阅读说明：本技术 一种利用废弃烟叶制备烟用香料的方法及烟用香料的应用 (Method for preparing tobacco flavor by using waste tobacco leaves and application of tobacco flavor ) 是由 陈芝飞 万帅 席高磊 于建春 王清福 蔡莉莉 李耀光 赵学斌 赵志伟 赵旭 杜佳 于 2021-09-20 设计创作，主要内容包括：本发明公开了一种利用废弃烟叶制备烟用香料的方法及烟用香料的应用,方法包括：对废弃烟叶进行粉碎处理；采用溶剂对第一份废弃烟叶进行萃取处理,得到烟叶提取液；对烟叶提取液进行过滤、减压蒸馏处理,得到烟叶浓缩液；对第二份废弃烟叶进行超高压提取处理,得到超高压处理液；将烟叶浓缩液稀释处理后得到的稀释液和超高压处理液混合后与氨基酸混匀,调节pH至8-10,于惰性气体氛围中高温高压反应得到香料液；将香料液的pH调至5-7后进行真空冷冻干燥处理,得到烟用香料。烟用香料的香味物质种类丰富,香气强度更高,能够与烟香更好的协调,适用于加热不燃烧卷烟应用。(The invention discloses a method for preparing tobacco flavor by using waste tobacco leaves and application of the tobacco flavor, wherein the method comprises the following steps: crushing the waste tobacco leaves; extracting the first waste tobacco leaves by using a solvent to obtain a tobacco leaf extracting solution; filtering and distilling the tobacco leaf extract under reduced pressure to obtain a tobacco leaf concentrated solution; carrying out ultrahigh pressure extraction treatment on the second part of waste tobacco leaves to obtain ultrahigh pressure treatment liquid; mixing a diluent obtained by diluting the concentrated tobacco leaf solution with the ultrahigh pressure treatment solution, uniformly mixing the diluent with amino acid, adjusting the pH to 8-10, and carrying out high-temperature high-pressure reaction in an inert gas atmosphere to obtain a spice solution; and adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the tobacco spice. The cigarette flavor has rich types of flavor substances and higher flavor intensity, can be better coordinated with the cigarette flavor, and is suitable for heating non-burning cigarettes.)

1. A method for preparing tobacco flavor by using waste tobacco leaves is characterized by comprising the following steps:

step (1): crushing the waste tobacco leaves;

step (2): extracting the first part of the waste tobacco leaves by using a solvent to obtain a tobacco leaf extracting solution, wherein the solvent is ethanol with the volume percentage of 45-60%, the temperature is 100-120 ℃, the extraction time is 5-8h, and the ratio of the mass of the solvent to the mass of the waste tobacco leaves is 1 (10-15);

and (3): filtering and distilling the tobacco leaf extract under reduced pressure to obtain a tobacco leaf concentrated solution;

and (4): carrying out ultrahigh pressure extraction treatment on the second part of waste tobacco leaves to obtain ultrahigh pressure treatment liquid, wherein the ultrahigh pressure extraction treatment pressure is 50-300MPa, the pressure maintaining time is 3-8min, the pressure relief time is 10-30s, and the mass ratio of the second part of waste tobacco leaves to the first part of waste tobacco leaves is 1: 1;

and (5): mixing a diluent obtained by diluting the concentrated tobacco leaf solution with the ultrahigh pressure treatment solution, then uniformly mixing the diluent with the amino acid, adjusting the pH to 8-10, and carrying out high-temperature high-pressure reaction in an inert gas atmosphere to obtain a spice solution, wherein the temperature of the high-temperature high-pressure reaction is 150-;

and (6): and adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the tobacco spice.

2. The method for preparing tobacco flavor using waste tobacco leaves according to claim 1, wherein the average size of the waste tobacco leaves after the pulverization treatment in the step (1) is 50-100 mesh.

3. The method for preparing tobacco flavor using waste tobacco leaves according to claim 1, wherein the temperature of the reduced pressure distillation treatment in the step (3) is 45 ℃, the pressure is 0.05MPa, and the time is 40-60 min.

4. The method for preparing the tobacco flavor using the waste tobacco leaves according to claim 1, wherein the second waste tobacco leaves are soaked before the second waste tobacco leaves are subjected to the ultra-high pressure treatment in the step (4).

