CN101445766A - Preparation method of cacao flavor, products obtained thereby and usage thereof - Google Patents
Preparation method of cacao flavor, products obtained thereby and usage thereof Download PDFInfo
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- CN101445766A CN101445766A CNA200810204737XA CN200810204737A CN101445766A CN 101445766 A CN101445766 A CN 101445766A CN A200810204737X A CNA200810204737X A CN A200810204737XA CN 200810204737 A CN200810204737 A CN 200810204737A CN 101445766 A CN101445766 A CN 101445766A
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- cacao
- water
- enzymolysis
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Links
- 244000299461 Theobroma cacao Species 0.000 title claims abstract description 105
- 239000000796 flavoring agent Substances 0.000 title claims abstract description 49
- 235000019634 flavors Nutrition 0.000 title claims abstract description 49
- 235000005764 Theobroma cacao ssp. cacao Nutrition 0.000 title claims abstract description 42
- 235000005767 Theobroma cacao ssp. sphaerocarpum Nutrition 0.000 title claims abstract description 42
- 235000001046 cacaotero Nutrition 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- 235000009470 Theobroma cacao Nutrition 0.000 claims description 63
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- 239000007787 solid Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 239000000047 product Substances 0.000 claims description 29
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- 239000002253 acid Substances 0.000 description 2
- WQZGKKKJIJFFOK-FPRJBGLDSA-N beta-D-galactose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-FPRJBGLDSA-N 0.000 description 2
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- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
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Abstract
The invention relates to the field of flavor preparation, in particular to a method for preparing cacao flavor, comprising the steps: composite liberation, zymohydrolysis, concentration, and the like, are carried on the cacao powder which is a raw material. The invention also relates to the cacao flavor prepared by the way and the usage of the flavor which is taken as cigarette additive. The preparation method can degrade giant molecule substances, such as starch, protein, pectine and the like, in cacao, improving the quality of the cacao flavor while maintaining the aroma of the cacao.
Description
[technical field]
The present invention relates to spices and preparation method thereof, be specifically related to the preparation method of cacao flavor and adopt the resulting cacao flavor of this method, with and in cigarette as the purposes of spice additive.
[background technology]
Cocoa powder is a kind of tobacco aromatics using commonly used in cigarette products, and it has unique cocoa aroma of strong fragrance, has cocoa inherent characteristic odor, has the rhythm of the fragrant end of beans like vanilla, can strengthen the characteristic cigarette flavor of cigarette product.Cocoa powder after treatment can close with tobacco is humorous because of its fragrance local flavor, therefore is usually used in tobacco product, plays and improves the effect that tobacco inhales flavor.In blended type cigarette, often cocoa powder is directly added in the sugared feed liquid.In tobacco aromatics using, general powder tincture or the shell tincture that adopts through alcohol extraction generally contains cocoa ester 12%, and its consumption can be decided according to the quality of tobacco of cigarette.Wherein, consumption is big slightly in the hybrid cigarette, and consumption is less in the fire-cured tobacco type cigarette.
Yet, contain macromolecular substance such as amount of starch, protein and pectin in the cocoa powder, produce a kind of offending smell behind these substance combustions, therefore the suction flavor to tobacco leaf plays negative impact, and influences the aroma quality of cigarette product.The existence of these materials simultaneously also can influence the solubility property of cacao flavor in ethanol, propylene glycol and glycerine.Therefore, how the starch in the efficient degradation cocoa powder is the problem of always constantly researching and solving at present.
For example Chinese patent application CN 99120366.6 discloses a kind of method that reclaims aroma/food essence, comprise that cooling comprises water and organic acid contains fragrance gas with condensation portion water and all basically organic acids, from gas, remove water of condensation and organic acid and be substantially free of containing fragrance gas and reclaim and containing fragrance gas of organic acid as aroma/food essence with generation.Yet the product that this method obtains only as foodstuff additive, does not relate to other application.
Chinese patent application CN 200580008335.7 discloses a kind of method that obtains cocoa polyphenol concentrate, comprises a) making not fermented beans process bleaching, to produce the not fermented beans that polyphenol oxidase activity reduces; B) drying is not more than not fermented beans of 15% exsiccant to obtain moisture content; C) make not fermented beans process particle size reduction step of exsiccant, to obtain not fermented beans intermediate product of exsiccant; E) extract the solid that polyphenol obtains the cocoa polyphenols extract and was extracted from middle product; D) concentrate the cocoa polyphenols extract to produce cocoa polyphenol concentrate.But aforesaid method does not all relate to the means of the starch in the degraded cocoa powder, and therefore resulting product can not be used as tobacco additive agent.
