CN101497845B - Method for producing cigarette flavor by maillard reaction with red date extract as raw material - Google Patents

Method for producing cigarette flavor by maillard reaction with red date extract as raw material Download PDF

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CN101497845B
CN101497845B CN 200810046835 CN200810046835A CN101497845B CN 101497845 B CN101497845 B CN 101497845B CN 200810046835 CN200810046835 CN 200810046835 CN 200810046835 A CN200810046835 A CN 200810046835A CN 101497845 B CN101497845 B CN 101497845B
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reaction
fructus jujubae
maillard reaction
tobacco
jujubae extract
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CN101497845A (en
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朱巍
殷发强
肜霖
潘婷婷
董世良
何佳文
佘跃群
邵璐
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China Tobacco Hunan Industrial Co Ltd
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Abstract

The invention discloses a method for producing tobacco perfume by adopting red jujube extract through the Maillard reaction, which relates to a preparation method of tobacco perfume. The preparation method comprises the following steps: (1) preparing the red jujube extract; (2) adding one or a plurality of types of aminophenol or amines in the red jujube extract, adding H2O and solvent which are placed in a reaction kettle to be mixed into a homogeneous reaction system, adjusting the pH value of the reaction system, putting reagent into a return pipe, leading the reagent to perform the Maillard reaction under the conditions of mixing, heating and normal pressure, and obtaining the tobacco perfume by the return reaction. The method enables the perfume material in the red jujube extract to mutually serve the perfume material produced in the Maillard reaction, thereby forming the tobacco perfume with rich and special fragrance and multiple type, having strong fruity coordinating with the smoke gas of a cigarette, increasing the smoke gas concentration, leading the smoke gas to be soft and exquisite, hiding the mixed gas and obviously improving the tobacco quality.

Description

With the Fructus Jujubae extract is the method for raw material through Maillard reaction to produce tobacco flavor
Technical field
The present invention relates to a kind of preparation method of tobacco aromatics using, especially is the method for raw material through Maillard reaction to produce tobacco flavor with the Fructus Jujubae extract.
Background technology
In the prior art, the tobacco aromatics using of cigarettes plus is general to adopt two big types: one type is natural extract spices, utilizes natural component that contain in the natural perfume or potential and flue gas coordination; Another kind of is exactly synthetic perfume, utilizes synthetic and flue gas to coordinate, and flue gas is had the perfume monomer of certain effect.The tobacco aromatics using that these two big types of spices are independent or allotment is processed is though technology is simple, because fragrance is dull, single to the effect of flue gas, effect is not fine.The research of China on tobacco aromatics using is relatively backward always, the spices dependence on import of the overwhelming majority, and therefore, the tobacco aromatics using that development effectiveness is good is necessary.Response class spices (being the Maillard reaction thing) is the spices that very important and the utmost point have using value on tobacco and the food always; The fragrance that reaction produces is also different according to sugared source, ammonia source difference; A large amount of heterocycle perfume compounds that reaction produces have the improvement effect to cigarette smoke.
The domestic people of having reacts glucose and amino acid simply, generates the Maillard reaction thing, and this spices kind is few, fragrance is single, improves limited to tobacco sucking quality.Chinese patent (CN1162008A) discloses " a kind of method of producing tobacco aromatics using ", and it is a raw material with the tobacco, after the raw material pulverizing; Add the water boiling sterilization, insert fermented bacterium, 20~70 ℃ of bottom fermentations 2 hours~3 days; Add SX subsequently, obtain product, this method through separating to purify again; Complex process, length consuming time, and also raw material sources are unstable.Chinese patent (CN1415717A and CN1175623A) discloses " being the method for raw material production spices with the tobacco extract " and has reached " preparation method of tobacco reacting substance perfume and utilization "; They all are raw material with the tobacco extract, add sugar and amino acid generation Maillard reaction, though this method has been utilized Maillard reaction; But because the kind of institute's sugaring is single; Some sugared cost is very high, and its fragrance is difficult to reach promising result, and its raw material sources are unstable equally.U.S. Pat 3,920,026 discloses " tobacco flavor enriches agent ", utilizes reducing sugar and amino acid to process tobacco aromatics using under certain condition, same, because the kind of sugar is more single, some sugared cost is very high, is difficult to reach promising result.
