CN106433982B - method for preparing fresh and sweet aroma essence from tobacco leaf cut stems - Google Patents
method for preparing fresh and sweet aroma essence from tobacco leaf cut stems Download PDFInfo
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- CN106433982B CN106433982B CN201610838241.2A CN201610838241A CN106433982B CN 106433982 B CN106433982 B CN 106433982B CN 201610838241 A CN201610838241 A CN 201610838241A CN 106433982 B CN106433982 B CN 106433982B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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Abstract
the invention provides a method for preparing fresh and sweet aroma essence from tobacco stem shreds, which comprises the following steps: 1) taking tobacco stem powder, adding water, stirring uniformly, and then adding fungal amylase and pectinase to carry out first-stage enzymolysis; 2) after the first-stage enzymolysis reaction is finished, adding protease for second-stage enzymolysis; 3) after the second-stage enzymolysis reaction is finished, deactivating enzyme of the product, and cooling to obtain tobacco stem enzymolysis liquid; 4) adding glycine and the waxberry extract into the tobacco stalk enzymolysis liquid, uniformly stirring, and carrying out Maillard reaction to obtain the required essence. The invention further provides application of the essence in tobacco leaves. The method for preparing the fresh-sweet aroma essence from the cut stems of the tobacco leaves, provided by the invention, has an obvious fresh-sweet aroma by enzymolysis-Maillard reaction, can obviously improve the aroma quality of cigarettes, enrich the tobacco aroma, enrich the smoke, and improve the smoking quality of the cigarettes.
Description
Technical Field
the invention belongs to the technical field of cigarette essence, and relates to a method for preparing fresh and sweet aroma essence from cut stems of tobacco leaves.
Background
solanum nigrum L of Nicotiana, annual or perennial herbaceous plant of Solanaceae, with slightly lignified basal part, terminal inflorescence, coniform and flowery; the capsule is egg-shaped or rectangular, has length approximately equal to that of preserved calyx, flowers and fruits in summer and autumn, and is mainly distributed in south America, south Asia and China. Tobacco, as a hobby consumer product, has a large number of consumers in every part of the world. However, in recent years, with the increasing global progress of the world economy, the problem of "smoking and health" has been receiving more and more attention from society, so that tar and harm reduction has become a serious concern in the cigarette industry. Generally, the tar and harm reduction causes a great loss of the beautiful smoking position components of the cigarette, the cigarette fragrance is insufficient, and the requirements of consumers are difficult to meet. In order to solve the problems, a large amount of essence is added in many cigarette factories while blending cigarette formulas, so that the defects of cigarette smoking positions are overcome, but the cigarette is lack of natural feeling and has offensive odor.
The tobacco stem refers to the stem shred of the tobacco leaf, namely the coarse and hard veins of the tobacco leaf, and accounts for about 25 to 30 percent of the weight of the leaf. China is a big country in the tobacco industry, and the tobacco stems are used as the largest byproducts in the tobacco industry, hundreds of thousands of tons of tobacco stems are discarded every year, so that the environmental pollution is caused, and the waste of natural resources is also caused. Researches show that the types of components contained in the tobacco stems are basically consistent with the components of the tobacco leaves, and the tobacco stems have great practical application value. At present, the utilization of the tobacco stems in the cigarette industry is only limited to filling expanded cut stems, cut stems and other products, but the products bring many disadvantages to cigarettes, such as insufficient cigarette fragrance, weak smoke, irritation, offensive odor and the like. Therefore, further research and discussion on the application of the tobacco stems is needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for preparing fresh and sweet flavor from tobacco stem shreds, which is used for solving the problem that the tobacco flavor with fresh and sweet flavor is not prepared from tobacco stems serving as raw materials by an enzymolysis-Maillard method in the prior art.
In order to achieve the above objects and other related objects, a first aspect of the present invention provides a method for preparing a sweet flavor from cut stems of tobacco leaves, comprising the steps of:
1) Taking tobacco stem powder, adding water, stirring uniformly, and then adding fungal amylase and pectinase to carry out first-stage enzymolysis;
preferably, the tobacco stems are cut tobacco stems. The tobacco leaves are flue-cured tobacco leaves.
Preferably, the preparation method of the tobacco stem powder comprises the steps of crushing tobacco stem shreds and then sieving the crushed tobacco stem shreds to obtain the required tobacco stem powder.
More preferably, the pulverization grinds the tobacco stems into powder using a pulverizer.
more preferably, the mesh number of the screen used in the screening is more than or equal to 120 meshes. Further preferably, the mesh number of the screen used in the screening is 120 meshes. Namely, the granularity of the tobacco stalk powder is more than or equal to 120 meshes, and is preferably 120 meshes.
preferably, the water is distilled water.
