CN114711455B

CN114711455B - Preparation method and application of alkaline flavor components with characteristics of Canadian tobacco smoke

Info

Publication number: CN114711455B
Application number: CN202210229934.7A
Authority: CN
Inventors: 许高燕; 许利平; 帖金鑫; 刘崇盛; 高阳; 张丽娜; 吴兆明; 廖付; 王辉; 吴继忠; 李石头; 毕一鸣; 杨靖
Original assignee: Zhengzhou University of Light Industry; China Tobacco Zhejiang Industrial Co Ltd
Current assignee: Zhengzhou University of Light Industry; China Tobacco Zhejiang Industrial Co Ltd
Priority date: 2022-03-10
Filing date: 2022-03-10
Publication date: 2022-12-23
Anticipated expiration: 2042-03-10
Also published as: CN114711455A

Abstract

The method takes the whole smoke components of the Canadian tobacco leaves as objects, and avoids the problem of loss of partial flavor components caused by only collecting smoke particle phase substances; meanwhile, the characteristic alkaline aroma fraction is selectively prepared by adopting a method of combining silica gel column chromatography and gel chromatography, so that not only can the characteristic aroma components showing the Canadian tobacco leaf style be accurately screened out, but also the characteristic components can be further enriched, therefore, the extraction efficiency is high, and the content of the effective components is high; after the additive is added into a reference cigarette, the aroma characteristics of Canadian cigarettes can be well reproduced, so that the sensory quality of the cigarettes is improved; meanwhile, the invention has simple equipment, convenient operation and convenient popularization.

Description

Preparation method and application of alkaline flavor component characteristic of Canadian tobacco smoke

Technical Field

The invention belongs to the field of separation and preparation of tobacco flavors and fragrances, and particularly relates to a preparation method and application of alkaline fragrant components with characteristics of Canadian tobacco smoke.

Background

As is known to all, cigarettes are a favorite product, the original aroma quality of tobacco leaves is influenced along with the great reduction of tar amount, tar reduction and aroma retention technologies become the key for restricting the development of low-tar cigarettes at present, and the difficulty of the tar reduction is increased particularly under the condition that the tar amount is greatly reduced, the smoking taste of the cigarettes is maintained, and the tar is further reduced greatly. How to reduce the tar content of the cigarettes and enable the fragrance of the cigarettes to be accepted by consumers still becomes a main subject of the cigarette industry and is also a key factor influencing the tar reduction of cigarette products in China. At present, food flavors and fragrances are added into cigarettes, but with the gradual regulation and strictness of the requirement of the Ministry of health on the addition of the food flavors and fragrances, grains, fruits, aquatic products, dairy products and the like advocate not to add the flavors and fragrances as much as possible, so that the great problem is also provided for the tobacco flavor compensation technology, and the flavor compensation technology becomes the important research content and direction of Chinese cigarettes.

The aroma substances in the smoke are important chemical components affecting the quality of the cigarette. The research on the flavor components in the main stream smoke of the cigarette can most directly understand the interrelation between the flavor components and the sensory effect, thereby providing important information for the flavoring and casing of the cigarette. Although traditional tobacco extracts can well compensate the cigarette fragrance, because the components are not selectively separated, and the components contain substances which have negative effects on the smoking taste of cigarettes, the smoking taste is increased, and side effects such as uncomfortable smoking taste, rough feeling, dry feeling and the like are brought. Therefore, it is particularly necessary to selectively separate the tobacco extract. However, the cigarette smoke has various components and different functions, and most substances in the smoke are trace components, so that the difficulty in separating and identifying key components in the smoke is further increased.