5. The method for preparing the tobacco flavor by using the waste tobacco leaves according to claim 4, wherein the mass ratio of the second waste tobacco leaves to water in the soaking treatment is 1 (3-4), the time is 1-2h, and the temperature is 40-60 ℃.

6. The method for preparing the tobacco flavor from the waste tobacco leaves according to claim 1, wherein the diluent in the step (5) is obtained according to the volume ratio of the tobacco leaf concentrated solution to water of 1 (3-5).

7. The method for preparing the tobacco flavor from the waste tobacco leaves according to claim 1, wherein the amino acid in the step (5) is at least one of glycine, alanine, leucine and tryptophan, and the volume ratio of the amino acid to the sum of the volumes of the diluent and the ultrahigh pressure treatment liquid is (1-4):20, wherein the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL.

8. The method for preparing the tobacco flavor from the waste tobacco leaves according to claim 7, wherein the feed-liquid ratio of the amino acid to the sum of the volumes of the diluent and the ultrahigh pressure treatment liquid is (2-3): 20.

9. The method for preparing tobacco flavor using waste tobacco leaves according to claim 1, wherein the parameters of the vacuum freeze-drying process in the step (6) are as follows:

freezing at-100 deg.C to-20 deg.C under vacuum pressure of 10-100 Pa.

10. The use of the tobacco flavor obtained by the method for preparing a tobacco flavor from waste tobacco leaves according to any one of claims 1 to 9, wherein the tobacco flavor is added in an amount of 1 to 3% o.

Technical Field

The invention relates to the field of preparation of tobacco flavors, in particular to a method for preparing a tobacco flavor by using waste tobacco leaves and application of the tobacco flavor.

Background

With the increase of the planting area of tobacco and the yield of tobacco leaves, a large amount of waste tobacco leaves generated in the purchasing, transportation and industrial processing production of the tobacco leaves are accumulated and difficult to treat, so that the environmental pollution and the resource waste are caused, and the harmless treatment cost is high. The waste tobacco leaves are reasonably utilized, so that not only can a raw material source be provided for the research and development of cigarette products, but also the production cost of enterprises can be reduced, and the environmental pollution is reduced.

At present, the waste tobacco leaves are mainly used for producing tobacco sheets, the capacity of the waste tobacco leaves is far insufficient to consume the huge amount of the waste tobacco leaves, and a certain technical problem still exists how to fully utilize the waste tobacco leaves.

The tobacco extract is one of the most important flavor raw materials for blending flavor of Chinese cigarettes, and has the effects of enhancing the characteristic flavor of the tobacco and improving the sensory quality of the cigarettes. By reasonably utilizing the tobacco extract, the cigarette industry enterprises can relieve the contradiction of insufficient supply of high-quality tobacco leaf raw materials to a certain extent and can fully utilize the waste tobacco leaves to a great extent.

The ultrahigh pressure extraction technology is a method with the advantages of simple operation, time saving, environmental protection, suitability for large-scale production and the like, the operation process is carried out at normal temperature or below, the protection of heat sensitive components is facilitated, and the method is particularly suitable for preparing the tobacco extract.

Therefore, how to provide a method for preparing tobacco flavor by effectively utilizing waste tobacco leaves becomes a technical problem which needs to be solved urgently in the field.

Disclosure of Invention

The invention aims to provide a new technical scheme of a method for preparing tobacco flavor by using waste tobacco leaves.

According to a first aspect of the present invention, there is provided a method of preparing a tobacco flavor from waste tobacco leaves.

The method for preparing the tobacco flavor by using the waste tobacco leaves comprises the following steps:

step (1): crushing the waste tobacco leaves;

step (2): extracting the first part of the waste tobacco leaves by using a solvent to obtain a tobacco leaf extracting solution, wherein the solvent is ethanol with the volume percentage of 45-60%, the temperature is 100-120 ℃, the extraction time is 5-8h, and the ratio of the mass of the solvent to the mass of the waste tobacco leaves is 1 (10-15);

and (3): filtering and distilling the tobacco leaf extract under reduced pressure to obtain a tobacco leaf concentrated solution;

and (4): carrying out ultrahigh pressure extraction treatment on the second part of waste tobacco leaves to obtain ultrahigh pressure treatment liquid, wherein the ultrahigh pressure extraction treatment pressure is 50-300MPa, the pressure maintaining time is 3-8min, the pressure relief time is 10-30s, and the mass ratio of the second part of waste tobacco leaves to the first part of waste tobacco leaves is 1: 1;

and (5): mixing a diluent obtained by diluting the concentrated tobacco leaf solution with the ultrahigh pressure treatment solution, then uniformly mixing the diluent with the amino acid, adjusting the pH to 8-10, and carrying out high-temperature high-pressure reaction in an inert gas atmosphere to obtain a spice solution, wherein the temperature of the high-temperature high-pressure reaction is 150-;

and (6): and adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the tobacco spice.