[summary of the invention]
[technical problem that will solve]
The preparation method who the purpose of this invention is to provide a kind of cacao flavor.
Another object of the present invention provides cacao flavor.
Another object of the present invention provides the purposes of cacao flavor
[technical scheme]
Adopt method of the present invention can access a kind of cacao flavor,,, improve cigarette quality so described cacao flavor can add in the tobacco because this method can be removed macromolecular substance such as the starch that contains in the cocoa powder, protein, pectin.
In order to address the above problem, the invention provides a kind of preparation method of cacao flavor, this method comprises the steps:
(1) mixes, separates
Cocoa powder and 70-85% ethanol aqueous solution are mixed with mass ratio 1:2-1:3, and at temperature 70-90 ℃, stirring velocity 300-500 rev/min following condensing reflux 1-2 hour, cooling is filtered and is obtained filtrate and filter cake;
(2) enzymolysis
In the filter cake that step (1) obtains, add water and obtain mixture, the mass ratio of cocoa powder is 5-7:1 in water that adds and the step (1), under 85-95 ℃, stir then, heating, the part alcohol that evaporation wherein exists, ethanol content in mixture is lower than 10%, then, add water again with institute's evaporating solns equal volume, add Ye Huamei down at 75-80 ℃ and carried out enzymolysis 1-3 hour, after enzymolysis was finished, adding saccharifying enzyme and polygalacturonase carried out enzymolysis 3-5 hour under 45-55 ℃ again, after enzymolysis is finished, at 90-100 ℃ of following 5-20 minute enzyme that goes out of heating, cool off centrifugally then, separate obtaining supernatant liquor and solid;
(3) concentrate
The solid that obtains in the step (2) is placed reactor, add concentrated hydrochloric acid and water, obtain the mixture that concentration of hydrochloric acid is 3-6mol/L, the mass ratio of cocoa powder dry mass and this hydrochloric acid soln is 1:4-7,100-110 ℃ of following heated and stirred, and condensing reflux 5-8 hour, cold filtration then, obtain filtrate and filter residue, filtrate concentrates, and obtains flowing shape thing solid; The supernatant liquor that stream shape thing solid and step (2) obtain concentrates after merging again, obtains brown stream shape thing solid;
(4) make product
The brown stream shape thing solid that filtrate that step (1) is obtained and step (3) obtain mixes and obtains described cacao flavor.
A kind of preferred embodiment according to the present invention, this method comprise that also the cacao flavor that will obtain in step (4) carries out reconcentration, is lower than 5% until the products therefrom water content.
A kind of embodiment according to the present invention, wherein the pH value of the mixture of filter cake and water is 5-7 in the step (2), stir speed (S.S.) is 150-300 rev/min.
According to the present invention, preferably described cocoa powder is selected from natural low fat cocoa powder or amount of cocoa butter content is lower than 10% natural cocoa powder.These cocoa powders can be bought acquisition on market.
A kind of preferred embodiment according to the present invention, concentrate in the vacuum concentration instrument in 45～65 ℃ of temperature and vacuum tightness be-0.09～-carry out under the 0.1MPa.
In the present invention, warm amylase during described Ye Huamei can be selected for use is for example by warm amylase in the liquid of the outstanding 3000U/ml that can zymin company of section provides in Wuxi.
In the present invention, described saccharifying enzyme can be selected barley beta-amylase for use, for example by the liquid barley beta-amylase of the outstanding 20000U/ml that can zymin company of section provides in Wuxi.
In the present invention, described polygalacturonase for example is provided for use by the liquid polygalacturonase of the 30000U/ml that is provided by the grand mcroorganism Engineering Co., Ltd in Shandong.
The present invention also provides the cacao flavor that obtains according to above-mentioned preparation method.
The invention still further relates to the cacao flavor that obtains according to above-mentioned preparation method purposes as additive in cigarette.
To at length be described the present invention below.
The present invention relates to natural low fat cocoa powder, particularly being lower than 10% natural cocoa powder with amount of cocoa butter content is the method that raw material extracts cacao flavor.
The product of cocoa tree.Cocoa contains oleic acid, linolic acid, stearic acid, Palmiticacid, protein, vitamin A, vitamins B
1, B
3, B
5, B
6, vitamins D, E, mineral calcium, magnesium, copper, potassium, sodium, iron, zinc, Mierocrystalline cellulose, polyphenol, comprise oligomer flavonoid material, wherein mainly contain Flavonol oligomer-pycnogenols and catechin, and the polymer tannin, phenylethylamine, Theobromine etc. contained.In addition, cocoa contains more than 500 kind of aromatoising substance, and the cocoa fusing point is 35-37 ℃, has to make us the taste of enjoying endless aftertastes.