Researches show that the alkaline components in the cigarette smoke mainly comprise nitrogen heterocyclic nicotine and a small amount of pyridine, pyrazine, pyrrole and other components. Nicotine mainly has important influence on satisfying the strength of smoking taste and endowing the tobacco with physiological strength, and pyrazine and pyridine compounds are very important compounds forming the characteristic aroma of the main stream smoke of the cigarette, most of the compounds have strong burnt aroma and baking aroma, are very easy to coordinate with the inherent aroma of the tobacco, can well modify and improve the natural tobacco aroma, can cover partial miscellaneous gas, and improve the aftertaste, thereby being concerned. Because the contents of pyrazine and pyridine are very low, the separation and preparation of the flavor components with very low contents are difficult, so that a large amount of components which have small contribution to the flavor components of cigarettes are removed, and the low-content key alkaline flavor components are enriched, thereby having important practical guiding significance for tobacco flavor blending. For example, in CN 20121024589.6, "a method for separating basic flavor components from mainstream smoke of cigarette" and its application ", a collected smoke particulate matter is subjected to steps of extraction, acid washing, concentration, vacuum distillation, etc. to obtain a fraction with a low alkaloid content, then the fraction is subjected to preparative gas chromatography to separate to obtain 5 fractions, and a fraction SF4 with an obvious sensory effect is selected by combining sensory evaluation, wherein the main substances of the fractions are 2-ethylpyrazine, 2, 5-dimethylpyrazine, 2, 6-dimethylpyrazine and 2, 3-dimethylpyrazine. Although the method can separate alkaline components, the separation effect is unsatisfactory, only a few key pyrazine components are contained in the target fraction, pyridine components which have obvious effects on sense organs are lacked, and the aroma characteristics of high-quality tobacco leaves cannot be accurately and completely reproduced.

The Canadian tobacco leaves are taken as a representative of high-quality tobacco leaves, and have unique style characteristics of 'strong, medium and clear, sweet and fragrant' and the like. However, the higher price of imported tobacco leaves puts pressure on the cigarette industry to have higher use cost. Therefore, research and discussion on the development of the Canadian tobacco substitute technology in China have important practical significance for promoting the level of the cigarette industry. Among them, the development and development of high-quality flavor characterizing the leaves of Canadian tobacco is one of effective means.

Disclosure of Invention

The invention aims to separate and prepare characteristic alkaline aroma substances from the smoke based on the flavor components of the Canadian tobacco smoke, thereby obtaining natural tobacco essence, and simultaneously applying the separated characteristic alkaline aroma substances in cigarettes. The essence is derived from tobacco, so that various problems caused by adding non-tobacco essence spice into cigarettes are avoided.

In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:

the invention provides a preparation method of alkaline flavor components characteristic to Canadian tobacco flue gas, which comprises the following steps:

making Canadian tobacco leaf into conventional cigarette, smoking on rotary smoking machine, collecting to obtain Canadian tobacco leaf smoke component, sequentially extracting and acid washing to obtain alkaline component of smoke, and separating by normal phase silica gel column chromatography and gel chromatography to obtain the final product. The method comprises the following specific steps:

(1) Extraction: the method comprises the following steps that a Cambridge filter disc is installed on a rotary smoking machine, and two absorption bottles which are connected in series are connected behind a catcher of the rotary smoking machine; methanol is filled in the absorption bottle, and the absorption bottle is placed below 70 ℃ below zero (the mixture of isopropanol and dry ice is trapped by a cold trap); smoking Canadian tobacco cigarettes in the rotary smoking machine, wherein smoke particulate matters are captured by the Cambridge filter disc to obtain a Cambridge filter disc containing smoke particulate matters, and smoke gaseous matters are captured by the methanol to obtain a methanol solution containing smoke gaseous matters; extracting the smoke particulate matter in the Cambridge filter containing the smoke particulate matter by using an organic solvent A to obtain an organic solution containing the smoke particulate matter; combining the organic solution containing the smoke particle phase matter and the methanol solution containing the smoke gas phase matter to obtain a mixed solution, and concentrating under reduced pressure to one twentieth of the volume of the mixed solution to obtain a crude extract (dark brown), namely the smoke components of the Canadian tobacco leaves; the organic solvent A is isopropanol, methyl tert-butyl ether or diethyl ether;