Optionally, the average size of the waste tobacco leaves after the crushing treatment in the step (1) is 50-100 meshes.

Optionally, the temperature of the reduced pressure distillation treatment in the step (3) is 45 ℃, the pressure is 0.05MPa, and the time is 40-60 min.

Optionally, in the step (4), before the second portion of the waste tobacco leaves is subjected to the ultrahigh pressure treatment, the second portion of the waste tobacco leaves is soaked.

Optionally, the mass ratio of the second waste tobacco leaves to water in the soaking treatment is 1 (3-4), the time is 1-2h, and the temperature is 40-60 ℃.

Optionally, the diluent in the step (5) is obtained according to the volume ratio of the tobacco leaf concentrated solution to water of 1 (3-5).

Optionally, the amino acid in the step (5) is at least one of glycine, alanine, leucine and tryptophan, and the feed-liquid ratio of the amino acid to the sum of the volumes of the diluent and the ultrahigh pressure treatment liquid is (1-4):20, wherein the unit of the feed in the feed-liquid ratio is g, and the unit of the liquid is mL.

Optionally, the feed-liquid ratio of the amino acid to the sum of the volumes of the diluent and the ultrahigh pressure treatment liquid is (2-3): 20.

Optionally, the parameters of the vacuum freeze-drying process in the step (6) are as follows:

freezing at-100 deg.C to-20 deg.C under vacuum pressure of 10-100 Pa.

According to a second aspect of the invention, the application of the tobacco flavor prepared by the method for preparing the tobacco flavor by using the waste tobacco leaves in the disclosure is provided, wherein the adding amount of the tobacco flavor is 1-3 per mill.

The invention has the following advantages:

(1) the method takes the waste tobacco leaves as the raw material, provides a new idea for the full utilization of the waste tobacco leaves of the flue-cured tobacco in the production of cigarette industry enterprises, not only can reduce the environmental pollution pressure, but also can save the cost and improve the industrial value of the product.

(2) The cigarette flavor has high pyrazine content and furfural content, can endow cigarettes with baking aroma, improve the sweet taste of the cigarettes, improve the aroma of cigarette products, reduce irritation and residue and has potential application value when being used for flavoring the cigarettes.

(3) The cigarette flavor has rich types of flavor substances and higher flavor intensity, can be better coordinated with the cigarette flavor, and is suitable for heating non-burning cigarettes.

Detailed Description

Various exemplary embodiments of the present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.

The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.

Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.

In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.

The method for preparing the tobacco flavor by using the waste tobacco leaves comprises the following steps:

step (1): and (4) crushing the waste tobacco leaves.

In order to achieve better treatment effect, the average size of the waste tobacco leaves after the crushing treatment in the step (1) is 50-100 meshes.

Step (2): extracting the first part of the waste tobacco leaves by using a solvent to obtain a tobacco leaf extracting solution, wherein the solvent is ethanol with the volume percentage of 45-60%, the temperature is 100-120 ℃, the extraction time is 5-8h, and the ratio of the mass of the solvent to the mass of the waste tobacco leaves is 1 (10-15).

And (3): and filtering and distilling the tobacco leaf extract under reduced pressure to obtain a tobacco leaf concentrated solution.

The temperature of the reduced pressure distillation treatment in the step (3) is 45 ℃, the pressure is 0.05MPa, and the time is 40-60 min.

And (4): and carrying out ultrahigh pressure extraction treatment on the second part of waste tobacco leaves to obtain ultrahigh pressure treatment liquid, wherein the ultrahigh pressure extraction treatment pressure is 50-300MPa, the pressure maintaining time is 3-8min, the pressure relief time is 10-30s, and the mass ratio of the second part of waste tobacco leaves to the first part of waste tobacco leaves is 1: 1.

In order to achieve a better ultrahigh pressure extraction treatment effect, in the step (4), before the second part of waste tobacco leaves are subjected to ultrahigh pressure treatment, the second part of waste tobacco leaves are soaked.