Get cocoa powder and be broken into the 200-400 order, or the cocoa powder of selling on the purchase market, carry out step (1), cocoa powder mixes with mass ratio 1:2-1:3 with the 70-85% ethanol aqueous solution, at temperature 70-90 ℃, stirring velocity 300-500 rev/min following condensing reflux 1-2 hour, cooling is filtered and is obtained filtrate and filter cake.
Carry out step (2) then, obtaining in above-mentioned steps added water and obtained mixture in the filter cake, the amount of adding water is 5-7 a times of cocoa powder quality in the step (1), stir down at 85-95 ℃ then, mixture comes to life, the part alcohol that evaporation wherein exists, up to the ethanol content of mixture enough low can obviously not influence enzyme work the time, in general, ethanol concn is lower than 10%.Then, add water again with the solution equal volume of described evaporation, adding Ye Huamei down at 75-80 ℃ carried out enzymolysis 1-3 hour, after enzymolysis is finished, add saccharifying enzyme and polygalacturonase down at 45-55 ℃ again and carried out enzymolysis 3-5 hour, after enzymolysis is finished, heat the 5-20 minute enzyme that goes out down at 90-100 ℃, cool off centrifugally then, separate to obtain supernatant liquor and solid, supernatant liquor is waited to concentrate.
Carry out step (3) again, the solid that obtains in the step (2) is placed reactor, add concentrated hydrochloric acid and water, obtain the mixture that concentration of hydrochloric acid is 3-6mol/L, the mass ratio of this hydrochloric acid soln and cocoa powder is 1:4-7,100-110 ℃ of following heated and stirred, condensing reflux 5-8 hour, cold filtration obtained filtrate and filter residue then, filtrate concentrates, and obtains flowing shape thing solid; Supernatant liquor in stream shape thing solid and the step (2) merges and then concentrates, and obtains brown stream shape thing solid;
Then, the brown stream shape thing solid mixing and stirring that obtains of filtrate that step (1) is obtained and step (3) obtains described cacao flavor.
In the present invention, stir employed equipment and be normally used equipment when stirring in the art, it should satisfy following condition: voltage rating is 220V, the agitator of stir speed (S.S.) 0-500rpm.Therefore, for example be the S-312 digital display thermostatic mixer of Shensheng Science ﹠ Tech. Co., Ltd., Shanghai's sale, the HS-50A digital display agitator that R-S type speed regulator is sold or Shanghai 1,001 chemical industry company limiteds sell that sell along bio tech ltd the Shen, Shanghai.
In the present invention, heat employed equipment and be normally used equipment when heating in the art, it should satisfy following condition: the water-bath controllable temperature is 0～100 ℃, and oil bath or heating jacket controllable temperature are 0～200 ℃, and specification is 2000ml.Therefore, for example be that the super Water Tank with Temp.-controlled of DKB-501A type of going up the sale of the grand experimental installation of Nereid company limited, the DRT-TW type that Great Wall, Zhengzhou industry and trade company limited sells are separated the TC-15 shell type thermostatted of hot jacket or the sale of medical treatment factory of Haining City Xinhua.
The enzymolysis reactor that uses in implementation process of the present invention, should satisfy following condition: controllable temperature 0-100 ℃, adj sp 0-500rpm can survey pH value 0-14.Therefore, for example be the HKG-II rotary type constant temperature speed regulator that sell along the glad stamen automatic equipment of super Water Tank with Temp.-controlled of DKB-501A type or the Shanghai company limited of the R-S type speed regulator of bio tech ltd sale, the upward grand experimental installation of Nereid company limited sale the Shen, Shanghai.
The centrifugation apparatus that uses in implementation process of the present invention should satisfy following condition: the constant temperature freezing function is arranged, and centrifugation rate is not less than 3000rpm and capacity is big.Therefore, for example be the LXJ-IIB low speed large vol multitube whizzer of company limited of Anting Scientific Instrument Factory, Shanghai sale or the TD5M low speed large capacity centrifuge that Shanghai Lu Xiang instrument whizzer instrument company limited sells.
In implementation process of the present invention, carry out spissated equipment and should satisfy following condition: vacuum tightness-0.09～-0.1MPa, temperature is controlled to be room temperature-90 ℃, 20～200 rev/mins of Rotary Evaporators speed of rotation.Therefore, for example be that the RE-3000 Rotary Evaporators that the anticorrosion desk-top recirculated water vacuum pump of SHZ-D (III) type that magnificent Instr Ltd. sells or the large photoelectron in Shanghai Science and Technology Ltd. sell is given in RE-52AA type Rotary Evaporators, Shanghai that Shanghai refined flourish biochemical instrument equipment company limited sells.
In the present invention, used water can be distilled water, deionized water or pure water.