(2) Acid washing: cooling with ice water bath, adding 2-10wt% (preferably 5 wt%) of H into the crude extract of step (1) ₂ SO ₄ Extracting the aqueous solution, combining the aqueous phases to obtain an aqueous extract, adjusting the pH to 11-12 (by using a 5-20% NaOH solution), adding an organic solvent B for extraction (three times), combining the organic phases, and concentrating under reduced pressure (the final volume is convenient for the next sampling) to obtain an organic phase extract; said H ₂ SO ₄ The volume of the aqueous solution is 1-2 times (preferably 2 times) the volume of the crude extract; the organic solvent B is petroleum ether;

(3) Normal phase silica gel column chromatographic separation: performing gradient elution on the organic phase extract in the step (2) by adopting a normal phase silica gel column, sequentially performing elution by using mixed liquids with the following dosage as eluents, collecting the extract as one fraction by eluting one column volume, and sequentially numbering the fractions A1-A24 according to the collection sequence:

7 column volumes of a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 40;

8 column volumes of a mixed solution of petroleum ether and ethyl acetate with the volume ratio of 10;

3 column volumes of a mixed solution of petroleum ether and ethyl acetate with the volume ratio of 3;

the volume ratio of the petroleum ether to the ethyl acetate is 1;

combining fractions A9, A10, A11, A22 and A23, and removing solvent to obtain primary alkaline component isolate;

(4) And (3) gel chromatography separation: and (4) separating the primary alkaline component separated matter obtained in the step (3) by using an LH-20 gel chromatographic column, eluting by using the following solvents in sequence, collecting the eluted alkaline component as one fraction by eluting one column volume, and numbering the fractions as fractions B1-B7 in sequence according to the collection sequence:

and combining the fractions B3 and B5, and removing the solvent to obtain the alkaline flavor components with the characteristics of the Canadian tobacco leaves.

Further, the volume of the methanol in the step (1) is 1/3-1/2 of the volume of the absorption bottle; the volume of the organic solvent A is 20-40 mL/sheet (preferably 30 mL/sheet) based on the number of sheets of the Cambridge filter sheet;

further, the volume of the organic solvent B added in the step (1) is 0.5 to 1 time (preferably 1 time) of the volume of the aqueous extract.

Further, the silica gel used in the normal phase silica gel column in the step (3) is 200-300 meshes, and the volume mass ratio of the organic phase extract to the silica gel is 1mL.

Further, the solvent is removed in step (3) by concentration under reduced pressure.

Further, the solvent is removed in step (4) by concentration under reduced pressure.

Compared with the prior art, the invention has the beneficial effects that:

1. the method takes the whole smoke components of the Canadian tobacco leaves as objects, and avoids the problem of loss of partial aroma components caused by only collecting smoke particle phase substances;

2. meanwhile, the characteristic alkaline aroma fraction is selectively prepared by adopting a method of combining silica gel column chromatography and gel chromatography, so that characteristic aroma components showing the style of Canadian tobacco leaves can be accurately screened out, and characteristic components can be further enriched, therefore, the extraction efficiency is high, and the content of effective components is high;

3. after the additive is added into a reference cigarette, the aroma characteristics of the Canadian cigarette can be well reproduced, so that the sensory quality of the cigarette is improved; meanwhile, the invention has simple equipment, convenient operation and convenient popularization.

Detailed Description

The invention is further illustrated by the following examples, which are given solely for the purpose of illustration and are not intended to limit the scope of the invention.

The cigarettes in the following examples were rolled up in a conventional manner, each cigarette containing 0.7 g of tobacco.