In a word, up to the present, utilize Maillard reaction to prepare the method for tobacco aromatics using, or complex process, cost is high, and raw material sources are unstable, or fragrance is dull, acts on singlely, and effect is undesirable.Therefore, provide a kind of effective, the Maillard reaction tobacco aromatics using that cost is low is very important.
Summary of the invention
To the above-mentioned deficiency of prior art, it is the method for raw material through Maillard reaction to produce tobacco flavor with the Fructus Jujubae extract that the technical problem that the present invention will solve provides a kind of.Method of the present invention organically combines the fragrance of natural jujube extract itself and the fragrance of Maillard reaction, and the fragrance matter that fragrance matter and Maillard reaction in the Fructus Jujubae extract are produced sets off mutually, thereby it is abundant, unique to form fragrance; Numerous in variety, have strong fruital note, with the spices of cigarette smoke coordination; Increase flue gas concentration; Make the soft exquisiteness of flue gas, cover assorted gas, significantly improve cigarette quality.
Technical scheme of the present invention: with the Fructus Jujubae extract is that raw material carries out through the method for Maillard reaction to produce tobacco flavor according to the following steps:
[1] produces Fructus Jujubae extract
Producing Fructus Jujubae extract carries out according to the following steps:
(1) commercially available have a nuclear red date dry fruit, and moisture content is 20% ± 2%, rejects mouldy, septic red date, cleans then, drains;
(2) put into reaction kettle after the red date flattening that will choose, clean, drains, the fragmentation; Require broken getting final product, size is not limit, and presses red date: the mixed of 75% edible ethanol=1: 4; Stirring heating reflux extraction is 6 hours under 90 ± 5 ℃ of temperature, is cooled to room temperature;
(3) supernatant is extracted in the clarification in 5 hours of the solution left standstill after will lowering the temperature; After lower floor's soup compound was centrifugal, the reject dregs merged clear liquid;
(4) clear liquid is poured in the concentration kettle concentrated, concentrate recovered alcohol in 80 ± 2 ℃ of temperature, vacuum tightness under greater than the condition of 0.95Mpa, the enriched material degree Beaume stops to concentrate when being 25 ° of B é, and gained dark-brown thick liquid is Fructus Jujubae extract.
[2] preparation tobacco aromatics using
In Fructus Jujubae extract, add one or more amino acid or Ammonia material, add H 2O and solvent; Place reaction kettle to stir into the reaction system of homogeneous; The pH value of conditioned reaction system is 2~11, the return line of packing into, at mixing speed between 100~1000 rev/mins, make reactant generation Maillard reaction under 70~120 ℃ of the Heating temperatures, condition of normal pressure; Reaction times was controlled between 1-7 hour, and the back flow reaction products therefrom is tobacco aromatics using.
Described amino acid or Ammonia material are L-Ala, proline(Pro), Xie Ansuan, l-arginine, Serine, phenylalanine(Phe), L-glutamic acid, aspartic acid, glycocoll, tyrosine, Secondary ammonium phosphate.
The add-on of described amino acid or Ammonia material is 2~30% of a Fructus Jujubae extract weight.
Described solvent is Ucar 35, USP Kosher, terepthaloyl moietie, and its add-on is 0~20% of a Fructus Jujubae extract weight.
The acidic cpd that the pH value of conditioned reaction system adopts is more than one in hydrochloric acid, acetic acid, the Hydrocerol A etc., and basic cpd is more than one among strong aqua, NaOH, the KOH.
Method of the present invention has the following advantages:
1. it is dull how to improve traditional Maillard reaction fragrance, and the shortcoming that adding cigarette fragrance stings is a difficult point of the present invention.Fructus Jujubae extract itself contains a lot of fragrance matters, contains saturated and unsaturated aldehyde, ketone, alcohol, acid, ester, hydrocarbon, terpenes and furans and lactone compound, these materials to cigarette flavouring is arranged, cover assorted, improve mouthfeel and fall the effect of thorn; The present invention selects the natural jujube extract for use, through testing repeatedly, groping, has chosen some nitrogenous compounds, solvent and reaction conditions; The fragrance of natural jujube extract itself and the fragrance of Maillard reaction are organically combined, and the fragrance matter that fragrance matter and Maillard reaction in the Fructus Jujubae extract are produced sets off mutually, thereby it is abundant, unique to form fragrance; Numerous in variety, have strong fruital note, with the spices of cigarette smoke coordination; Increase flue gas concentration; Make the soft exquisiteness of flue gas, cover assorted gas, significantly improve cigarette quality.
