CN116235984A - Flavor for tobacco prepared by using tobacco rod and its preparation method and application - Google Patents

Abstract

The present application discloses a method for preparing tobacco spices by using tobacco rods, which includes the following steps: using enzymes to treat the tobacco rods, drying the residue, grinding, dissolving in organic solvents, extracting, filtering, and adding acid to precipitate lignin , separated, and dried to obtain enzymatic lignin; treating the enzymatic lignin with yew xylobacter to obtain modified lignin; performing thermal cracking on the modified lignin to obtain tobacco flavor. The present application also provides tobacco spices and their uses. In this application, tobacco rods are used as the starting material to prepare flavors for tobacco, and glycoside latent aroma compounds are obtained by enzymatic hydrolysis, modification and thermal cracking of tobacco rods, which can be added to cigarettes to obtain the unique aroma of cigarettes. Make full use of resources; more alcohols, phenols, and ketones in spices are retained, and after being added to cigarettes, they can be burned to release the unique aroma of cigarettes, which can highlight the aroma style of cigarettes, increase the richness of aroma, and make the taste softer, improving The roundness and contentment of the smoke.

Description

Flavor for tobacco prepared by using tobacco rod and its preparation method and application

technical field

The present application relates to the technical field of tobacco additives, in particular to a flavoring for tobacco prepared from tobacco rods and its preparation method and application.

Background technique

Tobacco sheet is a sheet similar to tobacco made from tobacco by-products and waste (stalks, chips, etc.) by adding tobacco extract, forming aids, fillers and spices, and is reused in the cigarette industry . After years of development, the research and development and production of tobacco sheets have made great progress, but the aroma and taste of cigarettes are still in an unstable state. In order to meet the quality requirements of tobacco product processing and production, and to coordinate the miscellaneous gas of tobacco itself, it is necessary to make up for the lack of fragrance by adding flavors and fragrances, coordinate and improve the aroma and taste of tobacco.

At present, the preparation of flavors and fragrances used in cigarettes mainly includes Chinese herbal medicine natural plant flavor extracts, latent aroma compounds and the like. At present, the research progress of extracting spices from natural products focuses on traditional Chinese medicinal materials, including ginseng, Cordyceps sinensis, Ganoderma lucidum, Shennong chrysanthemum, etc. Latent aroma compounds are generally divided into two types, namely glycoside latent aroma compounds and sugar amine latent aroma compounds. The latent aroma compound is stable at room temperature, and can be decomposed to release aroma when heated. When smoking, the surface temperature of the cigarette butt is 200-300°C, and the center temperature is as high as 700-800°C. The latent aroma compound can be kept stable at 200-300°C, and it will decompose and release aroma at 700-800°C, which has obvious effects on cigarettes. The role of flavoring and flavoring has been widely used in cigarette processing.

However, the existing latent aroma compounds are usually obtained through synthesis, which is easy to introduce unnecessary chemical components into tobacco flavors and bring other unnecessary effects on smoking.

Contents of the invention

In order to solve the above-mentioned technical problems, the first object of the present invention is to provide a method for preparing tobacco spices by using tobacco rods; the second object of the present invention is to provide the tobacco flavors prepared by the above method; the third object of the present invention One purpose is to provide the application of the above-mentioned tobacco spices in tobacco sheets. In this application, tobacco rods are used as starting materials to prepare flavors for tobacco, and glycoside latent aroma compounds are obtained by enzymatic hydrolysis, modification and thermal cracking of tobacco rods, which can be added to cigarettes to obtain the unique aroma of cigarettes. Make full use of resources; more alcohols, phenols, and ketones in spices are retained, and after being added to cigarettes, Maillard reaction will occur when they are burned, releasing the unique aroma of cigarettes, which can highlight the aroma style of cigarettes and increase the richness of aroma. It also softens the taste and improves the roundness and satisfaction of the smoke.

The technical scheme provided by the invention is as follows:

A method for preparing tobacco spices by using a tobacco rod, comprising the following steps:

Treat tobacco stems with enzymes, dry the residue, grind, dissolve in an organic solvent, extract, filter, add acid to precipitate lignin, separate, and dry to obtain enzymatic lignin;

Treating enzymatically hydrolyzed lignin with yew Xylella cerevisiae to obtain modified lignin;

The modified lignin is pyrolyzed to obtain the tobacco flavor.

