CN110367583B

CN110367583B - Tobacco leaf microwave pyrolysis product and application thereof in novel tobacco products

Info

Publication number: CN110367583B
Application number: CN201910568907.0A
Authority: CN
Inventors: 袁岐山; 王根发; 杨静; 陈泽少; 赵阔; 张孟伟; 朱琦; 张东豫; 刘文博; 席高磊; 陈谦
Original assignee: China Tobacco Henan Industrial Co Ltd
Current assignee: China Tobacco Henan Industrial Co Ltd
Priority date: 2019-06-27
Filing date: 2019-06-27
Publication date: 2022-12-27
Anticipated expiration: 2039-06-27
Also published as: CN110367583A

Abstract

The application belongs to the technical field of novel tobacco products, and particularly relates to a tobacco leaf microwave pyrolysis product and application patent application affairs thereof in the novel tobacco products. The main technical thought of the application is as follows: firstly, tobacco leaves are cracked under the condition of simulating cigarette combustion through a microwave cracking technology, and then cracked products are separated through an extraction technology to obtain characteristic components of the tobacco leaves, so that the aroma quality of the electronic cigarette is improved. Compared with the existing electronic cigarette liquid preparation method, the method has the following advantages: (1) Because the cracking operation is carried out firstly, compared with the conventional preparation method, the tar and other harmful substances can be effectively reduced during the subsequent extraction; (2) After the components obtained after extraction are further prepared into the electronic cigarette liquid, the herbal fragrance of the electronic cigarette can be effectively improved, so that the electronic cigarette has the characteristic fragrance of the herbal fragrance of the traditional cigarette, and the sensory qualities of strength, satisfaction and the like are improved.

Description

Tobacco leaf microwave pyrolysis product and application thereof in novel tobacco products

Technical Field

The application belongs to the technical field of novel tobacco products, and particularly relates to a tobacco leaf microwave pyrolysis product and application patent application affairs thereof in the novel tobacco products.

Background

In general, the novel tobacco products mainly include novel cigarettes, electronic cigarettes and smokeless tobacco, wherein the novel cigarettes mainly comprise heating non-combustion cigarettes, and the smokeless tobacco products mainly comprise buccal tobacco and chewing tobacco. The novel tobacco product has the characteristics of less harm, higher safety, capability of properly eliminating the harm of second-hand smoke, particularly convenience in smoking and the like, so that the novel tobacco product is developed rapidly in recent years.

Compared with the existing traditional cigarette, the electronic cigarette in the novel tobacco product can simulate the smoking process more vividly and better meet the physiological, psychological and behavioral requirements of smokers, so the electronic cigarette is considered to be a good substitute of the traditional cigarette and a relatively healthy cigarette substitute. One of the core of the electronic cigarette technology lies in the preparation method and specific components of the electronic cigarette liquid (tobacco tar), which are the key factors for determining the taste and harm of smoking.

The main components of the electronic cigarette liquid (tobacco tar) are nicotine and characteristic aroma components obtained from tobacco by various physical and chemical means, and then other components are added for regulation and preparation. Therefore, the extraction of characteristic components in tobacco is the technical basis of electronic cigarette liquid (tobacco tar).

The existing research shows that the burning and smoking process of the traditional cigarette has a combustion area with the temperature of 600 to 1000 ℃, a pyrolysis distillation area with the temperature of 100 to 600 ℃ and a condensation area below 100 ℃. Just because the thermal cracking products generated by combustion are complex and various, the special aroma and taste of the cigarettes are formed. Therefore, the research and analysis of the thermal cracking products in the specific temperature intervals and the extraction of the products have very important technical significance for improving the quality of the electronic cigarette.

Disclosure of Invention

The application aims to provide a tobacco leaf microwave pyrolysis product, thereby laying a foundation for improving and stably promoting the quality of an electronic cigarette.

The technical solution adopted in the present application is detailed as follows.