2. contain the rich saccharide material in the Fructus Jujubae extract, like glucose, fructose and sucrose, also contain a spot of SANMALT-S, semi-lactosi, numerous in variety, content is high, accounts for about 50% of its total amount, for rich and varied Maillard reaction takes place the basis is provided;
3. the glucide in the red date is compared with pure glucide, has the low characteristics of cost;
4. through adding different nitrogenous sources such as ammoniacal liquor, ammonia salt, amino acid generation Maillard reaction, can make the different spices of effect.
5. contain in the Fructus Jujubae extract materials such as rich saccharide and amino acid participate in behind the Maillard reactions product than traditional single Maillard reaction thing to cause perfumery much more, enriched the fragrance of cigarette like this, promoted quality of cigarette.
Though Fructus Jujubae extract contain much to cigarette flavouring is arranged, cover assorted, improve mouthfeel and fall the material of thorn effect; Also there are shortcomings such as flavouring is not enough, pleasant impression is not good enough; Utilize the sugar generation Maillard reaction in the red date can produce abundant heterogeneous ring compound; These materials can remedy these shortcomings, set off mutually.
Embodiment
Further illustrate content of the present invention below in conjunction with embodiment, but these embodiment do not limit protection scope of the present invention.
Fructus Jujubae extract contains volatile component such as saturated and unsaturated aldehyde, ketone, alcohol, acid, ester, hydrocarbon, terpenes and furans and the lactone compound useful to flue gas, contains the rich saccharide material in addition.Such as: glucose, fructose, semi-lactosi or the like.Utilize these also variety of source sugar, through amino acid or the Ammonia material that adds one or more, and H 2O and solvent; Place reaction kettle to stir into the reaction system of homogeneous; Utilize the pH value of acidity or basic cpd conditioned reaction system, load onto return line then, under agitation heat normal pressure generation Maillard reaction; The fragrance matter that fragrance matter and Maillard reaction in the Fructus Jujubae extract are produced sets off mutually, thereby processes the good tobacco aromatics using of effect.
Wherein Fructus Jujubae extract itself also is a kind of tobacco aromatics using, is raw material with it, through adding amino acid or Ammonia material, Maillard reaction takes place, and can be made into tobacco aromatics using wide in variety, better effects if.
Because reaction is carried out under heating condition, therefore must controlled temperature and installation reflux.Through kind and amount and the proportioning that amino acid or Ammonia material are added in change, the amount and the kind of change solvent, thus obtain tobacco aromatics using wide in variety, to satisfy the production of cigarettes needs.
Because the reducing sugar content in the Fructus Jujubae extract is higher and wide in variety various; And contain saturated and unsaturated aldehyde, ketone, alcohol, acid, ester, hydrocarbon, terpenes and furans and lactone compound; These materials have flavouring, cover the effect of mixing and falling thorn cigarette, therefore, can use it as the abundant sugared source of Maillard reaction; But aminoacids content wherein is low, so must be toward the amino acid or the Ammonia material that wherein add one or more.
After add amino acid or Ammonia material, can be to wherein adding certain amount of solvent like H 2O, Ucar 35, USP Kosher, terepthaloyl moietie etc., its effect is to help amino acid whose dissolving and reaction.
Above-mentioned all compounds are added in the reaction kettle, stir into uniform reaction system, using the pH value of acidity or basic cpd conditioned reaction system then is 2~11, and said acidic cpd is one or more in hydrochloric acid, acetic acid, the Hydrocerol A etc.Basic cpd is one or more among strong aqua, NaOH, the KOH, opens the water coolant of reflux, is heated to 70~120 ℃, and it adds electrically heated of thermal recovery thermal oil or steam heating.
