium Element, dehydrogenation coniferyl alcohol, fenugreck lactone, 5 methyl furfural, maltol, formylpyrrole, benzyl carbinol, benzyl alcohol, 5- methylol two Hydrogen furans -2- ketone, methyl cyclopentenyl ketone, acetyl pyrrole, methylpyrazine, ethyl pyrazine, 3-Hydroxybutanone, 3- hydroxyl -2- pyrrole Mutter ketone, 2- hydroxyl -2- cyclopentene-1-one, 3-Hydroxybutanone, 4- hydroxyl -2,5- dimethyl -3(2H) furanone (pineapple ketone), 2, 3- dehydrogenation-3,5- dihydroxy-6- methyl (4H)-pyrans-4- ketone (DDMP), 3- methyl 3- butene-2 -one, 2- ethyl-1- hexanol Composition.That is, eliminate macromolecular compound pectin, cellulose, protein in compounding maple extract, and with paper-making method reconstructed cigarette Perfume monomer tartaric acid, shikimic acid, 2 ethyl hexanoic acid, caproic acid, furfural, furfuryl alcohol, the 2,3- dimethyl pyrazole of leaf style and features conflict The substances such as piperazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, syringaldehyde and 2,6- syringol;
The specific ingredient and proportion grading of traditional maple extract and compounding maple extract the results are shown in Table 1.
3) each raw material component is prepared by simulated formula, obtains compounding maple extract;
Specifically, perfume monomer ethyl alcohol, propylene glycol or water can be dissolved, then mix in proportion, then be diluted to biography Unite maple extract concentration to get to compounding maple extract;Wherein, carbohydrate and acids use water to dissolve as solvent, vanillic aldehyde, cucurbit Bar lactone is solvent dissolution with ethyl alcohol, and residual monomer raw material is that solvent dissolves with propylene glycol.
Embodiment 1
A kind of preparation method compounding maple extract Maillard reaction fragrance, specifically includes the following steps:
1) in 500 mL pressure autoclave type reactors, it is mixed that 75 g compounding maple extract, 75 g water and 4 g proline, stirring is added After closing uniformly, adjusting pH with 2 mol/L sodium hydrate aqueous solutions is 8, seals, air inlet and venthole is opened, by air inlet Hole is filled with nitrogen, and inner air is discharged by venthole, is then shut off venthole, is filled with nitrogen again.Adjust pressure autoclave type reaction Device temperature is 200 DEG C, and pressure is 1.0 MPa, reacts 4 h.It is cooled to room temperature after reaction, obtains the leaching of Maillard reaction maple maple Cream solution;
2) aqueous citric acid solution of 2 mol/L is added dropwise in Maillard reaction maple extract solution, adjusts pH to 5.It is then placed in In freeze dryer, refrigeration valve is opened, reducing temperature extremely makes freezing solution for -200 DEG C, is then turned on vacuum pump, vacuum pressure 80 Pa reduces pressure and distils, obtains 26.87 g solids after removing solvent;With propylene glycol dissolved dilution up to compounding after crushing Maple extract Maillard reaction fragrance, color are brown color.
Embodiment 2
A kind of preparation method compounding maple extract Maillard reaction fragrance, specifically includes the following steps:
1) in 500 mL pressure autoclave type reactors, 90 g compounding maple extract, 90 g water and 4.5 g histidines, stirring is added After mixing, adjusting pH with 3 mol/L potassium hydroxide aqueous solutions is 9, seals, opens air inlet and venthole, by into Stomata is filled with nitrogen, and inner air is discharged by venthole, is then shut off venthole, is filled with nitrogen again.It is anti-to adjust pressure autoclave type Answering device temperature is 230 DEG C, and pressure is 1.5 MPa, reacts 3 h.It is cooled to room temperature after reaction, obtains Maillard reaction maple maple Medicinal extract solution;
2) aqueous solution of malic acid of 4 mol/L is added dropwise in Maillard reaction maple extract solution, adjusts pH to 6.It is then placed in In freeze dryer, refrigeration valve is opened, reducing temperature extremely makes freezing solution for -180 DEG C, is then turned on vacuum pump, vacuum pressure 60 Pa reduces pressure and distils, obtains 31.24 g solids after removing solvent;With propylene glycol dissolved dilution up to compounding after crushing Maple extract Maillard reaction fragrance, color are brown color.