Preferably, before using the enzyme treatment, the step of grinding the tobacco rod is also included.

Preferably, the tobacco rods are ball milled for 48-72 hours.

Preferably, the organic solvent is any one of benzyl alcohol, benzene, and phenethyl alcohol.

Preferably, the enzymes are cellulases and hemicellulases.

Preferably, the mass ratio of cellulase and hemicellulase is (2-3):1.

Preferably, the mass ratio of the enzyme to the tobacco rod is 240-450U/g tobacco rod; the temperature of the enzyme-treated tobacco rod is 40-55°C, and the time is 6-8 days.

Preferably, the residue is dried at 50-60°C, ground to 100-200 mesh, dissolved in an organic solvent, extracted at 65-75°C for 2-4h, filtered, added acid, and kept at 60-70°C for 0.5-1h The lignin is precipitated, centrifuged, dried at 60-70°C, and ground to 40-60 mesh to obtain enzymatic lignin.

Preferably, the enzymatic lignin is treated with the first-grade seed liquid of the yew wood fungus; the first-grade seed liquid of the yew woody fungus is obtained by the following method:

Select the yew woody fungus, inoculate it on the PDB medium, and cultivate it for 7-10 days under the environment of 27-28° C. on a shaker with a rotating speed of 180-200 r/min to obtain the first-grade seed liquid of the yew woody tooth fungus.

Preferably, the ratio of the primary seed liquid of A. yewensis to the enzymatic lignin is 1 ml of the primary seed liquid of A. yew: (1-3) g enzymatic lignin.

Preferably, after mixing the first-grade seed liquid of A. yew yew and the enzymatic lignin, it is cultured statically at 27-28° C., and after 25-30 days of cultivation, it is dried at 60-70° C. to obtain the modified lignin.

Preferably, the modified lignin is pyrolyzed at 400-450° C. and kept for 30-60 s to obtain tobacco flavor.

Preferably, the initial temperature is 60°C, and the heating rate is 5-6°C/ms.

Flavor for tobacco prepared by the method described in any one of the above.

In the application of the above-mentioned tobacco spices in tobacco sheets, the tobacco flavors are added to the tobacco sheets in the form of fillers, and the mass ratio of the tobacco flavors to the tobacco sheets is (5-15):100.

Tobacco (scientific name: Nicotiana tabacum L.) is a plant of the genus Nicotiana in the family Solanaceae, an annual or limited perennial herb, all covered with glandular hairs; the roots are thick and strong. Tobacco stem refers to the stalk part of the tobacco plant other than the tobacco leaves.

The present application provides a method for preparing tobacco flavors by using tobacco rods. The tobacco rods are used as starting materials to prepare tobacco flavors, and glycoside latent substances are obtained by enzymatic hydrolysis, modification and thermal cracking of tobacco rods. Aroma compounds, these glycoside latent aroma compounds are used as tobacco spices, and can be added to cigarettes to obtain the unique aroma of cigarettes. The method provided by this application uses tobacco rods as the preparation material to make full use of resources; and the prepared tobacco flavors, alcohols, phenols and ketones are more retained, and the purity and yield are high, and the combustion will be reduced after being added to the cigarette. The Maillard reaction occurs to release the unique aroma of cigarettes, which can highlight the aroma style of cigarettes, increase the richness of aroma, soften the taste, and improve the roundness and satisfaction of smoke. Since the spice does not affect the bonding between the tobacco plant fibers, the loss of the strength of the tobacco sheet is avoided.

To sum up, the method provided by the present application has simple operation, low cost, remarkable effect, and can make high utilization of resources.

Specifically, in the method provided by this application, the tobacco rod is firstly subjected to enzymatic hydrolysis, carbohydrates such as cellulose and hemicellulose in the tobacco rod are decomposed into monosaccharides and dissolved, and only lignin is retained; and the residue is dried, ground, Dissolve in an organic solvent, extract, filter, add acid to precipitate lignin, separate, and dry to obtain purified enzymatic lignin, so that there are almost no impurities in the obtained enzymatic lignin, which is beneficial to subsequent thermal cracking No by-products are generated; and then the enzymatic lignin is modified by the yew wood bacteria, which can not only reduce the enzymatic resistance of the raw material, but also change its pyrolysis properties.

