WO2021223319A1 - Flavor additive for cigarettes and preparation method therefor - Google Patents

Abstract

A flavor additive for cigarettes, composed of the following components in parts by weight: 30-35 parts of poplar flower extract, 20-30 parts of propylene glycol, 10-20 parts of arabinose, and 10-50 parts of water. The preparation method for the poplar flower extract comprises the following steps: A, washing poplar flowers, freeze-drying and crushing the poplar flowers to obtain poplar flower powder; B, mixing petroleum ether, propyl isobutyrate, and glycerol in a mass ratio of 5:2:(3-8) to obtain a mixed solvent; soaking the poplar flower powder in the mixed solvent to obtain a soaking liquid; C, performing continuous circulating extraction on the soaking liquid using supercritical carbon dioxide fluid to obtain an extract liquid; and D, separating the extract liquid, collecting the product obtained by separation, and drying same to obtain a poplar flower extract. The technical solutions solves the problem of low extraction rate of poplar flower extracts in the prior art.

Description

Spice for tobacco and preparation method thereof Technical field

The invention belongs to the technical field of tobacco flavors, and relates to a tobacco flavor and a preparation method thereof.

Background technique

With the advancement of science and technology, people are paying more and more attention to the harm caused by smoking. Smokers have higher and higher requirements for the quality of cigarettes. It is imperative to produce cigarettes with low toxicity, good aroma and high quality. Poplars are tall and perennial trees. They are widely distributed in various parts of our country and are rich in resources. They account for a large proportion of the green trees in the country. Poplar flowers are rich in vitamins and fats, including alkaloids, organic acids, polyphenols, flavonoids and other substances, which have the functions of invigorating the stomach, nourishing the spleen, astringent intestines and alleviating diarrhea, clearing away heat and pain, and inhibiting bacteria. Polyphenols are important aroma precursors of tobacco and are closely related to the type and amount of aroma of tobacco leaves. Flavonoids will produce furans and their derivatives after combustion and pyrolysis. These substances are the main aroma components in the smoke. They will bring sweet, sweet and roasting aroma to the smoke, increasing the amount and quality of the aroma. . In view of the fact that poplar flowers are rich in polyphenols and flavonoids, poplar flower extracts can be used as tobacco flavors.

At present, poplar flower extract is widely used in animal feed because of its functions such as invigorating the stomach and nourishing the spleen, astringent intestines and alleviating diarrhea, clearing away heat and pain, and inhibiting bacteria. The poplar flower extract is obtained by refluxing with ethanol, and the method is specifically as follows: adopting a material-to-water ratio of 1:25, and extracting with 60% ethanol at 80° C. for 150 minutes to obtain a poplar flower extract. The extraction method has a high extraction temperature, which causes some unstable aroma components to deteriorate due to heat during the extraction process, and the low-boiling top aroma components are lost, thereby affecting the extraction rate of the poplar flower extract.

Summary of the invention

The present invention provides a tobacco flavor and a preparation method thereof, which solves the problem of low extraction rate of poplar flower extracts in the prior art.

The technical scheme of the present invention is realized as follows:

A tobacco flavor, which is composed of the following components by weight:

30 to 35 parts of poplar flower extract, 20 to 30 parts of propylene glycol, 10 to 20 parts of arabinose, and 10 to 50 parts of water.

As a further technical solution, it is composed of the following parts by weight:

32 parts of poplar flower extract, 25 parts of propylene glycol, 15 parts of arabinose, 25 parts of water.

As a further technical solution, the preparation method of the poplar flower extract includes the following steps:

A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

B. Mixing petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:(3-8) to obtain a mixed solvent, and soaking poplar pollen in the mixed solvent to obtain a soaking liquid;

C. The soaking liquid is continuously circulated and extracted with supercritical carbon dioxide fluid to obtain the extraction liquid;

D. Separate the extract, collect the separated product, and dry it to obtain a poplar flower extract.

As a further technical solution, the mass ratio of poplar pollen to the mixed solvent in step B is (6.2-9.5):1.

As a further technical solution, in step C, the extraction temperature is 40-50° C., the extraction pressure is 30 MPa, the carbon dioxide flow rate is 35 L/h, and the extraction time is 80-100 min.

As a further technical solution, the separation temperature in step D is 35-50° C., and the separation pressure is 10 MPa.