Example 1

(1) Extraction: connecting two absorption bottles connected in series behind a catcher of a rotary smoking machine, collecting smoke particulate matters by using a Cambridge filter disc and a cold trap catching mode to obtain Canada tobacco smoke components, wherein the Cambridge filter disc (the diameter is 92mm, 20 cigarettes smoke are collected by each Cambridge filter disc) is used for collecting smoke particulate matters, the cold trap catching (two absorption bottles filled with 30mL of methanol are connected in series, the absorption bottles are placed in a mixture of isopropanol-dry ice (the temperature is less than or equal to-70 ℃) to obtain smoke particulate matters, soaking 100 Cambridge filter discs for collecting the smoke particulate matters in 1500mL of isopropanol for 120min, then performing ultrasonic extraction for 30min, soaking the Cambridge filter discs in 1500mL of isopropanol for one time, performing ultrasonic extraction to obtain particulate matter extracting solutions, combining the methanol solutions in the cold trap, and concentrating under reduced pressure to 150mL to obtain a concentrated solution of a dark brown crude extract.

(2) Acid washing: subjecting the dark brown crude extract obtained in step (1) to 5% by volume of 300mL ₂ The aqueous SO4 solution was extracted 100mL each time 3 times, and the organic and aqueous phases were separated. The aqueous phase was adjusted to pH =12 with 10% sodium hydroxide solution and the process was cooled with an ice water bath to prevent loss of volatile components due to temperature increase, then extracted with additional 100mL of petroleum ether and separated by shaking thoroughly in a separatory funnel. The extraction process is repeated for 3 times, organic phases are combined, and the mixture is decompressed and concentrated to 5mL, namely the alkaline component of the Canadian tobacco leaf smoke.

(3) Normal phase silica gel column chromatographic separation: and (3) taking 5mL of the organic phase extract obtained in the step (2), performing gradient elution by adopting a normal phase silica gel column at room temperature, wherein the flow rate of an eluent is 10mL/min, and filling 200 g of 200-300-mesh silica gel into the silica gel column. When the organic phase extract is separated by column chromatography, the organic phase extract is collected in an equal volume by adopting a gradient elution mode, wherein the gradient elution adopts a gradient eluent with gradually increased polarity, and the composition and the dosage of the eluent are shown in table 1. Every 200ml is one fraction, 24 elution fractions A1-A24 are obtained in total, after GC-MS analysis, key alkaline components are mainly concentrated in fractions A9, A10, A11, A22 and A23, and after 5 fractions are combined, the solvent is removed by decompression concentration under the conditions that the vacuum degree is 400-800mbar and the water bath temperature is 30-50 ℃ to obtain an alkaline component primary isolate.

TABLE 1 composition and elution volume of eluent

(4) And (3) gel chromatography separation: and (4) separating the basic component preliminary separation substance obtained in the step (3) at room temperature by using an LH-20 gel chromatographic column, wherein the flow rate of an eluent is 2mL/min, and the basic component preliminary separation substance is collected in an isovolumetric manner by adopting a gradient elution mode, and the composition and the dosage of the eluent are shown in a table 2. Each 50ml fraction is used to obtain 7 elution fractions B1-B7, and the 7 elution fractions are subjected to GC-MS analysis after solvent removal by reduced pressure concentration under the conditions that the vacuum degree is 700mbar and the water bath temperature is 35 ℃. In combination with literature and experience, pyrazine and pyridine compounds are widely considered as very important compounds forming characteristic aroma of cigarette mainstream smoke, most of the compounds have strong burnt aroma and baking aroma, are very easy to coordinate with inherent aroma of tobacco, can well modify and improve natural tobacco aroma, can cover partial miscellaneous gas, and improve aftertaste. As can be seen from Table 3, B3 is mainly pyridines, mainly comprising 3, 5-lutidine, 2,4, 6-collidine and 3-ethylpyridine in an amount of 44.3%; from table 4, it can be seen that B5 is mainly pyrazine compounds, the main components are 2, 3-dimethylpyrazine, 2, 5-dimethylpyrazine, 2-ethyl-6-methylpyrazine and 2-ethylpyrazine, the content is 39.1%, these are alkaline components having important effect on sense organ, therefore, combining B2 and B5, and then concentrating under reduced pressure under the conditions of vacuum degree of 400-800mbar and water bath temperature of 30-50 ℃ to remove the solvent, namely the alkaline flavor components characteristic to the canadian tobacco leaves.