Preferably, the mass ratio of the tobacco stem powder to the added water is 1: 8-12. More preferably, the mass ratio of the tobacco stem powder to the added water is 1: 10.
Preferably, the mass ratio of the tobacco stem powder to the added fungal amylase is 100: 0.05-0.15. More preferably, the mass ratio of the tobacco stem powder to the added fungal amylase is 100: 0.1.
preferably, the fungal amylase is a conventionally used fungal amylase. The fungal amylase is 1, 4-alpha-D-glucan hydrolase, also known as fungal alpha-amylase, and has a CAS number of 9001-19-8. Specifically, the fungal amylase used in the present invention is a conventional fungal amylase (Mycolase) produced by imperial (china) limited (DSM).
Preferably, the mass ratio of the tobacco stem powder to the added pectinase is 100: 0.05-0.15. More preferably, the mass ratio of the tobacco stem powder to the added pectinase is 100: 0.1.
Preferably, the pectinase is a conventionally used pectinase. The CAS number of the pectinase is 9032-75-1. Specifically, the pectinase used in the present invention is C80 pectinase (RapidaseC80 Max) produced by Disemann (China) Co., Ltd. (DSM).
preferably, the reaction conditions of the first stage enzymolysis are as follows: enzymolysis temperature: 50-60 ℃; and (3) enzymolysis time: 1-3 h. More preferably, the reaction conditions of the first stage enzymolysis are as follows: enzymolysis temperature: 55 ℃; and (3) enzymolysis time: and 2 h.
2) After the first-stage enzymolysis reaction in the step 1) is finished, adding protease for second-stage enzymolysis;
Preferably, the protease is a conventionally used protease. The CAS number of the protease is 9014-01-1. Specifically, the protease used in the present invention is a conventional protease (MaxiproNPU) produced by imperial (china) limited (DSM).
preferably, the mass ratio of the tobacco stem powder to the added protease is 100: 0.1-0.3. More preferably, the mass ratio of the tobacco stem powder to the added protease is 100: 0.2.
Preferably, the reaction conditions of the second stage enzymolysis are as follows: enzymolysis temperature: 50-60 ℃; and (3) enzymolysis time: 1-3 h. More preferably, the reaction conditions of the second stage enzymolysis are as follows: enzymolysis temperature: 55 ℃; and (3) enzymolysis time: and 2 h.
3) after the second-stage enzymolysis reaction in the step 2) is finished, inactivating enzyme of the product, and cooling to obtain the tobacco stalk enzyme
Hydrolyzing the liquid;
preferably, the reaction conditions for enzyme deactivation are as follows: enzyme deactivation temperature: 80-90 ℃; enzyme deactivation time: 10-20 min. More preferably, the enzyme deactivation reaction conditions are: enzyme deactivation temperature: 85 ℃; enzyme deactivation time: and 15 min.
Preferably, the tobacco stem enzymolysis liquid does not need to be filtered.
4) Adding glycine and the waxberry extract into the tobacco stalk enzymolysis liquid obtained in the step 3), uniformly stirring, carrying out Maillard reaction,
the required essence is obtained.
preferably, the mass ratio of the tobacco stem powder to the glycine is 100: 2-4. More preferably, the mass ratio of the tobacco stem powder to the glycine is 100: 3.
Preferably, the mass ratio of the tobacco stem powder to the waxberry extract is 10: 1-2. More preferably, the mass ratio of the tobacco stem powder to the waxberry extract is 10: 1.4-1.7.
Preferably, the waxberry extract is a waxberry extract conventionally used, which is extracted from fruits, rhizomes, leaves, etc. of waxberries. Specifically, the bayberry extract used in the present invention is produced by Haikou Nishima perfumery Co. The mass percentage concentration of the waxberry components in the waxberry extract accounts for 80-100% of the total mass of the waxberry extract.
Preferably, the conditions of the maillard reaction are: reaction temperature: 90-110 ℃; reaction time: 2-4 h. More preferably, the maillard reaction conditions are: reaction temperature: 100 ℃; reaction time: and 3 h.
Preferably, the essence is an essence for cigarettes, and has a fresh and sweet aroma.
In a second aspect, the invention provides a fresh and sweet aroma prepared by the above method.
the third aspect of the invention provides application of the fresh and sweet aroma essence in tobacco leaves.
preferably, the tobacco leaves are flue-cured tobacco leaves.