In order to make the reaction system thermally equivalent, in heating, must stir, stir and use the adjustable speed whisking appliance, its rotating speed should be between 100~1000 rev/mins.Make the temperature of reaction reach predetermined temperature through heating.Its temperature of reaction is different and different according to amino acid that adds or Ammonia material, generally is controlled at 70~120 ℃, is reflected under the normal pressure and carries out.
Reaction times is different and different according to amino acid that adds or Ammonia material, generally is controlled at 1-7 hour.Reaction is put into storage tank with reaction product after finishing, and naturally cooling gets product-tobacco aromatics using of the present invention.
Embodiment 1
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 30 gram L-Ala, start stirring; Adding ammoniacal liquor adjusting pH again is 9.7, connects reflux condensing tube, is heated to 90 ℃ with oil bath; Constant temperature 3 hours, stirring velocity are 200 rev/mins, stop heating then; Pour out reactant, remove insolubles with gauze, gained filtrating is product of the present invention.Products obtained therefrom shows very strong jujube perfume, baking perfume (or spice) and nutty.This product joined with 0.8 ‰ amount please comment the cigarette expert to smoke panel test in the blank cigarette, the result sees table 1.
Embodiment 2
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 15 gram L-Ala, 15 gram proline(Pro); Start stirring, adding ammoniacal liquor adjusting pH again is 9.7, connects reflux condensing tube, is heated to 95 ℃ with oil bath; Constant temperature 3.5 hours, stirring velocity are 200 rev/mins, stop heating then; Pour out reactant, remove insolubles with gauze, gained filtrating is product of the present invention.It is fragrant, burnt fragrant and sweet that products obtained therefrom shows very strong jujube, this product joined with 0.8 ‰ amount please comment the cigarette expert to smoke panel test in the blank cigarette, and the result sees table 1.
Embodiment 3
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 40 gram proline(Pro), start stirring; Add 50 gram Ucar 35 again, it is 9.7 that strong aqua is regulated pH, connects reflux condensing tube, is heated to 110 ℃ with oil bath; Constant temperature 3 hours, stirring velocity are 300 rev/mins, stop heating then; Pour out reactant, remove insolubles with gauze, gained filtrating is product of the present invention.Products obtained therefrom shows very strong baking perfume, Mi Xiang.This product joined with 0.8 ‰ amount please comment the cigarette expert to smoke panel test in the blank cigarette, the result sees table 1.
Embodiment 4
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 30 gram l-arginine, start stirring; Adding phosphoric acid ammonia two ammoniums adjusting pH again is 7.2, connects reflux condensing tube, is heated to 90 ℃ with oil bath; Constant temperature 3 hours, stirring velocity are 200 rev/mins, stop heating then; Pour out reactant, remove insolubles with gauze, gained filtrating is product of the present invention.It is fragrant that this product shows very strong jujube perfume, baking.This product joined with 0.8 ‰ amount please comment the cigarette expert to smoke panel test in the blank cigarette, the result sees table 1.
Embodiment 5
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 10 gram proline(Pro), 10 gram glycocoll, 10 gram L-glutamic acid, start stirring; Adding the lemon acid for adjusting pH again is 3, connects reflux condensing tube, is heated to 90 ℃ with oil bath; Constant temperature 3 hours, stirring velocity are 200 rev/mins, stop heating then; Pour out reactant, remove insolubles with gauze, gained filtrating is product of the present invention.It is fragrant that this product shows very strong baking.This product joined with 0.8 ‰ amount please comment the cigarette expert to smoke panel test in the blank cigarette, the result sees table 1.
Embodiment 6
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 50 gram phosphoric acid ammonia, two ammoniums, pH is 7.4; Start stirring, connect reflux condensing tube, be heated to 85 ℃ with oil bath; Constant temperature 5 hours, stirring velocity are 200 rev/mins, then stopped reaction; Pour out reactant, use filtered through gauze, filtrating is product of the present invention.This product shows strong burnt sweet roasting fragrance breath.This product joined with 0.8 ‰ amount please comment the cigarette expert to smoke panel test in the blank cigarette, the result sees table 1.