The present invention also proposes a method for preparing tobacco flavors. According to the raw material components of the above tobacco flavors, the ingredients are mixed, poplar flower extract, propylene glycol, and water are mixed, heated to 40-50°C, stirred and dissolved, and then added The arabinose is stirred for 60 to 90 minutes to obtain the flavor for tobacco.

The working principle and beneficial effects of the present invention are:

1. In the present invention, the tobacco flavor uses poplar flower extract as the main raw material, and is compatible with propylene glycol and arabinose. After being used in shredded tobacco, it significantly improves the sensory quality of cigarettes, and makes the finished cigarettes have a soft and delicate aroma when inhaled. , Plump and natural, the overall improvement in sensory comfort is obvious, the harmony is significantly improved, the irritation is significantly reduced, the mouth feels better, and the sensory quality of the cigarette is significantly improved.

2. In the present invention, the poplar flower extract is prepared by the supercritical carbon dioxide fluid extraction method. Before the extraction, the poplar pollen is first extracted with petroleum ether, propyl isobutyrate, and glycerol in a mass ratio of 5:2:8. Soaked in mixed solvents, petroleum ether, propyl isobutyrate, and glycerol synergistically compatible, not only increased the extraction rate of poplar flower extract to 12.75%, but also significantly increased the content of total flavonoids and total polyphenols in poplar flower extract Polyphenol compounds are important aroma precursors in tobacco leaves, which increase the content of total polyphenols in poplar flower extracts, so that tobacco flavors with poplar flower extracts as the main raw material are added to the tobacco leaves more prominently, and the overall increase in cigarettes Sensory quality.

3. In the present invention, the poplar flower extract in the tobacco flavor is a pure natural plant extract, used in tobacco leaves, can significantly reduce the irritation of cigarettes after smoking, and at the same time have good coordination with the smoke, and improve the comfort after smoking Sense, green and natural, suitable for promotion and use.

Detailed ways

The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of the present invention.

A tobacco flavor, which is composed of the following components by weight:

30-35 parts of poplar flower extract, 20-30 parts of propylene glycol, 10-20 parts of arabinose, 10-50 parts of water;

The preparation method includes the following steps: mixing the above-mentioned raw material components, mixing poplar flower extract, propylene glycol, and water, heating to 40-50°C, stirring and dissolving, adding arabinose, and stirring for 60-90 minutes to obtain tobacco flavor;

Wherein, the preparation method of poplar flower extract includes the following steps:

A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

B. Mixing petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:(3-8) to obtain a mixed solvent, soak the poplar pollen with the mixed solvent to obtain a soaking liquid; The mass ratio of the mixed solvent is (6.2～9.5):1;

C. The soaking liquid is continuously cyclically extracted with supercritical carbon dioxide fluid, the extraction temperature is 40-50℃, the extraction pressure is 30MPa, the carbon dioxide flow rate is 35L/h, and the extraction time is 80-100min to obtain the extract;

D. Separate the extract, with a separation temperature of 35-50° C., and a separation pressure of 10 MPa, collect the separated products, and dry them to obtain poplar flower extracts.

Example 1

A tobacco flavor, which is composed of the following components by weight:

30 parts of poplar flower extract, 20 parts of propylene glycol, 10 parts of arabinose, 10 parts of water;

The preparation method includes the following steps: the above-mentioned raw material components are mixed, poplar flower extract, propylene glycol, and water are mixed, heated to 45° C., stirred and dissolved, and arabinose is added, and stirred for 80 minutes to obtain tobacco flavors;

Wherein, the preparation method of poplar flower extract includes the following steps:

A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

B. Mixing petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:5 to obtain a mixed solvent, and soaking poplar pollen in the mixed solvent to obtain a soaking liquid; the quality of the poplar pollen and the mixed solvent The ratio is 7.5:1;

C. The soaking liquid is continuously circulated and extracted with supercritical carbon dioxide fluid, the extraction temperature is 45°C, the extraction pressure is 30MPa, the carbon dioxide flow rate is 35L/h, and the extraction time is 90min to obtain the extract;

D. Separate the extract at a separation temperature of 40°C and a separation pressure of 10 MPa, collect the separated products, and dry them to obtain a poplar flower extract.