Embodiment 3
A kind of preparation method compounding maple extract Maillard reaction fragrance, specifically includes the following steps:
1) in 500 mL pressure autoclave type reactors, 110 g compounding maple extract, 110 g water and 5 g leucines, stirring is added After mixing, adjusting pH with 4 mol/L sodium hydrate aqueous solutions is 10, seals, opens air inlet and venthole, by into Stomata is filled with nitrogen, and inner air is discharged by venthole, closes venthole later, is filled with nitrogen again.It is anti-to adjust pressure autoclave type Answering device temperature is 260 DEG C, and pressure is 2.0 MPa, reacts 2 h.It is cooled to room temperature after reaction, obtains Maillard reaction maple maple Medicinal extract solution;
2) aqueous tartaric acid solution of 6 mol/L is added dropwise in Maillard reaction maple extract solution, adjusts pH to 7.It is then placed in In freeze dryer, refrigeration valve is opened, reducing temperature extremely makes freezing solution for -160 DEG C, is then turned on vacuum pump, vacuum pressure 40 Pa reduces pressure and distils, obtains 37.59 g solids after removing solvent;With propylene glycol dissolved dilution up to compounding after crushing Maple extract Maillard reaction fragrance, color are brown color.
Embodiment 4
A kind of preparation method compounding maple extract Maillard reaction fragrance, specifically includes the following steps:
1) in 500 mL pressure autoclave type reactors, 125 g compounding maple extract, 125 g water and 6 g leucines, stirring is added After mixing, adjusting pH with 5 mol/L potassium hydroxide aqueous solutions is 9, seals, opens air inlet and venthole, by into Stomata is filled with nitrogen, and inner air is discharged by venthole, closes venthole later, is filled with nitrogen again.It is anti-to adjust pressure autoclave type Answering device temperature is 300 DEG C, and pressure is 2.5 MPa, reacts 2 h.It is cooled to room temperature after reaction, obtains Maillard reaction maple maple Medicinal extract solution;
2) aqueous citric acid solution of 8 mol/L is added dropwise in Maillard reaction maple extract solution, adjusts pH to 6.It is then placed in In freeze dryer, refrigeration valve is opened, reducing temperature extremely makes freezing solution for -140 DEG C, is then turned on vacuum pump, vacuum pressure 20 Pa reduces pressure and distils, obtains 42.34 g solids after removing solvent;With propylene glycol dissolved dilution up to compounding after crushing Maple extract Maillard reaction fragrance, color are brown color.
Embodiment 5
A kind of preparation method compounding maple extract Maillard reaction fragrance, specifically includes the following steps:
1) in 500 mL pressure autoclave type reactors, 100 g is added and compound maple extract, 100 g water, 1.5 g proline, 1.5 G histidine, 1.5 g leucines and 1.5 g tryptophans after being uniformly mixed, are adjusted with 4 mol/L potassium hydroxide aqueous solutions PH is 9, is sealed, and opens air inlet and venthole, is filled with nitrogen by air inlet, inner air is discharged by venthole, later Venthole is closed, is filled with nitrogen again.Adjusting pressure autoclave type temperature of reactor is 300 DEG C, and pressure is 2.5 MPa, reacts 2 h. It is cooled to room temperature after reaction, obtains Maillard reaction maple extract solution;
2) aqueous citric acid solution of 8 mol/L is added dropwise in Maillard reaction maple extract solution, adjusts pH to 6.It is then placed in In freeze dryer, refrigeration valve is opened, reducing temperature extremely makes freezing solution for -180 DEG C, is then turned on vacuum pump, vacuum pressure 20 Pa reduces pressure and distils, obtains 38.95 g solids after removing solvent;With propylene glycol dissolved dilution up to compounding after crushing Maple extract Maillard reaction fragrance, color are brown color.