The thermal cracking of lignin is affected by different bond types and substituents. After being treated with enzymes and Taxus sp., the bond types and substituents can be selectively retained, and then the aromatics that are beneficial to the preparation of tobacco flavors can be obtained by controlling the thermal cracking temperature. compound. The method adopted in the invention can selectively retain the glycoside latent aroma compounds which are beneficial to the preparation of tobacco flavors, and retain the flavor components suitable for tobacco.

Lignin is a polymer compound with a three-dimensional spatial structure that is formed by linking phenylpropane structural units through ether bonds and carbon-carbon bonds in the plant cell wall and intercellular layer. Among the natural polymer compounds in nature, its The content of lignin is second only to cellulose and chitin. As people pay more attention to the problem of resource scarcity, the development and utilization of lignin is also paid more and more attention. However, due to the mutual immersion of lignin, cellulose, and hemicellulose in plants, it is difficult to completely separate and extract lignin. In recent years, with the continuous development and utilization of biomass resources, such as the development of bioethanol, a large amount of enzymatic biomass resource waste has been produced, and it was subsequently found that these waste materials contain a large amount of lignin, which is called enzymatic hydrolysis. Lignin. Since it is not damaged by high temperature and chemicals, the enzymatic lignin basically retains the chemical activity of lignin, so using the enzymatic lignin from tobacco stems as the initial reactant can better retain the original chemical activity of lignin.

After the enzymatic lignin is obtained, it is modified by the yew woody fungus. The yew wood fungus is a kind of fungi that can effectively modify aromatic compounds such as lignin. The pyrolysis properties of the lignin modified by the yew wood tooth fungus will change, The efficiency of lignin pyrolysis can be improved, and the types and yields of products will also be significantly affected. Finally, the modified lignin is pyrolyzed to obtain the tobacco flavor.

Wherein, the acid used may be inorganic acids such as hydrochloric acid and sulfuric acid. The organic solvent is added in excess, so that the substances in the tobacco rod are completely dissolved,

Preferably, before using the enzyme treatment, the step of grinding the tobacco rod is also included. Grinding is more preferably ball milling for 48-72 hours, which is conducive to the full contact reaction between the substance in the tobacco rod and the enzyme.

Preferred enzymes are cellulases and hemicellulases. The mass ratio of cellulase and hemicellulase is (2-3):1. Preferably, the mass ratio of the total amount of added enzyme to the tobacco rod is 240-450U/g tobacco rod. Preferably, the temperature of the enzyme-treated tobacco rod is 40-55° C., and the time is 6-8 days.

When the tobacco rod is used after grinding, the dosage of the enzyme is calculated according to the weight of the tobacco rod after grinding, and 240-450 U of enzyme is added to each gram of the tobacco rod.

The residue is preferably dried at 50-60°C, ground to 100-200 mesh, dissolved in an organic solvent, extracted at 65-75°C for 2-4 hours, filtered, added acid to precipitate lignin, centrifuged, and heated at 60-70°C drying to obtain enzymatic lignin. Benzyl alcohol, benzene, and phenylethyl alcohol are organic solutions that can dissolve lignin without changing the properties of lignin. Grinding to 100-200 mesh is conducive to the dissolution of residues in organic solvents, and then formic acid is extracted and separated to obtain enzymatic hydrolysis Lignin.

It is preferred that the used Taxus sp. is its primary seed solution. The activity of Taxus sp. in the primary seed liquid is relatively high, which enhances the modification effect of Taxus sp. on enzymatic lignin, and finally successfully prepares an appropriate modified Proactive enzymatic degradation of lignin. After obtaining the first-grade seed liquid, mix the first-grade seed liquid of the yew tree tooth fungus with the enzymatic lignin, culture it statically at 27-28°C, and dry it at 60-70°C after culturing for 25-30 days to obtain Modified lignin for subsequent pyrolysis.

Preferably, the thermal cracking temperature is 400-450° C. and the time is 30-60 s to obtain the tobacco flavor. More preferably, during thermal cracking, the initial temperature is 60°C, and the heating rate is 5-6°C/ms.

The present application also provides the tobacco flavor prepared by the above method, and the application of the above tobacco flavor in tobacco sheets.

Detailed ways

In order to enable those skilled in the art to better understand the technical solution in the application, the technical solution in the embodiment of the application will be clearly and completely described below, obviously, the described embodiment is only a part of the embodiment of the application , but not all examples. Based on the embodiments in this application, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the scope of protection of this application.