A tobacco leaf microwave pyrolysis product is prepared by the following steps:

(1) Microwave pyrolysis

Shredding tobacco leaves, placing the shredded tobacco leaves into a container (such as a cracking bottle), and then performing microwave cracking in a cracking furnace;

the tobacco leaves are, for example, strong aromatic tobacco leaves or leaf groups (or tobacco leaves or leaf groups such as redried tobacco strips, burley tobacco and sun-cured tobacco);

before cracking, preferably, the cut tobacco after shredding is balanced for 24 hours at the temperature of 22 ℃ and the relative humidity of 60 percent, and then cracking operation is carried out;

during specific cracking, the microwave cracking power is 500W-1000W, and the cracking time is 60-300s;

(2) Extraction of

Extracting the cracked product subjected to microwave cracking in the step (1) by using an organic solvent, and removing an extracting agent (the organic solvent) after extraction is finished to obtain a cracked product;

the organic solvent (extractant) is one or more of ethanol, dichloromethane, ethyl acetate, acetone, etc. in any proportion, preferably ethanol;

in the specific extraction operation, the cleavage product: organic solvent =1g:5 to 20mL;

and when the extractant is removed after extraction is finished, specifically removing the extractant by using a reduced pressure concentration heating mode, specifically, increasing the heating temperature to 45-60 ℃ under the condition that the initial value of the reduced pressure concentration heating temperature is 25-35 ℃ and no liquid drops, and keeping the temperature for 10-20 min under the condition that no liquid drops so as to ensure that the solvent is completely removed.

The electronic cigarette liquid prepared by using the tobacco leaf microwave pyrolysis product comprises the tobacco leaf microwave pyrolysis product and an atomizing agent; the microwave pyrolysis product of tobacco leaves is as follows by volume ratio: atomizing agent =1, 15 to 30 (V: V);

the atomizing agent comprises propylene glycol and glycerol =2 to 10 (V: V).

In specific application, the addition amount of the electronic cigarette liquid in an electronic cigarette cartridge is 0.3 to 0.8g.

The main technical idea of the application is as follows: firstly, tobacco leaves are cracked under the condition of simulating cigarette combustion through a microwave cracking technology, and then cracking products are separated through an extraction technology to obtain characteristic components of the tobacco leaves, so that the aroma quality of the electronic cigarette is improved.

Generally, compared with the existing electronic cigarette liquid preparation method, the method has the following technical advantages:

(1) Because the cracking operation is carried out firstly, compared with the conventional preparation method, the tar and other harmful substances can be effectively reduced during the subsequent extraction;

(2) After the components obtained after extraction are further prepared into the electronic cigarette liquid, the herbal fragrance of the electronic cigarette can be effectively improved, so that the electronic cigarette has the characteristic fragrance of the herbal fragrance of the traditional cigarette, and the sensory qualities of strength, satisfaction and the like are improved.

Drawings

FIG. 1 is a graph of the effect of different microwave lysis times on volatile flavour components;

FIG. 2 shows the effect of different microwave cleavage powers on volatile flavour components.

Detailed Description

The present application is further explained with reference to the following embodiments so that those skilled in the art can more clearly understand the technical solutions of the present application, and before describing the specific embodiments, the following embodiments are briefly described with reference to some experimental materials, experimental backgrounds, and the like.

Experimental materials:

flue-curing: schchang B011 and schchang C076 in Henan;

burley tobacco: enshi B1F in Hubei;

experimental equipment:

CM-02S type microwave pyrolysis furnace, nanjing zemu microwave science and technology Co., ltd;

agilent model 7890B/5977A gas chromatography-mass spectrometer, agilent, USA.

Example 1

In this example, flue-cured tobacco leaves of schchang B011 from southern Henan were subjected to microwave pyrolysis, and the specific preparation process is briefly described as follows.

(1) Microwave pyrolysis

After tobacco leaves of flue-cured tobacco of Schachang B011 in Henan are shredded, the tobacco leaves are balanced (the temperature is 22 ℃, and the relative humidity is 60 +/-2% RH) for 24 hours, then 50g of the tobacco leaves are taken and placed in a quartz cracking bottle, and the quartz cracking bottle is placed in the center of a furnace chamber of a cracking furnace for microwave cracking;

during specific cracking, the microwave cracking power is 900W, and the cracking time is 120s.

(2) Extraction of

And (2) extracting the cracked product subjected to microwave cracking in the step (1) by using 100mL of absolute ethanol, concentrating under reduced pressure after extraction is finished, heating to 30 ℃, raising the heating temperature to 45 ℃ under the condition that no solvent is distilled out, and keeping for 20 min to ensure that the solvent is completely distilled out.

The electronic cigarette liquid prepared by utilizing the tobacco leaf microwave pyrolysis product comprises electronic cigarette oil and an atomizing agent; the microwave pyrolysis product of tobacco leaves is as follows by volume ratio: nebulant =1 (V: V);

the atomizing agent is prepared from propylene glycol and glycerol =5 (V: V).

In specific application, the addition amount of the electronic cigarette liquid in the electronic cigarette cartridge is 0.5g, and sensory evaluation is performed by using an electronic cigarette gun, and specific results are shown in the following table 2.