In enzyme digestion reaction of the present invention, described Ye Huamei can be selected warm amylase in the LTTA new liquid for use, and this enzyme is to be formed through fermentation, refinement exquisiteness by subtilis, is a kind of random hydrolysis α-D-1, the restriction endonuclease of 4 glycosidic links can produce soluble dextrins and oligose.The Ye Huamei that the present invention uses for example is the refining α-Dian Fenmei of solid of the 4000U/ml that sells of warm amylase in the liquid of the outstanding 3000U/ml that can zymin company of section sells in Wuxi, Wuxi zymin company limited.
Described saccharifying enzyme can be selected barley beta-amylase for use, and this enzyme is a kind of restriction endonuclease, mainly is starch, and soluble dextrins and oligose resolve into maltose and a spot of glucose etc., and this enzyme maltose transformation efficiency reaches more than 50%.Described saccharifying enzyme for example is the liquid barley beta-amylase of the 20000U/ml of Wuxi zymin company of outstanding energy section sale, the fungal amylase that Novozymes Company sells.
Described polygalacturonase generally adopts aspergillus niger to make with extra care and form through fermentation, extraction, is the general name of the plurality of enzymes of decompose pectin matter.Mainly contain poly-methyl galacturonate lytic enzyme, polygalacturonic acid, polygalacturonic acid lyase and Rohapect MPE can resolve into the solubility small-molecule substance with macromole mucopolysaccharide (pectin).Described polygalacturonase for example adopts the liquid polygalacturonase of the 30000U/ml that the grand mcroorganism Engineering Co., Ltd in Shandong sells, snow plum board 20000U/ml polygalacturonase that Wuxi City zymin factory sells or Shanghai to step the 20000U/ml polygalacturonase that female chemical industry company limited sells.
Utilize preparation method of the present invention can fully degrade on the one hand starch and pectin in the cocoa powder, make its hydrolysis generate monose and micromolecular oligose; On the other hand the protein in the cocoa powder is hydrolyzed, generates dissimilar amino acid and soluble polypeptide.The smell that when effectively removing macromolecular substance, can keep essence.
The invention still further relates to the cacao flavour that obtains with above-mentioned preparation method, this cacao flavour product adopts liquid phase, and liquid-instruments such as matter coupling chromatographic instrument have carried out the mensuration of chemical constitution, character and physicals.Measurement result is:
Monose and oligosaccharide contg are 15-25 weight %; Amino acid and micromolecule polypeptide content are 12-25 weight %; Theobromine, trimethyl-xanthine, polyphenol and fragrance matter content are 8-15 weight %; Ethanol aqueous solution contains 40-60%.
Performance: stable under the product room temperature, outward appearance is brown, reddish stream shape semisolid; Has strong cocoa aroma breath.
The invention still further relates to and adopt the purposes of cacao flavour noted earlier in cigarette, when using described cacao flavour, according to 0.05～0.30 weight % of tobacco leaf weight, 0.15～0.30 weight % adds cacao flavour of the present invention especially in producing the cigarette process.Except general tobacco leaf; described tobacco leaf can also be a reconstituted tobacco; claim tobacco sheet, recombination tobacco leaf, homogeneous tobacco leaf again, be meant that adding processing such as tackiness agent and other additive in tobacco material (as offal, fragment, offal or discarded tobacco leaf) makes the product that forms again.Thin at the reconstituted tobacco smoke, assorted gas, flue gas is coarse, and pungency is big, and the uncomfortable shortcoming of pleasant impression is added cacao flavor and can be kept cocoa aroma, improves the reconstituted tobacco smell of burning, covers the assorted peculiar smell of reconstituted tobacco, and reducing stimulates, and improves soften.
The effect evaluation method that uses cacao flavour of the present invention is that the perfumer smokes panel test, and its standard of smokeing panel test is:
The work of smokeing panel test must be carried out under ventilation, free from extraneous odour, peace and quiet, interference-free environment.