Compounding maple extract Maillard reaction fragrance Agilent7890A-5975C type makings connection prepared by embodiment 5 Analyzed with instrument (Anjelen Sci. & Tech. Inc of the U.S.) and 400 nuclear magnetic resonance chemical analysers (VARIAN Oncology Systems), find its at Subpackage contains glucose, fructose, sucrose, maltose, malic acid, fumaric acid, citric acid, acetic acid, n-nonanoic acid, tartaric acid, vanillic aldehyde, takes off Hydrogen coniferyl alcohol, fenugreck lactone, 5 methyl furfural, maltol, benzyl carbinol, benzyl alcohol, 5- methylol dihydrofuran -2- ketone, first Cyclopentene alcohol ketone, pyridine, 3- picoline, 1- methyl -2- N-ethyl pyrrole N, 1- ethyl -2- acetyl pyrrole, piperidines, furfuryl group Mercaptan, 2- methylpyrazine, 2- ethyl pyrazine, furfuryl mercaptan, formylpyrrole, acetyl pyrrole, methylpyrazine, 2,3- dimethyl pyrazole Piperazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, ethyl pyrazine, trimethylpyrazine, 6- methyl -2- ethyl pyrazine, 2,5- bis- Methyl -3,6- diisobutyl pyrazine, 5- isobutyryl -2,3- dimethyl pyrazine, 3-Hydroxybutanone, 3- hydroxyl -2- pyranone, 2- Hydroxyl -2- cyclopentene-1-one, two furanone of 3- methyl -2,5-, 3-Hydroxybutanone, 3- hydroxyl -2- pyranone, 3- methyl -2,5- Two furanones, 4- hydroxyl -2,5- dimethyl -3(2H) furanone (pineapple ketone), 2,3- dehydrogenation -3,5- dihydroxy -6- methyl (4H)-pyrans-4- ketone (DDMP), 3- methyl 3- butene-2 -one, 2- ethyl-1- hexanol 2- methyl-2,5- cyclohexadiene-1,4- The organic compounds such as diketone, 2- cyclopentenol, acetosyringone.Compared with traditional maple extract and compounding maple extract, this hair Bright novel built maple extract Maillard reaction fragrance obtained without the pectin unfavorable to papermaking-method reconstituted tobaccos, cellulose and The macromolecular compounds such as protein, and the perfume compound to conflict with papermaking-method reconstituted tobaccos style and features;And increase n-nonanoic acid, Pyridine, 3- picoline, 1- methyl -2- N-ethyl pyrrole N, 1- ethyl -2- acetyl pyrrole, piperidines, furfuryl mercaptan, 2- methyl pyrrole Piperazine, 2- ethyl pyrazine, furfuryl mercaptan, trimethylpyrazine, 6- methyl -2- ethyl pyrazine, 2,5- dimethyl -3,6- diisobutyl pyrrole Piperazine, 5- isobutyryl -2,3- dimethyl pyrazine, two furanone of 3- methyl -2,5-, 3- hydroxyl -2- pyranone, 3- methyl -2,5- The perfume compounds such as two furanones, 2- methyl -2,5- cyclohexadiene -1,4- diketone, 2- cyclopentenol and acetosyringone.These Newly-generated perfume compound can increase flue gas of papermaking-method reconstituted tobaccos concentration and perfume quantity, and raising cigarette perfume is rich, more than improvement Taste reduces miscellaneous gas and irritation, plays an important role to tobacco papermaking-method reconstituted tobaccos organoleptic quality is improved.
By novel built maple extract Maillard reaction made from traditional maple extract, compounding maple extract and embodiment 5 Fragrance quantitative component analysis result category is listed in table 1.
The content of perfume compound in 1 three kinds of table different maple extracts
By table 1 it can be seen that traditional maple extract contents of saccharide is very high, total content 32.44%;Compound maple extract Contents of saccharide reduces, and is 29.85%;And novel built maple extract Maillard reaction fragrance contents of saccharide made from embodiment 5 is only It is 22.82%, compared with traditional maple extract and compounding maple extract, contents of saccharide is substantially reduced.In addition, made from embodiment 5 Aldoketones, alcohols, phenols, acids, esters and heterocycle compound content in novel built maple extract Maillard reaction fragrance It greatly increases.Due to the reduction of sugared content and dramatically increasing for perfume compound content, keep its note more abundant, aroma strength It is higher, there is better application effect, be suitable for being applied in papermaking-method reconstituted tobaccos.