The invention provides a use method of fresh and sweet essence, which is characterized in that after the essence is diluted by alcohol, the essence diluent and the flue-cured tobacco leaves are weighed according to a proportion, and the essence diluent is uniformly sprayed in the flue-cured tobacco leaves.
preferably, the alcohol is edible alcohol, which is an aqueous solution containing anhydrous ethanol in conventional proportions. More preferably, the alcohol is edible alcohol containing 70% by volume of anhydrous ethanol.
preferably, the essence diluent is an ethanol solution containing essence in a conventional proportion. More preferably, the essence in the essence diluent accounts for 10% by mass.
preferably, the adding proportion of the essence diluent to the flue-cured tobacco leaf group is a conventional mass ratio. More preferably, the mass ratio of the essence diluent to the flue-cured tobacco leaf group is 5: 1000.
preferably, the flue-cured tobacco leaf is a flue-cured tobacco leaf of yunan yuxi brand cigarette.
Preferably, the spraying is performed using a medical sprayer.
as described above, according to the method for preparing the fresh and sweet flavor from the cut stems of the tobacco leaves, provided by the invention, the precursor of the reactive flavor is prepared through enzymolysis reaction of the cut stems of the tobacco leaves, and the tobacco flavor with the fresh and sweet flavor is obtained through Maillard reaction by adding the waxberry extract. The tobacco essence prepared by the invention takes tobacco leaves and stems as raw materials, and has the advantages of rich raw material sources, simple process and easy operation. Compared with the traditional flavoring essence, the tobacco essence prepared by the invention has obvious fresh and sweet aroma, can obviously improve the aroma quality of cigarettes, enrich the tobacco aroma, enrich the smoke, promote the production of body fluid and increase the sweetness, improves and harmonizes the smoking quality of the cigarettes, can effectively improve the defects of insufficient tobacco aroma, weak smoke, irritation, bitter taste and the like of the existing common cigarettes, and can be widely applied to the field of the cigarette essence.
drawings
Fig. 1 shows a GC map of an enzymatic hydrolysate of tobacco stems obtained by performing only an enzymatic hydrolysis reaction on the tobacco stems according to the present invention.
Fig. 2 shows a GC-spectrum of the essence (formula 11) obtained by performing enzymolysis-maillard reaction on the tobacco stems of the present invention without adding the waxberry extract.
Fig. 3 shows a GC-spectrum of the waxberry extract-added essence (formula 15) obtained by subjecting tobacco stems to enzymolysis-maillard reaction in the present invention.
FIG. 4 shows a GC spectrum of the tobacco stem extract in the present invention.
Figure 5 shows the GC-spectrum of Hongda smoke cream.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It should be understood that the processing equipment or devices not specifically mentioned in the following examples are conventional in the art; all pressure values and ranges refer to relative pressures and the apparatus or reagents used in the present invention are conventional in the art and are commercially available.
furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
Example 1
the tobacco stem shreds are crushed and sieved by a sieve with the mesh size of more than or equal to 120 to obtain the required tobacco stem powder. Adding distilled water into a certain amount of tobacco stalk powder, stirring, adding fungal amylase and C80 pectinase, and performing first-stage enzymolysis at 50-60 deg.C for 1-3 h. Wherein the mass ratio of the tobacco stalk powder to the distilled water is 1: 8-12; the mass ratio of the tobacco stem powder to the added fungal amylase is 100: 0.05-0.15; the mass ratio of the tobacco stem powder to the added C80 pectinase is 100: 0.05-0.15.
And then adding protease for enzymolysis for the second stage at 50-60 ℃ for 1-3h, wherein the mass ratio of the tobacco stem powder to the protease is 100: 0.1-0.3. Inactivating enzyme of the enzymolysis product at 80-90 deg.C for 10-20min, and cooling to obtain tobacco stalk enzymolysis solution. Wherein the total enzymolysis reaction time of the first stage enzymolysis and the second stage enzymolysis is 2-6 h.
And finally, adding glycine and the waxberry extract into the tobacco stalk enzymolysis liquid, uniformly stirring, and carrying out Maillard reaction for 2-4h at 90-110 ℃ to obtain the required essence. Wherein the mass ratio of the tobacco stalk powder to the glycine is 100: 2-4; the mass ratio of the tobacco stem powder to the waxberry extract is 10: 1-2.
When the essence is used in tobacco leaves, diluting the essence with edible alcohol containing 70% of absolute ethyl alcohol by volume percent to prepare essence diluent accounting for 10% of the essence by mass percent, and adding the essence diluent and the flue-cured tobacco leaves according to the mass ratio of 5: 1000, weighing the essence diluent and the flue-cured tobacco leaves, and uniformly spraying the essence diluent in the flue-cured tobacco leaves by adopting a medical sprayer.
Example 2
In the process of preparing the essence by carrying out enzymolysis-Maillard reaction on cut stems of tobacco leaves, the enzymolysis reaction temperature is discussed under the condition of not adding red bayberry extract, so that the influence of different enzymolysis reaction temperatures on the aroma of a reaction product is obtained, and the optimal enzymolysis reaction temperature is judged, and the specific preparation process is as follows.