It should be noted that, taking burley tobacco as an example, the inventor has performed optimization experimental verification for the microwave cracking time and microwave cracking power in step (1), and the specific situation is briefly described as follows.

(1) Microwave pyrolysis time

Referring to the above operation, the microwave cracking power is set at 900W, the amount and total content of the cracked volatile components are used as evaluation indexes, and the influence of the cracking time is examined, and the result is shown in FIG. 1.

As can be seen from FIG. 1, the amount and content of volatile aroma substances in the cleavage product increased and then decreased with the increase of the cleavage time, and reached a maximum at 120s and then decreased. Therefore, the cracking time is more suitable within the range of 60 to 150s, and the optimal microwave cracking time is 120s.

(2) Microwave cracking power

Referring to the above operation, the microwave cracking time is set to 120s, the amount and total content of the cracked volatile components are used as evaluation indexes, and the effect of cracking power is examined, with the result as shown in fig. 2.

As can be seen from FIG. 2, the content of volatile flavor substances and the amount of the flavor substances in the microwave pyrolysis product both show a continuously increasing trend below 900W of power, but show a significant decrease when the microwave power reaches 1000W; therefore, the optimal microwave power is about 800 to 900W.

(3) Compared with the prior method

Further, the inventor takes CN105077570A (a tobacco extract pyrolysis product and its application in novel tobacco products) of the prior art as a control, takes burley tobacco as an example, and respectively prepares the electronic cigarette oil by using the optimized preparation method and the prior art (also taking the optimized mode in the prior art as an experimental basis), and performs GC-MS analysis.

During GC-MS analysis, the specific method comprises the following steps: respectively taking 1g of the electronic cigarette oil prepared by the two methods, adding 20mL of dichloromethane solvent with internal standard, carrying out ultrasonic oscillation for 30min, taking 1mL of extract, passing through an organic membrane with the diameter of 0.45 mu m, carrying out sample injection, and determining the content of the fragrant substances.

A summary of the comparisons of the major flavor components in the tobacco products prepared by the two methods is shown in Table 1 below:

TABLE 1 comparative analysis (unit: mg/g) of the main flavor components in tobacco tar prepared by two methods

。

As can be seen from the table above, the contents of the main flavor substances obtained by the method of the patent are higher than those in the prior CN105077570A, and the method shows better improvement effect.

Examples 2 to 3

Example 2 and example 3 take cured tobacco leaf of schchang C076 in the south of the river and B1F tobacco leaf of hakuri north of hushi as examples respectively, electronic tobacco tar and electronic tobacco liquid are prepared, and the specific preparation process is the same as example 1.

Similarly, using schchang B011, schchang C076 in the river south, and schbei engshi B1F as raw materials, the inventors prepared electronic cigarette oil and electronic cigarette liquid, respectively, by the method described in the existing CN105077570A (the optimized method is used as the experimental basis).

Further, sensory evaluation was performed on each of the examples and the control samples, and the results are summarized in table 2 below.

TABLE 2 sensory evaluation results comparison

。

It can be seen from the above table that the sensory quality of the electronic cigarette oil prepared by the method of the present patent is obviously superior to that of the electronic cigarette oil prepared by the method of the present patent CN105077570A, and the sensory evaluation effect of the electronic cigarette oil is outstanding compared with that of the electronic cigarette oil prepared by the method of CN105077570A, the amount of the cigarette is sufficient, and the coordination is good.

Claims

1. A microwave pyrolysis method for increasing the content of flavor substances in tobacco leaf microwave pyrolysis products is characterized by comprising the following steps:

(1) Microwave pyrolysis

Shredding tobacco leaves, and performing microwave pyrolysis;

before cracking, balancing the shredded tobacco for 24h at 22 ℃ and relative humidity of 60 +/-2%, and then cracking;

the microwave cracking power is 900W, and the cracking time is 120 s;

the tobacco leaves are burley tobaccos;

the fragrance material is: 2-furfural, 2-furfuryl alcohol, DDMP, solanone, beta-damascenone, dihydroactinidiolide, megastigmatrienone, nicotine, 4-hydroxy-beta-dihydrodamascenone, alpha-ionone, farnesol, ethyl palmitate, cembretriene-4 alcohol, methyl linolenate, phytol, ethyl linoleate, ethyl oleate, ethyl linolenate and ethyl stearate;

(2) Extraction of

Extracting the cracked product subjected to microwave cracking in the step (1) by using an organic solvent, and removing the organic solvent after extraction is finished to obtain a cracked product;

the organic solvent is ethanol.