Example 2

A tobacco flavor, which is composed of the following components by weight:

35 parts of poplar flower extract, 30 parts of propylene glycol, 20 parts of arabinose, 50 parts of water;

The preparation method includes the following steps: the above-mentioned raw material components are mixed, poplar flower extract, propylene glycol, and water are mixed, heated to 45° C., stirred and dissolved, and arabinose is added, and stirred for 80 minutes to obtain tobacco flavors;

Among them, the preparation method of the poplar flower extract is the same as in Example 1.

Example 3

A tobacco flavor, which is composed of the following components by weight:

32 parts of poplar flower extract, 25 parts of propylene glycol, 15 parts of arabinose, 25 parts of water;

The preparation method includes the following steps: the above-mentioned raw material components are mixed, poplar flower extract, propylene glycol, and water are mixed, heated to 45° C., stirred and dissolved, and arabinose is added, and stirred for 80 minutes to obtain tobacco flavors;

Among them, the preparation method of the poplar flower extract is the same as in Example 1.

Example 4

A tobacco flavor, which is composed of the following components by weight:

32 parts of poplar flower extract, 25 parts of propylene glycol, 15 parts of arabinose, 25 parts of water;

The preparation method includes the following steps: mixing the above-mentioned raw material components, mixing poplar flower extract, propylene glycol, and water, heating to 50°C, stirring and dissolving, adding arabinose, and stirring for 60 minutes to obtain tobacco flavor;

Among them, the preparation method of the poplar flower extract is the same as in Example 1.

Example 5

A tobacco flavor, which is composed of the following components by weight:

32 parts of poplar flower extract, 25 parts of propylene glycol, 15 parts of arabinose, 25 parts of water;

The preparation method includes the following steps: mixing the above-mentioned raw material components, mixing poplar flower extract, propylene glycol, and water, heating to 40°C, stirring and dissolving, adding arabinose, and stirring for 90 minutes to obtain tobacco flavor;

Among them, the preparation method of the poplar flower extract is the same as in Example 1.

Example 6

The difference between this embodiment and embodiment 3 is only that the preparation method of poplar flower extract includes the following steps:

A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

B. Mix petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:3 to obtain a mixed solvent, soak the poplar pollen with the mixed solvent to obtain a soaking liquid; the quality of the poplar pollen and the mixed solvent The ratio is 6.2:1;

C. The soaking liquid is continuously circulated and extracted with supercritical carbon dioxide fluid, the extraction temperature is 45°C, the extraction pressure is 30MPa, the carbon dioxide flow rate is 35L/h, and the extraction time is 90min to obtain the extract;

D. Separate the extract at a separation temperature of 40°C and a separation pressure of 10 MPa, collect the separated products, and dry them to obtain a poplar flower extract.

Example 7

The difference between this embodiment and embodiment 3 is only that the preparation method of poplar flower extract includes the following steps:

A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

B. Mix petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:8 to obtain a mixed solvent, soak the poplar pollen in the mixed solvent to obtain a soaking liquid; the quality of the poplar pollen and the mixed solvent The ratio is 9.2:1;

C. The soaking liquid is continuously circulated and extracted with supercritical carbon dioxide fluid, the extraction temperature is 45°C, the extraction pressure is 30MPa, the carbon dioxide flow rate is 35L/h, and the extraction time is 90min to obtain the extract;

D. Separate the extract at a separation temperature of 40°C and a separation pressure of 10 MPa, collect the separated products, and dry them to obtain a poplar flower extract.

Example 8

The difference between this embodiment and embodiment 3 is only that the preparation method of poplar flower extract includes the following steps:

A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

B. Mixing petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:5 to obtain a mixed solvent, and soaking poplar pollen with the mixed solvent to obtain a soaking liquid; the quality of the poplar pollen and the mixed solvent The ratio is 7.5:1;

C. The soaking liquid is continuously circulated and extracted with supercritical carbon dioxide fluid, the extraction temperature is 40°C, the extraction pressure is 30MPa, the carbon dioxide flow rate is 35L/h, and the extraction time is 100min to obtain the extract;

D. Separate the extract with a separation temperature of 35°C and a separation pressure of 10 MPa, collect the separated products, and dry them to obtain a poplar flower extract.