[beneficial effect]
Because contain the aromatoising substance that is grouped into by multiple one-tenth in the natural low fat cocoa powder, they belong to alcohols, phenols, ethers, aldehydes, ketone, ester class or lactone, and nitrogenous and S-contained substance, can enrich cigarette perfume (or spice) in burning and sucking.Though the content of these materials is little, and is indispensable for cigarette, these materials mainly utilize the ethanol aqueous solution lixiviate to obtain.Contain macromolecular substance such as a certain amount of starch and a spot of pectin in the natural cocoa powder, wherein starch, smart class material are by α-1, the polysaccharide material that the 4-glycosidic link is polymerized by a plurality of D-glucose; Pectin is the macromolecular substance that is polymerized by beta galactose aldehydic acid, also contain many small molecular sugars on its side chain, as glucose, pectinose, maltose etc., enzymolysis becomes monose and oligose under the effect of Ye Huamei and polygalacturonase, these small molecules carbohydrate materials burn and suck tobacco and can be used as sugared source participation Maillard reaction in the process, therefore enrich cigarette perfume (or spice).Protein in the cocoa powder is to pass through C by amino acid, the N bond is closed the macromolecular substance that forms, by acid hydrolysis, can generate a small amount of polypeptide and a large amount of amino acid, protein is to having burnt and sucked disadvantageous effect, and micromolecule polypeptide and amino acid can play Maillard reaction with sugared source, enrich cigarette perfume (or spice), improve to burn and suck soften.
By preparation method of the present invention can degrade macromolecular substance such as starch, protein and pectin etc. in the cocoa, the quality that improves cacao flavor keeps cocoa aroma simultaneously.
China is world's cigarette first country of consumption, and the utilization ratio of U.S.'s tobacco material has reached 99%, and China is less than 50%, and as seen market outlook is wide.Simultaneously, add the usage quantity that a certain amount of reconstituted tobacco can reduce tobacco leaf, reduce the tar content of cigarette.
[embodiment]
Can further be expressly understood the present invention by the specific embodiment of the invention given below, but these embodiment not limiting the scope of the invention.
Embodiment 1
(1) take by weighing 250g and place reactor from the natural low fat cocoa powder that Wuxi Fuhua Flavor ﹠ Fragrance Co., Ltd. buys, adding cumulative volume is the spirituous solution (V of 550mL85%
Water: V
Alcohol=15:85) forming mixture, turn on agitator stirs with 400 rev/mins speed, with 8 ℃ of/minute clock rate heating.Treat that temperature rises to 78 ℃, mixture beginning boiling, condensing reflux 1.5h then, and constantly stirring refluxes and finishes the postcooling cooling, treats that temperature reduces to normal temperature, filters then, separates and obtain solid and filtrate.
(2) solid that obtains in the step (1) is added distilled water and insert together in the bio-reactor, solid and distilled water is (M by quality ratio
Cocoa powder: M
Distilled water) 1:6, turn on agitator, speed with 250 rev/mins stirs, and with 10 ℃ of/minute clock rate heating, treats that temperature rises to 93 ℃, come to life, distill out spirituous solution 215mL, add 215mL distilled water again, cool to 80 ℃, add warm amylase in the outstanding liquid of can zymin company of section selling in 0.5g Wuxi, enzymolysis time is 2h.Enzymolysis finishes postcooling and is cooled to 55 ℃ and keep constant temperature, add the 20000U/ml barley beta-amylase of 0.5g Wuxi zymin company of outstanding energy section sale and the snow plum board 20000U/ml liquid polygalacturonase that 0.25g Wuxi City zymin factory sells, stir speed (S.S.) is 250 rev/mins, enzymolysis time 4h.After enzymolysis is finished, enzymatic hydrolysis system is heated the enzyme that goes out, the temperature of the enzyme that goes out is 95 ℃, and the time is 15 minutes, and stir speed (S.S.) still is controlled at 250 rev/mins.After the enzyme that goes out finishes, with being water-cooled to normal temperature, the product in the reactor is carried out centrifugal, centrifugation rate is 4000 rev/mins, and centrifugation time is 15 minutes, and centrifugal ends be separation afterwards, obtains supernatant liquor and solid respectively, and wherein supernatant liquor is little red-brown, and solid is red-brown.
(3) the centrifugal back solid in the step (2) is placed reactor, adding concentrated hydrochloric acid, distilled water to cumulative volume are 1500mL, and the hydrochloric acid volumetric molar concentration is 6mol/L in the mixture.Turn on agitator stirs with 300 rev/mins, with 10 ℃ of/minute clock rate heating, treats that temperature rises to 106 ℃, and mixture comes to life, and keeps constant temperature and constantly stirs heating condensing reflux 8h.After reaction finishes, be cooled to normal temperature, filter to get filtrate and filter residue, filtrate is transferred in the vacuum concentration instrument, carry out concentration, spissated temperature is controlled at 55 ℃, and vacuum degree control is at-0.096MPa, and the heat-eliminating medium of vacuum concentration instrument is an ordinary tap water, when filtrate is concentrated into stream shape thing solid, reconcentration 15 minutes makes as far as possible that hydrochloric acid is residual reduces to minimumly, stops to concentrate.