The tobacco stem shreds are sieved by a 120-mesh sieve after being crushed to obtain the required tobacco stem powder. Taking 10.00g of tobacco stalk powder, adding 100.00g of distilled water, uniformly stirring, adding 0.01g of fungal amylase and 0.01g C80 g of pectinase, and carrying out first-stage enzymolysis for 2 hours at different enzymolysis reaction temperatures.
Then, 0.02g of protease is added to carry out second-stage enzymolysis for 2 hours at different enzymolysis reaction temperatures of 55 ℃, enzyme deactivation is carried out on the enzymolysis products for 15 minutes at 85 ℃, and cooling is carried out to obtain the tobacco stem enzymolysis liquid. Wherein the total enzymolysis reaction time of the first stage enzymolysis and the second stage enzymolysis is 4 h. The enzymolysis reaction temperature is 50 ℃, 55 ℃ and 60 ℃.
And finally, adding 0.30g of glycine into the tobacco stalk enzymolysis liquid, uniformly stirring, and carrying out Maillard reaction for 3 hours at 100 ℃ to obtain formulas 1, 2 and 3 of essences 1#, 2# and 3#, and essences 1#, 2# and 3#, respectively, as shown in Table 1.
As can be seen from Table 1, the temperature of the enzymolysis reaction in the formula 1 is controlled to be about 50 ℃, and the product is sprayed on the flue-cured tobacco leaves of Yuxi brand cigarettes in Yunnan province, so that the tobacco leaves are not full in aroma, have miscellaneous gas and are not coordinated with the tobacco aroma after being smoked by a spice maker; the enzymolysis reaction temperature in the formula 2 is controlled to be about 55 ℃, and the sweet aroma is still a little weak point through suction, but the smoke is very thick and is fuller than the previous smoke; the enzymolysis reaction temperature in the formula 3 is controlled to be about 60 ℃, and the tobacco fragrance is poor, has scorched bitter and is incompatible with the tobacco fragrance through suction. The comparison of the above 3 formulas shows that the enzymolysis reaction temperature in the formula 2 is controlled at 55 ℃, which is the optimal enzymolysis reaction temperature, and the enzymolysis temperature is the maximum activity of the enzyme, so that the whole aroma is full, the smoke is dense, but the aroma is slightly sweet, which may be related to the reaction time and the blending in the later period.
TABLE 1 Effect of different enzymolysis reaction temperatures on the aroma of the reaction products
Example 3
In the process of preparing the essence by carrying out enzymolysis-Maillard reaction on cut stems of tobacco leaves, the reaction time in the enzymolysis reaction is discussed under the condition of not adding the waxberry extract, so that the influence of different enzymolysis reaction times on the aroma of a reaction product is obtained, and the optimal enzymolysis reaction time is judged, wherein the specific preparation process is as follows.
The tobacco stem shreds are sieved by a 120-mesh sieve after being crushed to obtain the required tobacco stem powder. Taking 10.00g of tobacco stalk powder, adding 100.00g of distilled water, stirring uniformly, adding 0.01g of fungal amylase and 0.01g C80 of pectinase, and performing first-stage enzymolysis for 1h, 2h and 3h at 55 ℃.
then, 0.02g protease is added to carry out second-stage enzymolysis for 1h, 2h and 3h at 55 ℃, the enzymolysis product is subjected to enzyme deactivation for 15min at 85 ℃, and then cooling is carried out, so as to obtain the tobacco stem enzymolysis liquid. Wherein, the total enzymolysis reaction time of the first stage enzymolysis and the second stage enzymolysis is 2h, 4h and 6h respectively.
and finally, adding 0.30g of glycine into the tobacco stalk enzymolysis liquid, uniformly stirring, and carrying out Maillard reaction for 3 hours at 100 ℃ to obtain formulas 4, 5 and 6 of essences 4#, 5# and 6#, and essences 4#, 5# and 6#, respectively, as shown in Table 2.
As can be seen from table 2, the total enzymatic hydrolysis reaction time in formula 4 was controlled at about 2 hours, and the product was sprayed on the flue-cured tobacco leaves of yuxi brand cigarettes, and after being smoked by a perfumer, the fragrance was found to be insufficient and incompatible with the tobacco fragrance; the total enzymolysis reaction time in the formula 5 is controlled to be about 4 hours, and the sweet note is a slight weakness through suction, but the smoke is very thick and is fuller than the previous smoke; the total enzymolysis reaction time in the formula 6 is controlled to be about 6 hours, and the smoking is poor in fragrance, miscellaneous gas exists, and the aftertaste is dry and astringent. The comparison of the above 3 formulas shows that the total enzymolysis reaction time in the formula 5 is controlled to be 4h, which is the optimal enzymolysis reaction time, and the sweet and fragrant note of the obtained product is still slightly weak, so that some raw materials such as fruit extracts and the like need to be added in the Maillard reaction process, so that the sweet and fragrant smell is increased, and the fragrance is more harmonious and full.