In the specific implementation, the mass ratio of the second waste tobacco leaves to water in the soaking treatment can be 1 (3-4), the time can be 1-2h, and the temperature can be 40-60 ℃.

And (5): mixing the diluted solution obtained after diluting the concentrated solution of the tobacco leaves with the ultrahigh pressure treatment solution, then uniformly mixing the diluted solution with amino acid, adjusting the pH to 8-10, and carrying out high-temperature high-pressure reaction in an inert gas atmosphere to obtain the spice solution, wherein the temperature of the high-temperature high-pressure reaction is 150-250 ℃, the pressure is 0.5-2.5MPa, and the reaction time is 2-4 h. The dilution treatment is beneficial to improving the efficiency of the subsequent Maillard reaction.

In specific implementation, 1-5mol/L aqueous solution of sodium hydroxide or potassium hydroxide can be used for adjusting the pH.

And (5) obtaining the diluent in the step (5) according to the volume ratio of the concentrated tobacco leaf liquid to water of 1 (3-5).

In order to ensure the effect of the Maillard reaction, the amino acid in the step (5) is at least one of glycine, alanine, leucine and tryptophan, and the feed-liquid ratio of the amino acid to the sum of the volumes of the diluent and the ultrahigh pressure treatment liquid is (1-4):20, wherein the unit of the feed in the feed-liquid ratio is g, and the unit of the liquid is mL.

In order to improve the tobacco fragrance intensity of the tobacco flavor, the material-liquid ratio of the amino acid to the sum of the volumes of the diluent and the ultrahigh pressure treatment liquid is (2-3): 20.

And (6): and adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the tobacco spice.

In specific implementation, the pH of the spice liquid can be adjusted by adopting citric acid aqueous solution, malic acid aqueous solution and tartaric acid aqueous solution.

The parameters of the vacuum freeze-drying process in step (6) may be as follows:

freezing at-100 deg.C to-20 deg.C under vacuum pressure of 10-100 Pa.

The disclosure also provides an application of the tobacco flavor prepared by the method for preparing the tobacco flavor by utilizing the waste tobacco leaves, wherein the adding amount of the tobacco flavor is 1-3 per mill.

The experimental procedures used in the examples below are conventional unless otherwise specified, the materials and reagents used therein are commercially available, and the equipment used in the experiments are well known to those skilled in the art without otherwise specified.

Example 1

20g of crushed waste tobacco leaves (average size of 100 meshes) are weighed and added into a 250mL round-bottom flask, 200mL of 60% absolute ethyl alcohol is added, and the extraction conditions are as follows: the temperature is 120 ℃, the time is 8 hours, and the ratio of the mass of the solvent to the mass of the waste tobacco leaves is 1: 10. And cooling to room temperature after extraction is finished, filtering, collecting filtrate, and distilling under reduced pressure to obtain the tobacco leaf concentrated solution. Diluting the tobacco leaf concentrated solution according to the volume ratio of the tobacco leaf concentrated solution to water of 1:4 to obtain a diluent.

Weighing 20g of crushed waste tobacco leaves (average size is 100 meshes), adding 80g of water, soaking at 60 ℃ for 2h, and then carrying out ultrahigh pressure extraction treatment to obtain ultrahigh pressure treatment liquid, wherein the ultrahigh pressure extraction treatment pressure is 200MPa, the pressure maintaining time is 5min, and the pressure relief time is 20 s.

Mixing the diluent with the ultrahigh pressure treatment solution, mixing with amino acid (the material-liquid ratio of the amino acid to the sum of the volumes of the diluent and the ultrahigh pressure treatment solution is 3:20) and pH adjusting solution (pH is adjusted to 9), adding into a 500mL autoclave reactor, covering and sealing, opening an air inlet hole and an air outlet hole, filling nitrogen gas into the air inlet hole, discharging the internal air from the air outlet hole, closing the air outlet hole, and filling nitrogen gas again. The temperature of the high-pressure kettle type reactor is adjusted to be 180 ℃, the pressure is 1.0MPa, the reaction is carried out for 3.5h, and the reactor is naturally cooled to the room temperature.

And (3) adjusting the pH value of the reacted spice liquid to 6, and then freezing and drying at-80 ℃ and 25Pa to obtain the tobacco spice 1.