Example 9

The difference between this embodiment and embodiment 3 is only that the preparation method of poplar flower extract includes the following steps:

A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

B. Mixing petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:5 to obtain a mixed solvent, and soaking poplar pollen with the mixed solvent to obtain a soaking liquid; the quality of the poplar pollen and the mixed solvent The ratio is 7.5:1;

C. The soaking liquid is continuously circulated and extracted with supercritical carbon dioxide fluid, the extraction temperature is 50°C, the extraction pressure is 30MPa, the carbon dioxide flow rate is 35L/h, and the extraction time is 80min to obtain the extract;

D. Separate the extract, with a separation temperature of 50°C and a separation pressure of 10 MPa, collect the separated products, and dry them to obtain a poplar flower extract.

Comparative example 1

The difference between this comparative example and Example 3 is only that arabinose is not added to the tobacco flavor.

Comparative example 2

The difference between this comparative example and Example 3 is only that in the preparation method of the poplar flower extract, the poplar pollen is directly extracted with supercritical carbon dioxide fluid for continuous circulation.

Comparative example 3

The difference between this comparative example and Example 3 is only that in the preparation method of the poplar flower extract, the poplar pollen is soaked in petroleum ether and then continuously cyclically extracted with supercritical carbon dioxide fluid.

Comparative example 4

The difference between this comparative example and Example 3 is only that in the preparation method of poplar flower extract, poplar pollen is soaked with propyl isobutyrate and then continuously cyclically extracted with supercritical carbon dioxide fluid.

Comparative example 5

The difference between this comparative example and Example 3 is only that in the preparation method of the poplar flower extract, the poplar pollen is soaked with glycerol and then continuously cyclically extracted with supercritical carbon dioxide fluid.

Comparative example 6

The difference between this comparative example and Example 3 is only that the mixed solvent in the preparation method of the poplar flower extract is obtained by mixing petroleum ether and propyl isobutyrate in a mass ratio of 5:2.

Comparative example 7

The difference between this comparative example and Example 3 is only that the mixed solvent in the preparation method of the poplar flower extract is obtained by mixing petroleum ether and glycerol with a mass ratio of 1:1.

Comparative example 8

The difference between this comparative example and Example 3 is only that the mixed solvent in the preparation method of the poplar flower extract is obtained by mixing propyl isobutyrate and glycerol in a mass ratio of 5:2.

Taking the tobacco flavors obtained in Examples 1-9 and Comparative Example 1 as samples, they were evaluated in the "Hebei" leaf group and added to the cut tobacco according to the amount of five ten-thousandths of the weight of the cut tobacco. The specific addition method is: each sample Spray evenly into shredded tobacco. After spraying, store the shredded tobacco at room temperature for 4 hours to make it naturally alcoholic, and then roast the shredded tobacco at 60℃ to a moisture content of 12% to 13%. The smokers conducted sensory evaluation and identification, and took the cigarettes without adding snow pear extract for cigarettes as the blank control group. The evaluation method refers to the national standard GB5606.4-2005 "Cigarette Part 4: Sensory Technical Requirements". The evaluation results are shown in the table below. :

Table 1 Cigarette smoking evaluation sensory evaluation scoring results

It can be seen from Table 1:

Compared with the blank control group, after the tobacco flavors of Examples 1-9 of the present invention are used in shredded tobacco, the aroma and harmony of the cigarettes made during smoking are significantly improved, the odor and irritation are significantly reduced, and the aftertaste is cleaner and more comfortable This shows that after the tobacco flavoring of the present invention is used in cut tobacco, the sensory quality of cigarettes is significantly improved.

When the tobacco flavor of the present invention is used for smoking cigarettes made after cut tobacco, the aroma is soft, delicate, full and natural, and the overall sensory comfort is significantly improved, the harmony is significantly improved, the irritation is significantly weakened, and the mouth feel is better.

Compared with Comparative Example 1, after the tobacco flavors of Examples 1-9 of the present invention are used in shredded tobacco, the aroma, harmony, aftertaste, etc. of the manufactured cigarettes during smoking are significantly improved, and the overall sensory quality is improved, which illustrates the advantages of the present invention Among tobacco flavors, poplar flower extract and arabinose are compatible with each other, which significantly improves the sensory quality of cigarettes.