TABLE 2 Effect of different enzymatic reaction times on the aroma of the reaction products
example 4
In the process of preparing the essence by carrying out enzymolysis-Maillard reaction on cut stems of tobacco leaves, the reaction temperature in the Maillard reaction is discussed under the condition of not adding a waxberry extract, so that the influence of different Maillard reaction temperatures on the aroma of a reaction product is obtained, the optimal Maillard reaction temperature is judged, and the specific preparation process is as follows.
the tobacco stem shreds are sieved by a 120-mesh sieve after being crushed to obtain the required tobacco stem powder. Taking 10.00g of tobacco stalk powder, adding 100.00g of distilled water, stirring uniformly, adding 0.01g of fungal amylase and 0.01g C80 g of pectinase, and performing first-stage enzymolysis for 2h at 55 ℃.
Then, 0.02g of protease is added to carry out second-stage enzymolysis for 2 hours at 55 ℃, the enzymolysis products are subjected to enzyme deactivation for 15min at 85 ℃, and then cooling is carried out, so as to obtain the tobacco stem enzymolysis liquid. Wherein, the total enzymolysis reaction time of the first stage enzymolysis and the second stage enzymolysis is 4h respectively.
And finally, adding 0.30g of glycine into the tobacco stalk enzymolysis liquid, uniformly stirring, and carrying out Maillard reaction for 3 hours at different reaction temperatures to obtain formulas 7, 8 and 9 of essences 7#, 8# and 9#, and essences 7#, 8# and 9#, respectively, as shown in Table 3. Wherein the Maillard reaction temperature is 90 ℃, 100 ℃ and 110 ℃.
As can be seen from table 3, in formula 7, the maillard reaction temperature was controlled at about 90 ℃, and by spraying the product onto the flue-cured tobacco leaves of yuxi brand cigarettes in yunan, after smoking by a perfumer, the fragrance was found to be less than full, there was miscellaneous gas, and the fragrance was not coordinated with the tobacco fragrance; in the formula 8, the Maillard reaction temperature is controlled to be about 100 ℃, and the sweet note is a slight weakness through suction, but the smoke is very thick and is fuller than the previous smoke; in the formula 9, the Maillard reaction temperature is controlled to be about 110 ℃, and the aroma is poor and the smell is bitter through suction. The comparison of the above 3 formulations shows that the Maillard reaction temperature in formulation 8 is controlled at 100 ℃, which is the optimum Maillard reaction temperature.
TABLE 3 Effect of different Maillard reaction temperatures on the aroma of the reaction products
Example 5
In the process of preparing the essence by carrying out enzymolysis-Maillard reaction on cut stems of tobacco leaves, the reaction time in the Maillard reaction is discussed under the condition of not adding a waxberry extract, so that the influence of different Maillard reaction times on the aroma of reaction products is obtained, the optimal Maillard reaction time is judged, and the specific preparation process is as follows.
The tobacco stem shreds are sieved by a 120-mesh sieve after being crushed to obtain the required tobacco stem powder. Taking 10.00g of tobacco stalk powder, adding 100.00g of distilled water, stirring uniformly, adding 0.01g of fungal amylase and 0.01g C80 g of pectinase, and performing first-stage enzymolysis for 2h at 55 ℃.
Then, 0.02g of protease is added to carry out second-stage enzymolysis for 2 hours at 55 ℃, the enzymolysis products are subjected to enzyme deactivation for 15min at 85 ℃, and then cooling is carried out, so as to obtain the tobacco stem enzymolysis liquid. Wherein, the total enzymolysis reaction time of the first stage enzymolysis and the second stage enzymolysis is 4h respectively.
And finally, adding 0.30g of glycine into the tobacco stalk enzymolysis liquid, uniformly stirring, and carrying out Maillard reaction at 100 ℃ for different time periods to obtain formulas 10, 11 and 12 of essences 10#, 11# and 12#, and essences 10#, 11# and 12#, respectively, as shown in Table 4. Wherein the Maillard reaction time is 2h, 3h and 4h respectively.
TABLE 4 Effect of different Maillard reaction times on the fragrance of the reaction products
as can be seen from table 4, in the formula 10, the maillard reaction time is controlled to about 2 hours, and the product is sprayed on the flue-cured tobacco leaves of yuxi brand cigarettes in Yunnan, and after being smoked by a spice maker, the fragrance is not full and is not coordinated with the tobacco fragrance; the Maillard reaction time in the formula 11 is controlled to be about 3h, and the sweet note is a slight weakness through suction, but the smoke is very thick and is fuller than the previous smoke; the Maillard reaction time in the formula 12 is controlled to be about 4h, and the aroma is poor through suction, and the obvious bitter taste is generated. The comparison of the above 3 formulas shows that the optimal Maillard reaction time is 3 hours in formula 11.