Example 1

A method for preparing tobacco spices by using a tobacco rod, comprising the following steps:

Mill 200g of tobacco stalks for 48 hours, then use cellulase and hemicellulase to ferment for 7 days at 40-55°C; the ratio of the sum of the mass of cellulase and hemicellulase to tobacco stalk powder is 300U /g tobacco rod; the mass ratio of cellulase and hemicellulase is 2:1;

Take the fermentation residue and dry it at 50°C, grind it to 100 mesh, take 50g and dissolve it in 150ml benzyl alcohol, extract at 65°C for 2 hours, filter, add hydrochloric acid to adjust the filtrate to about pH=3, and keep it at 60°C for 0.5h. The lignin is precipitated, centrifuged, and dried at 60°C to obtain the enzymatic lignin; the enzymatic lignin is ground, and the enzymatic lignin between 40 mesh and 60 mesh is taken for use.

Select the yew wood tooth fungus on the slant medium, inoculate it in a 250ml Erlenmeyer flask containing 100ml PDB medium, and culture it on a shaker with a rotation speed of 180r/min at 27°C for 7 days to obtain the yew wood tooth Bacteria primary seed liquid;

Then take 20ml of the first-grade seed liquid of P. chinensis and mix it with 20g of enzymatic lignin. After aseptic stirring, let it stand for 25 days at 27°C and then dry it in an oven at 60°C to obtain modified lignin. ;

Take 0.5mg of modified lignin and put it into a quartz tube. The initial temperature is 60°C, and the temperature is raised to 400°C. to save.

The above tobacco flavor is added to the tobacco sheet in the form of filling, and the mass ratio of the tobacco flavor to the tobacco sheet is 10:100.

Example 2

A method for preparing tobacco spices by using a tobacco rod, comprising the following steps:

Mill 200g of tobacco stems for 60 hours, then use cellulase and hemicellulase to ferment for 7 days at 40-55°C; the ratio of the sum of the mass of cellulase and hemicellulase to tobacco stem powder is 400U /g tobacco rod; the mass ratio of cellulase and hemicellulase is 2:1;

Take the fermentation residue and dry it at 55°C, grind it to 200 mesh, take 50g and dissolve it in 150ml benzyl alcohol, extract at 70°C for 3 hours, filter, add hydrochloric acid to adjust the filtrate to about pH=3, and keep it at 65°C for 0.5h. The lignin is precipitated, centrifuged, and dried at 65°C to obtain the enzymatic lignin; the enzymatic lignin is ground, and the enzymatic lignin between 40 mesh and 60 mesh is taken for use.

Select the yew wood tooth fungus on the slant medium, inoculate it in a 250ml Erlenmeyer flask containing 100ml PDB medium, and cultivate it on a shaker with a rotation speed of 200r/min for 8 days at 28°C to obtain the yew wood tooth Bacteria primary seed liquid;

Then take 20ml of the first-grade seed liquid of A. chinensis and mix it with 20g of enzymatic lignin. After aseptic stirring, let it stand for 25 days at 28°C, and then dry it in an oven at 65°C to obtain modified lignin. ;

Take 0.5mg of modified lignin and put it into a quartz tube. The initial temperature is 60°C, and the temperature is raised to 450°C. to save.

The above-mentioned tobacco spices are added to the tobacco sheet in the form of filling, and the mass ratio of the tobacco flavor to the tobacco sheet is 15:100.

The tobacco flavor prepared in Example 1-2 was taken and analyzed by gas-mass spectrometry. The results are shown in Table 1.

Among them, the blank group is tobacco rod powder that has only been ball milled for 48 hours.

Table 1

Note a: P: phenolic compound; G: guaiac-based phenolic compound; C: bisphenolic compound; AH: aromatic hydrocarbon compound

It can be seen from Table 1 that after the tobacco rod is modified by the method provided by the application, its pyrolysis properties have changed significantly, which provides conditions for improving pyrolysis efficiency and enrichment of pyrolysis products.

The tobacco sheet prepared in Example 1-2 was taken for smoking evaluation. The results are shown in Table 2.

Among them, the blank group is tobacco sheet made of tobacco rod powder only after ball milling for 48 hours.