The extraction rate of the poplar flower extract and the content of total flavonoids and total polyphenols in the method for preparing poplar flower extracts in tobacco flavors in Example 3 and Comparative Examples 2-8 were determined. The specific methods are as follows:

Extraction rate: Weigh the poplar flowers and the obtained poplar flower extracts used in each example and comparative example, and calculate the extraction rate according to the following formula: extraction rate (%)=(poplar flower extract mass/poplar flower mass)×100;

Total flavonoids content: using rutin as the reference substance, the standard curve is rutin Y = 0.0011X + 0.0205 (R = 0.9996), the total flavonoids (flavonoids) in the poplar flower extracts obtained in Example 3 and Comparative Examples 2-8 were measured ) Content;

Total polyphenol content: using gallic acid as the reference substance, the standard curve is gallic acid Y = 0.0027X + 0.083 (R ² = 0.9933), the total polyphenols in the poplar flower extracts obtained in Example 3 and Comparative Examples 2-8 were determined ( Polyphenolic compound) content:

The test results are as follows:

Table 2 The extraction rate and the total flavonoids and total polyphenol content of the methods for preparing poplar flower extracts in Example 3 and Comparative Examples 2-8

Group	Extraction rate (%)	Total flavonoid content (%)	Total polyphenol content (%)
Example 3	12.75	2.75	8.26
Comparative example 2	10.68	2.09	6.33

Comparative example 3	10.75	2.22	6.42
Comparative example 4	10.63	2.35	7.95
Comparative example 5	10.67	2.55	6.57
Comparative example 6	10.72	2.41	8.15
Comparative example 7	10.66	2.67	6.79
Comparative example 8	8.52	2.58	8.02

As can be seen from the above table, compared with Comparative Examples 2-8, the extraction rate of the poplar flower extract obtained by the method for preparing poplar flower extracts of the examples of the present invention is as high as 12.75%, and the total flavonoid content in the poplar flower extract is high To 2.75%, the total polyphenol content is as high as 8.26%, indicating that the method for preparing poplar flower extract of the present invention not only improves the extraction rate of poplar flower extract, but also significantly increases the content of total flavonoids and total polyphenols in poplar flower extract Therefore, the aroma of tobacco flavors, which use poplar flower extract as the main raw material, is added to the tobacco leaves more prominently, and the sensory quality of the cigarette is improved as a whole.

The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention. within.

Claims (7)

1. A tobacco flavor, which is characterized in that it is composed of the following components by weight:

   30 to 35 parts of poplar flower extract, 20 to 30 parts of propylene glycol, 10 to 20 parts of arabinose, and 10 to 50 parts of water.
2. A tobacco flavor according to claim 1, characterized in that it is composed of the following components by weight:

   32 parts of poplar flower extract, 25 parts of propylene glycol, 15 parts of arabinose, 25 parts of water.
3. The tobacco spice according to claim 1, wherein the method for preparing the poplar flower extract comprises the following steps:

   A. The poplar flowers are washed, freeze-dried, and crushed to obtain poplar pollen;

   B. Mixing petroleum ether, propyl isobutyrate, and glycerol with a mass ratio of 5:2:(3-8) to obtain a mixed solvent, and soaking poplar pollen with the mixed solvent to obtain a soaking liquid;

   C. The soaking liquid is continuously circulated and extracted with supercritical carbon dioxide fluid to obtain the extraction liquid;

   D. Separate the extract, collect the separated product, and dry it to obtain a poplar flower extract.
4. The tobacco flavor according to claim 3, wherein the mass ratio of poplar pollen to the mixed solvent in step B is (6.2-9.5):1.
5. The tobacco flavor according to claim 3, wherein in step C, the extraction temperature is 40-50°C, the extraction pressure is 30 MPa, the carbon dioxide flow rate is 35 L/h, and the extraction time is 80-100 min.
6. The tobacco flavor according to claim 3, characterized in that, in step D, the separation temperature is 35-50°C, and the separation pressure is 10 MPa.
7. A method for preparing tobacco flavors, characterized in that it comprises the following steps: according to the raw material components of a tobacco flavor of claim 1 or 2, mixing poplar flower extract, propylene glycol, and water, and heating to 40~ Add arabinose after stirring and dissolving at 50°C and stirring for 60-90 minutes to obtain tobacco flavors.