Example 6
In the process of preparing the essence by performing enzymolysis-Maillard reaction on cut stems of tobacco leaves, the waxberry extract can be added in order to increase the fresh and sweet aroma of the essence, so that the dosage of the waxberry extract needs to be discussed, the influence of different dosages of the waxberry extract on the aroma of a reaction product is obtained, and the optimal dosage of the waxberry extract is determined, and the specific preparation process is as follows.
The tobacco stem shreds are sieved by a 120-mesh sieve after being crushed to obtain the required tobacco stem powder. Taking 10.00g of tobacco stalk powder, adding 100.00g of distilled water, stirring uniformly, adding 0.01g of fungal amylase and 0.01g C80 g of pectinase, and performing first-stage enzymolysis for 2h at 55 ℃.
Then, 0.02g of protease is added to carry out second-stage enzymolysis for 2 hours at 55 ℃, the enzymolysis products are subjected to enzyme deactivation for 15min at 85 ℃, and then cooling is carried out, so as to obtain the tobacco stem enzymolysis liquid. Wherein, the total enzymolysis reaction time of the first stage enzymolysis and the second stage enzymolysis is 4h respectively.
And finally, adding 0.30g of glycine and the waxberry extracts with different contents into the tobacco stalk enzymolysis liquid, uniformly stirring, and carrying out Maillard reaction for 3 hours at 100 ℃ to obtain formulas 13, 14, 15 and 16 of essences 13#, 14#, 15# and 16# respectively, wherein the formulas are shown in Table 5. Wherein the dosage of fructus Myricae Rubrae extract is 1g, 1.4g, 1.7g, and 2g respectively.
TABLE 5 Effect of the amount of different waxberry extracts added on the aroma of the reaction products
As can be seen from table 5, the mass ratio of the cut tobacco stem powder to the red bayberry extract in the formula 13 is controlled to be about 10:1, the product is sprayed on the flue-cured tobacco leaves of the yuxi brand cigarettes, and after the tobacco leaves are smoked by a flavorist, the fragrance is not sufficiently round and the sweet fragrance is weak; the mass ratio of the tobacco leaf cut stem powder to the red bayberry extract in the formula 14 is controlled to be about 10:1.4, smoke is dense through suction, and the sweet and fragrant note is higher than that of the formula 13; the mass ratio of the tobacco leaf cut stem powder to the waxberry extract in the formula 15 is controlled to be about 10:1.7, and through suction, the smoke is very thick, the sweet and fragrant note is better, and the effects of promoting the production of body fluid and returning sweet are achieved; the mass ratio of the tobacco leaf cut stem powder to the red bayberry extract in the formula 16 is controlled to be about 10:2, and the tobacco leaf cut stem powder has weak fragrance, obvious caramel smell and miscellaneous smell by suction. The comparison of the 4 formulas shows that the quality ratio of the cut tobacco stem powder to the red bayberry extract is controlled to be 10: 1.4-10: 1.7, so that the best red bayberry extract dosage can be obtained.
example 7
In order to examine the influence of the preparation method on the quality of the essence, the tobacco stem extract, the tobacco stem enzymolysis liquid obtained only through enzymolysis reaction, the essence without the waxberry extract obtained through enzymolysis-Maillard reaction, the essence with the waxberry extract obtained through enzymolysis-Maillard reaction and the Hongda tobacco paste with the best quality are respectively prepared and compared.
Firstly, preparing a tobacco stem extracting solution: the tobacco stem is crushed and sieved by a 120-mesh sieve to obtain the required tobacco stem powder. Taking 10.00g of tobacco stem powder, adding 100.00g of distilled water, stirring uniformly, and then extracting for 4h at 70 ℃ to obtain a tobacco stem extracting solution.
Secondly, preparing tobacco stalk enzymolysis liquid obtained only through enzymolysis reaction: the tobacco stem is crushed and sieved by a 120-mesh sieve to obtain the required tobacco stem powder. Taking 10.00g of tobacco stalk powder, adding 100.00g of distilled water, stirring uniformly, adding 0.01g of fungal amylase and 0.01g C80 g of pectinase, and performing first-stage enzymolysis for 2h at 55 ℃. Adding 0.02g protease, performing second stage enzymolysis at 55 deg.C for 2 hr, inactivating enzyme at 85 deg.C for 15min, cooling, filtering, and collecting supernatant to obtain tobacco stalk enzymolysis solution. Wherein, the total enzymolysis reaction time of the first stage enzymolysis and the second stage enzymolysis is 4h respectively.