Adjust the water content of the sample according to GB/T 16447 before evaluation. For the senses, the dark scoring method is adopted, and an evaluation team composed of 7 people is used to evaluate and score the four aspects of luster, aroma, harmony and miscellaneous atmosphere. The sensory quality results are shown in the table.

test group Gloss ⁵ Aroma ³⁰ coordination ¹⁰ miscellaneous gas ²⁰ blank group 5 28.42 9.01 18.16 Example 1 5 29.11 9.35 18.78 Example 2 5 29.78 9.89 18.99

Smoking experiments show that the cigarettes prepared in Examples 1-2 have more obvious aroma, soft mouthfeel and improved aftertaste.

The above description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (15)

1. A method for preparing tobacco flavor by using tobacco stems, which is characterized by comprising the following steps:

treating tobacco stems by using enzyme, taking residues, drying, grinding, dissolving in an organic solvent, extracting, filtering, adding acid to separate out lignin, separating, and drying to obtain enzymatic hydrolysis lignin;

treating the enzymatic hydrolysis lignin by using the taxifola to obtain modified lignin;

and (3) thermally cracking the modified lignin to obtain the tobacco flavor.

2. The method of preparing a tobacco flavor using tobacco stems according to claim 1, further comprising the step of grinding the tobacco stems prior to the enzyme treatment.

3. The method for preparing tobacco flavor by using tobacco stems according to claim 2, wherein the tobacco stems are ball-milled for 48-72 hours.

4. The method for preparing tobacco flavor by using tobacco stems according to claim 1, wherein the organic solvent is any one of benzyl alcohol, benzene and phenethyl alcohol.

5. The method for preparing a tobacco flavor using tobacco stems according to claim 1, wherein the enzymes are cellulases and hemicellulases.

6. The method for producing tobacco flavor using tobacco stems according to claim 5, wherein the mass ratio of cellulase to hemicellulase is (2-3): 1.

7. The method for preparing tobacco flavor by using tobacco stems according to claim 1, wherein the mass ratio of enzyme to tobacco stems is 240-450U/g tobacco stems; the temperature of the enzyme-treated tobacco stems is 40-55 ℃ and the time is 6-8 days.

8. The method for preparing tobacco flavor by using tobacco stems according to claim 1, wherein the residue is dried at 50-60 ℃, ground to 100-200 meshes, dissolved in an organic solvent, extracted at 65-75 ℃ for 2-4 hours, filtered, added with acid, kept at 60-70 ℃ for 0.5-1 hour to separate out lignin, centrifuged, dried at 60-70 ℃ and ground to 40-60 meshes, thus obtaining the enzymatic lignin.

9. The method for preparing tobacco flavor by using tobacco stems according to claim 1, wherein the enzymatic lignin is treated with a primary seed solution of the genus taxillus; the first-stage seed liquid of the kaurena is obtained by the following steps:

selecting Sphaeria kauri, inoculating on PDB culture medium, and culturing on shaking table at 180-200r/min at 27-28deg.C for 7-10 days to obtain Sphaeria kauri primary seed solution.

10. The method for preparing tobacco flavor by using tobacco stems according to claim 9, wherein the ratio of the primary seed liquid of the kaurena to the enzymatically hydrolyzed lignin is 1ml of the primary seed liquid of the kaurena, (1-3) g of the enzymatically hydrolyzed lignin.

11. The method for preparing tobacco flavor by using tobacco stems according to claim 9, wherein the modified lignin is obtained by mixing the primary seed solution of the kaurena sinensis with the enzymatic lignin, performing stationary culture at 27-28 ℃, culturing for 25-30 days, and drying at 60-70 ℃.

12. The method for preparing tobacco flavor by using tobacco stems according to claim 1, wherein the modified lignin is thermally cracked at 400-450 ℃, and the temperature is kept for 30-60 seconds, so as to obtain the tobacco flavor.

13. The method for preparing tobacco flavor using tobacco stems according to claim 12, wherein the initial temperature is 60 ℃, and the heating rate is 5-6 ℃/ms.

14. A tobacco flavor produced by the method of any one of claims 1-13.

15. Use of a tobacco flavor according to claim 14 in tobacco flakes, characterized in that the tobacco flavor is added to the tobacco flakes in a filled form, the mass ratio of tobacco flavor to tobacco flakes being (5-15): 100.