(4) after being stirred, the stream shape thing solid in the supernatant liquor combining step (3) in the step (2) concentrates again, spissated temperature is controlled at 55 ℃, vacuum degree control is at-0.097MPa, heat-eliminating medium is an ordinary tap water, the solution to be concentrated water content is lower than at 5% o'clock, stop to concentrate, merge the alcoholic extract liquid in (1) and stir and promptly obtain cacao flavor.Stable under this product room temperature, outward appearance is brown, reddish stream shape semisolid; Has strong cocoa aroma breath.
This cacao flavor product liquid phase, liquid chromatograph/mass spectrometer analysis, its chemical constitution is: monose and oligose contain 16.4%; Amino acid and micromolecule polypeptide contain 15.0%; Theobromine, trimethyl-xanthine, polyphenol and fragrance matter contain 12.9%; Ethanol aqueous solution contains 55.5%.
Smoke panel test by eight perfumers, its smoking result is for having cocoa feature perfume (or spice), harmony still, and slightly assorted gas, pungency obviously descends, and is softer, and pleasant impression is still comfortable.
Embodiment two:
(1) take by weighing 250g and place reactor from the natural low fat cocoa powder that company of Wuxi Fuhua Flavor ﹠ Fragrance Co., Ltd. buys, adding cumulative volume is 500mL80% (V
Water: V
Alcohol=20:80) ethanol aqueous solution obtains mixture, stirs with the speed of agitator with 400 rev/mins then, with 10 ℃ of/minute clock rate heating, treats that temperature rises to 78 ℃, and mixture comes to life.Condensing reflux 2h, and continue to stir refluxes and finishes the postcooling cooling, treats that temperature reduces to normal temperature and filter, and separates obtaining solid and filtrate.
(2) in bio-reactor, be M with the mass ratio
Cocoa powder: M
Distilled waterThe solid and the distilled water that obtain in=the 1:5 mixing step (1), turn on agitator, speed with 220 rev/mins stirs, with 8 ℃ of/minute clock rate heating, treat that temperature rises to 94 ℃, come to life, distill out spirituous solution 220mL, add 220mL distilled water postcooling again and be cooled to 75 ℃, add warm Ye Huamei in the 1.0g liquid, enzymolysis time 1.5h, enzymolysis finishes postcooling and is cooled to 50 ℃ and keep constant temperature, adds the 30000U/ml liquid polygalacturonase that the grand mcroorganism Engineering Co., Ltd in 0.4g liquid barley beta-amylase and 0.2g Shandong sells, and stir speed (S.S.) is 250 rev/mins, enzymolysis time 4h, after enzymolysis is finished, enzymatic hydrolysis system is heated the enzyme that goes out, the temperature of the enzyme that goes out is 95 ℃, time is 20 minutes, and stir speed (S.S.) still is controlled at 250 rev/mins.After the enzyme that goes out finished, with being water-cooled to normal temperature, the product in the reactor carried out centrifugal, and centrifugation rate is 4000 rev/mins, and centrifugation time is 15 minutes, and separate centrifugal end back, obtains supernatant liquor and solid respectively.
(3) the centrifugal back solid in the step (2) is placed reactor, adding concentrated hydrochloric acid and distilled water to cumulative volume is 1250mL, the hydrochloric acid volumetric molar concentration is 5mol/L in the mixture, turn on agitator stirs with 250 rev/mins speed, with 8 ℃ of/minute clock rate heating, treat that temperature rises to 103 ℃, come to life, keep constant temperature and constantly stir heating condensing reflux 8h, after reaction finishes, be cooled to normal temperature, filter to get filtrate and filter residue, filtrate is transferred in the vacuum concentration instrument, carry out concentration, spissated temperature is controlled at 57 ℃, and vacuum degree control is at-0.095MPa, and the heat-eliminating medium of vacuum concentration instrument is an ordinary tap water, when filtrate is concentrated into stream shape thing solid, reconcentration 20min makes as far as possible that hydrochloric acid is residual reduces to minimumly, stops to concentrate.
(4) after being stirred, the stream shape thing solid in the supernatant liquor combining step (3) in the step (2) concentrates again, thickening temperature is 57 ℃, vacuum tightness is-0.096MPa, heat-eliminating medium is an ordinary tap water, the solution to be concentrated water content is lower than at 3% o'clock, stop to concentrate, the alcoholic extract liquid in the combining step (1) also stirs and promptly obtains product.This product appearance is brown, reddish stream shape semisolid; Has strong cocoa aroma breath.
This cacao flavor product liquid phase, liquid chromatograph/mass spectrometer analysis, its chemical constitution is: monose and oligose contain 15.1%; Amino acid and micromolecule polypeptide contain 14.2%; Theobromine, trimethyl-xanthine, polyphenol and fragrance matter contain 12.0%; Ethanol aqueous solution contains 58.3%.