Then, preparing the essence which is obtained by enzymolysis-Maillard reaction and is not added with the waxberry extract: the preparation was carried out as in formulation 11 of example 5.
then preparing the essence which is obtained by enzymolysis-Maillard reaction and is added with the waxberry extract: the preparation was the same as for formulation 15 in example 6.
finally, Hongda cigarette cream produced by Haikou Nishima perfumery Co., Ltd was directly taken as a reaction solution.
The obtained reaction liquid is respectively subjected to GC-MS detection, the detection results of the tobacco stalk extracting solution are shown in a figure 4 and a table 6, the detection results of the tobacco stalk enzymolysis liquid obtained only through enzymolysis reaction are shown in a figure 1 and a table 6, the detection results of the essence without added peanut powder obtained through enzymolysis-Maillard reaction are shown in a figure 2 and a table 6, the detection results of the essence with added peanut powder obtained through enzymolysis-Maillard reaction are shown in a figure 3 and a table 6, and the detection results of the Hongda tobacco paste are shown in a figure 5 and a table 6.
Wherein, the GC-MS detection conditions are as follows:
GC conditions were as follows: a chromatographic column: INNOWAX, 60 m.times.0.25 mm.times.0.25 μm; carrier gas: he; flow rate of carrier gas: 1 mL/min; sample introduction mode: no flow diversion; sample inlet temperature: 250 ℃; temperature rising procedure: keeping at 40 deg.C for 6min, heating to 100 deg.C at 3 deg.C/min, and heating to 230 deg.C at 5 deg.C/min for 10 min;
MS conditions: an ion source: an EI source; ion source temperature: 230 ℃; electron energy: 70 eV; mass scan range: 30-350 amu; scanning mode: and (4) full scanning.
TABLE 6 names and contents of perfume ingredients in different reaction solutions
as can be seen from table 6, (1) compared with the tobacco stalk enzymatic hydrolysate, the tobacco stalk enzymatic hydrolysis-maillard reaction essence, the tobacco stalk enzymatic hydrolysis-maillard reaction and the addition of the waxberry essence and the red big tobacco paste, the types of aroma substances in the tobacco stalk extract are obviously reduced, and the content is lower, which indicates that the aroma quality of the raw material cut stems is lower, and the raw material cut stems cannot be directly used as cigarettes. (2) After the raw material cut stems are subjected to enzymolysis and Maillard reaction, the types of tobacco fragrance are obviously increased, the contents of components of the roasted fragrance and the tobacco fragrance are increased, and the contents of green smell, peculiar smell and low-grade tobacco fragrance are reduced, which shows that after the enzymolysis and the Maillard reaction, the fragrant substances of the raw material cut stems are obviously increased, and the defects of insufficient tobacco fragrance, peculiar smell, miscellaneous gas and the like in the tobacco essence are overcome. (3) The waxberry extract is added into the Maillard reaction of the cut stems, so that the content of fresh and sweet components is obviously increased, the contents of baking fragrance and aroma components are not reduced but slightly increased, and the enzymatic hydrolysis-Maillard reaction liquid of the cut stems of the tobacco leaves has obvious fresh and sweet fragrance and baking fragrance, can effectively improve the aroma quality of the cigarettes, enrich the tobacco fragrance, promote the secretion of saliva or body fluid and increase the sweetness, and has the effect of improving the smoking quality of the cigarettes.
therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (4)
1. the fresh and sweet aroma essence is prepared by a method for preparing the fresh and sweet aroma essence according to cut stems of tobacco leaves, and comprises the following steps:
1) Taking tobacco stem powder, adding water, stirring uniformly, and then adding fungal amylase and pectinase to carry out first-stage enzymolysis;
2) after the first-stage enzymolysis reaction in the step 1) is finished, adding protease for second-stage enzymolysis;
3) After the second-stage enzymolysis reaction in the step 2) is finished, deactivating enzyme of the product, and cooling to obtain tobacco stem enzymolysis liquid;
4) Adding glycine and the waxberry extract into the tobacco stalk enzymolysis liquid obtained in the step 3), uniformly stirring, and carrying out Maillard reaction to obtain the required essence;
In step 1), any one or more of the following conditions are included:
A1) The mass ratio of the tobacco stalk powder to the added water is 1: 8-12;
A2) the mass ratio of the tobacco stem powder to the added fungal amylase is 100: 0.05-0.15;
A3) The mass ratio of the tobacco stem powder to the added pectinase is 100: 0.05-0.15;
A4) The reaction conditions of the first-stage enzymolysis are as follows: enzymolysis temperature: 50-60 ℃; and (3) enzymolysis time: 1-3 h;
step 2), any one or more of the following conditions are included:
B1) the mass ratio of the tobacco stem powder to the added protease is 100: 0.1-0.3;
B2) The reaction conditions of the second stage enzymolysis are as follows: enzymolysis temperature: 50-60 ℃; and (3) enzymolysis time: 1-3 h;
In the step 3), the enzyme deactivation reaction conditions are as follows: enzyme deactivation temperature: 80-90 ℃; enzyme deactivation time: 10-20 min;
In the step 4), the step of mixing the raw materials,
C1) The mass ratio of the tobacco stem powder to the glycine is 100: 2-4;
C2) The mass ratio of the tobacco stem powder to the waxberry extract is 10: 1-2;
C3) The conditions of the Maillard reaction are as follows: reaction temperature: 90-110 ℃; reaction time: 2-4 h;
in the step 1), the preparation method of the tobacco stem powder comprises the steps of crushing tobacco leaf cut stems and sieving the crushed tobacco leaf cut stems to obtain the required tobacco stem powder;
the granularity of the tobacco stalk powder is more than or equal to 120 meshes;
The fungal amylase is a fungal amylase with CAS number 9001-19-8; the pectinase is a pectinase with CAS number of 9032-75-1; the protease is the protease with CAS number 9014-01-1.