Application test as tobacco aromaticss in papermaking-method reconstituted tobaccos
The novel built maple extract Maillard reaction fragrance for weighing the preparation of embodiment 5, with ethyl alcohol and distilled water (volume ratio 1:4) Be diluted to 5%(mass percent) solution, it is spare.The not spiced Bright Yellow papermaking-method reconstituted tobaccos of 100 g are weighed respectively Silk, it is evenly laid out in clean pallet, the spice solution prepared is uniformly sprayed on papermaking-method reconstituted tobaccos silk, maple is compounded Maple medicinal extract Maillard reaction fragrance papermaking-method reconstituted tobaccos silk specific gravity be respectively 0,0.10 ‰, 0.50 ‰, 1.00 ‰, 1.50 ‰, 2.00 ‰, 2.50 ‰, 3.00 ‰, 2 h are placed in sealing;Be subsequently placed into the drying of 100 DEG C of baking ovens, with distilled water humidify to Standard moisture (12.5%), rolls into standard cigarette, and equilibrium water conten (humidity 60% ± 2%, 25 ± 1 DEG C of temperature) 48 h smoke panel test.It is right It is in the same old way the Bright Yellow blank papermaking-method reconstituted tobaccos silk of addition same amount tradition maple extract, control sample is equally in phase equality of temperature 48 h are balanced under degree, damp condition.Sensory evaluating smoking the results are shown in Table 2.
2 sensory evaluating smoking's result of table
By the smoking result of table 2 it can be seen that compared with traditional maple extract, it is anti-that the present invention compounds maple extract Mei Lade It answers fragrance note more abundant, not only bakes fragrant and sweet breath, also add baking fragrance breath, preferably can improve and modify Papermaking-method reconstituted tobaccos fragrance increases fragrant baking, the miscellaneous gas of cover, reduces cigarette irritation, improves aroma quality and perfume quantity, improvement Inhale taste and pleasant impression.When compounding maple extract Maillard reaction fragrance dosage is smaller, to the effect in papermaking-method reconstituted tobaccos It is not apparent;When its additive amount is more than 2.50 ‰, there is phenomena such as baking perfume is overweight, sweet sense is excessively high and withered and burnt smell;When Sucking quality is best when its additive amount is 2.00 ‰.Therefore, the 0.20g present invention is added in papermaking-method reconstituted tobaccos silk in 100g Effect is best when compounding maple extract Maillard reaction fragrance, i.e., optimum dosage is 2.00 ‰.Therefore, the present invention compounds maple maple The Optimum of medicinal extract Maillard reaction fragrance is 0.50~2.50 ‰.

Claims (7)

1. a kind of preparation method for compounding maple extract Maillard reaction fragrance, which comprises the following steps:
1) composition analysis result according to traditional maple extract, rejects component pectin, cellulose, protein, tartaric acid, thick grass Acid, 2 ethyl hexanoic acid, caproic acid, furfural, furfuryl alcohol, 2,3- dimethyl pyrazine, 2,5-dimethyl pyrazine, 2,6 dimethyl pyrazine, fourth Fragrant aldehyde and 2, after 6- syringol, as simulated formula;
2) each raw material component is prepared by simulated formula, obtains compounding maple extract;
3) it after compounding maple extract being diluted with water, is mixed with amino acid, and adjust pH to 8~10, then in inert gas atmosphere In enclosing, 2~4 h are reacted under the conditions of 200~300 DEG C of temperature, 0.6~3.0 MPa of pressure, obtain Maillard reaction maple extract Solution;
4) pH of Maillard reaction maple extract solution is adjusted to 5~7, then after vacuum freeze drying to obtain the final product.
2. the preparation method of compounding maple extract Maillard reaction fragrance as described in claim 1, which is characterized in that step 3) In, the additional amount of water is 1~5 times for compounding maple extract quality;The amino acid is proline, histidine, leucine and color One or more of propylhomoserin, amino acid additive amount are compound maple extract quality 5%~20%.
3. the preparation method of compounding maple extract Maillard reaction fragrance as claimed in claim 2, which is characterized in that step 4) In, pH to 5~7 is adjusted using organic acid soln, the organic acid soln is aqueous citric acid solution, aqueous solution of malic acid and winestone One or more of aqueous acid.
4. the preparation method of compounding maple extract Maillard reaction fragrance as claimed in claim 2, which is characterized in that step 4) In, cryogenic temperature is -200~-120 DEG C when vacuum freeze drying, and vacuum pressure is 10~100Pa.
5. the compounding maple extract Maillard reaction fragrance being prepared using any preparation method of Claims 1-4.
6. application of the compounding maple extract Maillard reaction fragrance in papermaking-method reconstituted tobaccos described in claim 5.
7. application of the compounding maple extract Maillard reaction fragrance in papermaking-method reconstituted tobaccos as claimed in claim 6, special Sign is that the additive amount of compounding maple extract Maillard reaction fragrance is 0.5 ‰~the 2.5 ‰ of papermaking-method reconstituted tobaccos weight.
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