Smoke panel test by seven perfumers, its smoking result is for having cocoa feature perfume (or spice), and little have assorted gas, and pungency descends, and soften obviously improves, and pleasant impression is still clean.
Embodiment three:
(1) takes by weighing the natural low fat cocoa powder of 250g (amount of cocoa butter content is 8%) and place reactor, add cumulative volume 600mL70% (V
Water: V
Alcohol=30:70) ethanol aqueous solution, speed with 350 rev/mins stirs, with 10 ℃ of/minute clock rate heating, treat that temperature rises to 78 ℃, mixture comes to life, condensing reflux 1h, and constantly stir, reflux to finish the postcooling cooling, treat that temperature reduces to normal temperature and filter, separate obtaining solid and filtrate.
(2) with the solid that obtains in the step (1), distilled water with M
Cocoa powder: M
Distilled water=1:7 inserts in the HKG-II rotary type type bio-reactor of Shanghai glad stamen automatic equipment company limited producing and selling, stir with 250 rev/mins, with 8 ℃ of/minute clock rate heating, treat that temperature rises to 94 ℃, come to life, distill out spirituous solution 200mL, add 200mL distilled water postcooling again and be cooled to 70 ℃, add the neutral Ye Huamei of 0.75g liquid, enzymolysis time 2h, enzymolysis finish postcooling and are cooled to 50 ℃ and keep constant temperature, add 0.25g liquid barley beta-amylase and 0.1g liquid polygalacturonase, stir speed (S.S.) is 200 rev/mins, enzymolysis time 3h.After enzymolysis is finished, enzymatic hydrolysis system is heated the enzyme that goes out, the temperature of the enzyme that goes out is 95 ℃, and the time is 15 minutes, and stir speed (S.S.) still is controlled at 250 rev/mins.After the enzyme that goes out finished, with being water-cooled to normal temperature, the product in the reactor carried out centrifugal, and centrifugation rate is 4000 rev/mins, and centrifugation time is 15 minutes, and separate centrifugal end back, obtains supernatant liquor and solid respectively.
(3) the centrifugal back solid that step (2) is obtained places reactor, adds concentrated hydrochloric acid, and distilled water to total mass is 1500mL, the solution volumetric molar concentration is 4mol/L, speed with 250 rev/mins stirs, and with 8 ℃ of/minute clock rate heating, treats that temperature rises to 103 ℃, come to life, keep constant temperature and constantly stirring, heating condensing reflux 8h is after reaction finishes, be cooled to normal temperature, filter to get filtrate and filter residue.Filtrate is transferred in the vacuum concentration instrument, carried out concentration, spissated temperature is 60 ℃, and vacuum tightness is-0.094MPa, and the heat-eliminating medium of vacuum concentration instrument is an ordinary tap water, and when filtrate is concentrated into stream shape thing solid, reconcentration 15 minutes stops to concentrate.
(4) after being mixed, stir, the stream shape thing solid in supernatant liquor in the step (2) and the step (3) concentrates again, spissated temperature is 55 ℃, vacuum tightness is-0.094MPa, heat-eliminating medium is an ordinary tap water, the solution to be concentrated water content is lower than at 5% o'clock, stop to concentrate, the alcoholic extract liquid that combining step (1) obtains also stirs and promptly obtains product.This product appearance is brown, reddish stream shape semisolid; Has strong cocoa aroma breath.
This cacao flavor product liquid phase, liquid chromatograph/mass spectrometer analysis, its chemical constitution is: monose and oligose contain 17.2%; Amino acid and micromolecule polypeptide contain 16.0%; Theobromine, trimethyl-xanthine, polyphenol and fragrance matter contain 13.5%; Ethanol aqueous solution contains 53.3%.
Smoke panel test by eight perfumers, smoke panel test to such an extent that be divided into the fragrance abundance, coarse slightly, than harmony, little have a stimulation, and pleasant impression is cleaner, and soften strengthens.
Preparation method of the present invention can be good at keeping the many aroma components in the cocoa powder, can learn that from product analysis big variation does not all take place these aroma components.On the basis that keeps these materials, the present invention produces non-existent material in many cocoa powders by enzymolysis, comprises the beta galactose aldehydic acid that is mainly derived from monose that amylorrhexis generates and oligose, pectin enzymolysis and generates, amino acid and the polypeptide that the protein acid hydrolysis generates.These materials itself do not have fragrance, but they can obviously improve the suction flavor when tobacco burns and sucks, increase soften, improve the cigarette quality.Through the stability experiment checking, the quality guaranteed period of this product is long, and it is water-soluble also relatively good simultaneously.