2. A method for preparing fresh and sweet aroma essence from tobacco stem shreds comprises the following steps:
1) Taking tobacco stem powder, adding water, stirring uniformly, and then adding fungal amylase and pectinase to carry out first-stage enzymolysis;
2) After the first-stage enzymolysis reaction in the step 1) is finished, adding protease for second-stage enzymolysis;
3) after the second-stage enzymolysis reaction in the step 2) is finished, deactivating enzyme of the product, and cooling to obtain tobacco stem enzymolysis liquid;
4) Adding glycine and the waxberry extract into the tobacco stalk enzymolysis liquid obtained in the step 3), uniformly stirring, and carrying out Maillard reaction to obtain the required essence;
In step 1), any one or more of the following conditions are included:
A1) The mass ratio of the tobacco stalk powder to the added water is 1: 8-12;
A2) the mass ratio of the tobacco stem powder to the added fungal amylase is 100: 0.05-0.15;
A3) The mass ratio of the tobacco stem powder to the added pectinase is 100: 0.05-0.15;
A4) The reaction conditions of the first-stage enzymolysis are as follows: enzymolysis temperature: 50-60 ℃; and (3) enzymolysis time: 1-3 h;
Step 2), any one or more of the following conditions are included:
B1) the mass ratio of the tobacco stem powder to the added protease is 100: 0.1-0.3;
B2) the reaction conditions of the second stage enzymolysis are as follows: enzymolysis temperature: 50-60 ℃; and (3) enzymolysis time: 1-3 h;
in the step 3), the enzyme deactivation reaction conditions are as follows: enzyme deactivation temperature: 80-90 ℃; enzyme deactivation time: 10-20 min;
In the step 4), the step of mixing the raw materials,
C1) The mass ratio of the tobacco stem powder to the glycine is 100: 2-4;
C2) The mass ratio of the tobacco stem powder to the waxberry extract is 10: 1-2;
C3) The conditions of the Maillard reaction are as follows: reaction temperature: 90-110 ℃; reaction time: 2-4 h;
in the step 1), the preparation method of the tobacco stem powder comprises the steps of crushing tobacco leaf cut stems and sieving the crushed tobacco leaf cut stems to obtain the required tobacco stem powder;
The granularity of the tobacco stalk powder is more than or equal to 120 meshes;
the fungal amylase is a fungal amylase with CAS number 9001-19-8; the pectinase is a pectinase with CAS number of 9032-75-1; the protease is the protease with CAS number 9014-01-1.
3. use of a fresh and sweet aroma according to claim 1 in tobacco leaves.
4. The use method of the fresh and sweet aroma essence according to claim 1, wherein the essence is diluted by alcohol, and then the essence diluent and the flue-cured tobacco leaf are weighed according to a certain proportion, and the essence diluent is uniformly sprayed in the flue-cured tobacco leaf.
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| CN104351944A (en) * | 2014-10-22 | 2015-02-18 | 浙江中烟工业有限责任公司 | Tobacco perfuming agent prepared through molecular distillation treatment of extractum obtained through Maillard reaction from inferior tobacco leaves, preparation method and application of tobacco perfuming agent |
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| CN104152268A (en) * | 2014-08-06 | 2014-11-19 | 浙江中烟工业有限责任公司 | Tobacco perfume material prepared by compound enzyme enzymolysis coupling Maillard reaction, and preparation method and application of tobacco perfume material |
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| CN104351944A (en) * | 2014-10-22 | 2015-02-18 | 浙江中烟工业有限责任公司 | Tobacco perfuming agent prepared through molecular distillation treatment of extractum obtained through Maillard reaction from inferior tobacco leaves, preparation method and application of tobacco perfuming agent |
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