Embodiment 7
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 30 gram Xie Ansuans, start stirring; Adding NaOH adjusting pH again is 11, connects reflux condensing tube, is heated to 90 ℃ of temperature with oil bath; Constant temperature 4 hours, stirring velocity are 300 rev/mins, stop reacting by heating then; Pour out reactant, use filtered through gauze, filtrating is product of the present invention.This product shows tangible chocolate fragrant.This product joined by 1 ‰ please comment the cigarette expert to smoke panel test in the blank cigarette, the result sees table 1.
Embodiment 8
Take by weighing 500 gram Fructus Jujubae extracts, put into three-necked flask, add 20 gram L-Ala, start stirring; Adding acetic acid adjusting pH again is 3, connects reflux condensing tube, is heated to 95 ℃ with oil bath; Constant temperature 3.5 hours, stirring velocity are 800 rev/mins, stop heating then; Pour out reactant, remove insolubles with gauze, gained filtrating is product of the present invention.It is fragrant that products obtained therefrom shows very strong jujube, this product joined with 0.8 ‰ amount please comment the cigarette expert to smoke panel test in the blank cigarette, and the result sees table 1.
Table 1 smoking result
Figure GSB00000831598300081
Figure GSB00000831598300091
Visible by above embodiment 1~8: as,, Maillard reaction to take place through amino acid or the Ammonia material that adds one or more with containing the Fructus Jujubae extract that enriches reducing sugar; The tobacco aromatics using fragrance of processing is abundant, and comfortable taste is covered assorted gas; Fragrance remaining time is long, obviously improves quality of cigarette.
In a word, tobacco aromatics using making method of the present invention can be tobacco industry colory tobacco aromatics using is provided, and promotes the development of cigarette industry.

Claims (2)

1. one kind is the method for raw material through Maillard reaction to produce tobacco flavor with the Fructus Jujubae extract, it is characterized in that described method carries out according to the following steps:
[1] produces Fructus Jujubae extract
Producing Fructus Jujubae extract carries out according to the following steps:
(1) commercially available have a nuclear red date dry fruit, and moisture content is 20% ± 2%, rejects mouldy, septic red date, cleans then, drains;
(2) put into reaction kettle after the red date flattening that will choose, clean, drains, the fragmentation; Require broken getting final product, size is not limit, and presses red date: the mixed of 75% edible ethanol=1: 4; Stirring heating reflux extraction is 6 hours under 90 ± 5 ℃ of temperature, is cooled to room temperature;
(3) supernatant is extracted in the clarification in 5 hours of the solution left standstill after will lowering the temperature; After lower floor's soup compound was centrifugal, the reject dregs merged clear liquid;
(4) clear liquid is poured in the concentration kettle concentrated, concentrate recovered alcohol in 80 ± 2 ℃ of temperature, vacuum tightness under greater than the condition of 0.95Mpa, the enriched material degree Beaume stops to concentrate when being 25 ° of B é, and gained dark-brown thick liquid is Fructus Jujubae extract;
[2] preparation tobacco aromatics using
In Fructus Jujubae extract, add one or more amino acid or Ammonia material, add H 2O and solvent; Place reaction kettle to stir into the reaction system of homogeneous; The pH value of conditioned reaction system is 2~11, the return line of packing into, at mixing speed between 100~1000 rev/mins, make reactant generation Maillard reaction under 70~120 ℃ of the Heating temperatures, condition of normal pressure; Reaction times was controlled between 1-7 hour, and the back flow reaction products therefrom is tobacco aromatics using;
Described amino acid or Ammonia material are L-Ala, proline(Pro), Xie Ansuan, l-arginine, Serine, phenylalanine(Phe), L-glutamic acid, aspartic acid, glycocoll, tyrosine, Secondary ammonium phosphate;
The add-on of described amino acid or Ammonia material is 2~30% of a Fructus Jujubae extract weight; Described solvent is Ucar 35, USP Kosher, terepthaloyl moietie, and its add-on is 0~20% of a Fructus Jujubae extract weight.
2. according to claim 1 is the method for raw material through Maillard reaction to produce tobacco flavor with the Fructus Jujubae extract; It is characterized in that: the acidic cpd that the pH value of conditioned reaction system adopts is more than one in hydrochloric acid, acetic acid, the Hydrocerol A, and basic cpd is more than one among strong aqua, NaOH, the KOH.
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