The prepared tobacco flavor is analyzed by an Agilent7890A-5975C type gas chromatography-mass spectrometer (Agilent technologies, Inc., USA) and an Agilent 1290-micOTOF Q II type liquid chromatography-mass spectrometer (Agilent technologies, Inc., USA) respectively, and the content of pyrazine and the content of furfural in the tobacco flavor are found to be high.

Comparative example 1

20g of crushed waste tobacco leaves (average size of 100 meshes) are weighed and added into a 250mL round-bottom flask, 200mL of 60% absolute ethyl alcohol is added, and the extraction conditions are as follows: the temperature is 120 ℃, the time is 8 hours, and the ratio of the mass of the solvent to the mass of the waste tobacco leaves is 1: 10. And cooling to room temperature after extraction is finished, filtering, collecting filtrate, and distilling under reduced pressure to obtain the tobacco leaf concentrated solution. Diluting the tobacco leaf concentrated solution according to the volume ratio of the tobacco leaf concentrated solution to water of 1:4 to obtain a diluent.

Mixing the diluent with amino acid (the material-liquid ratio of the amino acid to the diluent is 3:20) and pH adjusting solution (pH is adjusted to 9), adding into a 500mL autoclave reactor, covering and sealing, opening an air inlet hole and an air outlet hole, filling nitrogen into the air inlet hole, discharging the internal air from the air outlet hole, then closing the air outlet hole, and filling nitrogen again. The temperature of the high-pressure kettle type reactor is adjusted to be 180 ℃, the pressure is 1.0MPa, the reaction is carried out for 3.5h, and the reactor is naturally cooled to the room temperature.

And (3) adjusting the pH value of the reacted spice liquid to 6, and then freezing and drying at-80 ℃ and 25Pa to obtain the tobacco spice 1'.

Comparative example 2

Weighing 20g of crushed waste tobacco leaves (average size is 100 meshes), adding 80g of water, soaking at 60 ℃ for 2h, and then carrying out ultrahigh pressure extraction treatment to obtain ultrahigh pressure treatment liquid, wherein the ultrahigh pressure extraction treatment pressure is 200MPa, the pressure maintaining time is 5min, and the pressure relief time is 20 s.

Mixing the ultrahigh pressure treatment liquid with amino acid (the material-liquid ratio of the amino acid to the ultrahigh pressure treatment liquid is 3:20) and pH adjusting liquid (the pH is adjusted to 9), adding into a 500mL autoclave reactor, covering and sealing, opening an air inlet hole and an air outlet hole, filling nitrogen into the air inlet hole, discharging the internal air from the air outlet hole, then closing the air outlet hole, and filling nitrogen again. The temperature of the high-pressure kettle type reactor is adjusted to be 180 ℃, the pressure is 1.0MPa, the reaction is carried out for 3.5h, and the reactor is naturally cooled to the room temperature.

And (3) adjusting the pH value of the reacted spice liquid to 6, and then freezing and drying at-80 ℃ and 25Pa to obtain the tobacco spice 2'.

Weighing a certain amount of tobacco flavors 1, 1 'and 2', and diluting the tobacco flavors 1, 1 'and 2' into a flavor solution of 5% (mass percent) by using ethanol and distilled water (the volume ratio is 1:4) for later use. Weighing 100g of blank non-combustible cigarette slice shreds without tobacco flavor, uniformly spreading in a clean tray, uniformly spraying flavor solution on the slice shreds to obtain the tobacco flavor in which the proportion of the slice shreds is 2.00 per mill, sealing and standing for 2 h. Then the mixture is put into a baking oven at 100 ℃ for drying, is humidified by distilled water to reach the standard moisture (12 percent), and is rolled into a standard cigarette bullet for heating the non-combustible cigarette, and the balance time (the humidity is 50 percent +/-2 percent, and the temperature is 25 +/-1 ℃) is 48 hours. The smoke cartridge was heated by a special heating source of the appliance and the results of the smoke panel test are shown in table 1.

TABLE 1 results of the test

As can be seen from the results of smoking evaluation in Table 1, the tobacco flavor disclosed by the invention can improve the aroma and the overall comfort of the heated cigarette, can effectively improve and modify the smoke of the non-burning heated cigarette, and can improve the aroma quality and the aroma quantity, so that the smoke is fine and smooth, and the sweetness is improved. The tobacco flavor disclosed by the invention is used for flavoring cigarettes, can endow the heated cigarettes with mellow characteristic, improves the sweet taste of the cigarettes, improves the aroma of cigarette products, reduces irritation and residues, and has potential application value.

Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.