The outward appearance of the cacao flavor product that the present invention obtains is brown, reddish stream shape semisolid; Has strong cocoa aroma breath; Natural low fat cocoa powder total sugar content accounts for gross weight 23%, utilize Ye Huamei and saccharifying enzyme enzymolysis to handle after, generate monose and oligosaccharides, product is through the detected carbohydrate content of LC-MS chromatographic instrument and relative content such as table 1:
Table 1
Natural low fat cocoa powder protein content accounts for 21% of gross weight, through acid hydrolysis, protein complete hydrolysis, generates amino acid and a spot of polypeptide of solubility, and amino acid is analyzed composition and relative content such as table 2 by high performance liquid chromatography amino acid post:
Table 2
As can be seen from the above table, the amino acid kind is abundanter, more than at least 16 kinds, may comprise that also some fail the amino acid of detected amino acid and more complicated, and this flavour to cigarette plays good effect.
Natural low fat cocoa powder extracts by ethanol aqueous solution, the compound biological enzyme enzymolysis, and series of steps such as acid hydrolysis, last transformation efficiency can reach more than 70%.
Claims (9)
1, a kind of preparation method of cacao flavor is characterized in that this method comprises the steps:
(1) mixes, separates
Cocoa powder and 70-85% ethanol aqueous solution are mixed with mass ratio 1:2-1:3, and at temperature 70-90 ℃, stirring velocity 300-500 rev/min following condensing reflux 1-2 hour, cooling is filtered and is obtained filtrate and filter cake;
(2) enzymolysis
In the filter cake that step (1) obtains, add water and obtain mixture, the mass ratio of cocoa powder is 5-7:1 in water that adds and the step (1), the gained mixture stirs under 85-95 ℃, heating, the part alcohol that evaporation wherein exists, ethanol content in mixture is lower than 10%, then, add water again with institute's evaporating solns equal volume, add Ye Huamei down at 75-80 ℃ and carried out enzymolysis 1-3 hour, after enzymolysis was finished, adding saccharifying enzyme and polygalacturonase carried out enzymolysis 3-5 hour under 45-55 ℃ again, after enzymolysis is finished, at 90-100 ℃ of following 5-20 minute enzyme that goes out of heating, cool off centrifugally then, separate obtaining supernatant liquor and solid;
(3) concentrate
The solid that obtains in the step (2) is placed reactor, add concentrated hydrochloric acid and water, obtain the mixture that concentration of hydrochloric acid is 3-6mol/L, the mass ratio of cocoa powder and hydrochloric acid soln is 1:4-7,100-110 ℃ of following heated and stirred, condensing reflux 5-8 hour, cold filtration then, obtain filtrate and filter residue, filtrate concentrating obtains flowing shape thing solid; Concentrate after the supernatant liquor that gained stream shape thing solid and step (2) obtain merges, obtain brown stream shape thing solid;
(4) make product
The brown stream shape thing solid that filtrate that step (1) is obtained and step (3) obtain mixes and obtains described cacao flavor.
2, preparation method according to claim 1 is characterized in that the cacao flavor that this method comprises that also step (4) obtains carries out reconcentration, is lower than 5% until gained cacao flavor water content.
3, preparation method according to claim 1 is characterized in that the pH value of the mixture of middle filter cake of step (2) and water is 5-7, and stir speed (S.S.) is 150-300 rev/min.
4, preparation method according to claim 1 is characterized in that described cocoa powder is selected from natural low fat cocoa powder.
5, preparation method according to claim 1 and 2, it is characterized in that described concentrate be in the vacuum concentration instrument 45～65 ℃ of temperature, vacuum tightness-0.09～-carry out under the condition of 0.1MPa.
6, preparation method according to claim 1 is characterized in that Ye Huamei described in the step (1) is middle temperature amylase.
7, preparation method according to claim 1 is characterized in that saccharifying enzyme is a barley beta-amylase described in the step (1).
8, the cacao flavor that obtains according to the described preparation method of arbitrary claim among the claim 1-7.
9, cacao flavor according to claim 8 is as the purposes of tobacco additive agent.
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Patentee after: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee before: Huabao flavor Ltd. Patentee before: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee after: Huabao flavor Ltd. Patentee after: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. Address before: 201821 Yecheng Road, Shanghai, No. 1299, No. Patentee before: Huabao Flavours & Fragrances Co.,Ltd Patentee before: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Patentee after: Wuxi Huaxin essence Co.,Ltd. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee before: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Patentee before: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. |
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Effective date of registration: 20170405 Address after: 201821 Road, Jiading Industrial Zone, Shanghai, building C, No. 1299 Patentee after: SHANGHAI HUABAO PEACOCK ESSENCE CO.,LTD. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee before: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Patentee before: Wuxi Huaxin essence Co.,Ltd. |