TABLE 2 composition and elution volume of eluent

TABLE 3 GC-MS qualitative analysis of the B3 fraction

TABLE 4 GC-MS qualitative analysis of the B5 fraction

(5) Sensory evaluation: diluting 0.1ml of the characteristic alkaline flavor components of the Canadian tobacco leaves obtained in the step (4) into 1% concentration by using 9.9ml of ethanol with volume fraction of 95%, adding 5 mu L of the diluted alkaline flavor components into cigarettes, and performing smoking comparison by using a smoking panel mainly composed of smoking experts in the industry. According to evaluation, compared with a blank cigarette (not added), the cigarette has the advantages that the cigarette is outstanding in baking aroma, fine in smoke and reduced in miscellaneous gas due to the addition of the characteristic alkaline aroma component, the aroma style of Canadian tobacco leaves can be well reproduced, and the sensory quality of the cigarette is improved.

Example 2

The preparation method is the same as that in the example 1 except that 100 Cambridge filter sheets for collecting smoke particulate matters in the step (1) are soaked in 1500mL of diethyl ether for 120min, and finally the characteristic alkaline flavor components of the Canadian tobacco leaves are obtained. Diluting 0.1ml of the obtained canadian tobacco leaf characteristic alkaline flavor component into 1% concentration by using 9.9ml of 95% ethanol in volume fraction, taking 5 mu L of the diluted alkaline flavor component to be added into cigarettes, and performing smoking evaluation comparison by a smoking panel which mainly comprises smoking experts in the industry. According to evaluation, compared with a blank cigarette (not added), the cigarette has the advantages that the cigarette is outstanding in baking aroma, fine in smoke and reduced in miscellaneous gas due to the addition of the characteristic alkaline aroma component, the aroma style of Canadian tobacco leaves can be well reproduced, and the sensory quality of the cigarette is improved.

Example 3

The preparation method is the same as that of the example 1 except that 100 Cambridge filter sheets for collecting smoke particulate matters in the step (1) are soaked in 1500mL of methyl tert-butyl ether for 120min, and finally the characteristic alkaline flavor components of the Canadian tobacco leaves are obtained. Diluting obtained 0.1ml of characteristic alkaline flavor component of Canadian tobacco leaf with 9.9ml of 95% ethanol by volume fraction to 1% concentration, adding 5 μ L into cigarette, and performing smoking comparison by a smoking panel mainly composed of industry smoking experts. According to evaluation, compared with a blank cigarette (not added), the cigarette has the advantages that the cigarette is outstanding in baking aroma, fine in smoke and reduced in miscellaneous gas due to the addition of the characteristic alkaline aroma component, the aroma style of Canadian tobacco leaves can be well reproduced, and the sensory quality of the cigarette is improved.

Example 4

Except that the dark brown crude extract obtained in step (2) was used 4% H in a volume of 250mL ₂ The preparation method is the same as that in example 1 except that the SO4 solution is extracted, and finally the alkaline flavor components with the characteristics of the Canadian tobacco leaves are obtained. Diluting 0.1ml of the obtained canadian tobacco leaf characteristic alkaline flavor component into 1% concentration by using 9.9ml of 95% ethanol in volume fraction, taking 5 mu L of the diluted alkaline flavor component to be added into cigarettes, and performing smoking evaluation comparison by a smoking panel which mainly comprises smoking experts in the industry. The evaluation shows that compared with a blank cigarette (not added), the cigarette has outstanding baking aroma, fine smoke and reduced offensive odor due to the addition of the characteristic alkaline aroma components, can better reproduce the aroma style of Canadian tobacco leaves, and improves the sensory quality of the cigarette.

Example 5

The preparation method is the same as that of example 1 except that the aqueous phase is adjusted to pH =12 with 10% sodium hydroxide solution in step (2), and the process is cooled with ice water bath, and finally the alkaline flavor component characteristic to the canadian tobacco leaves is obtained. Diluting obtained 0.1ml of characteristic alkaline flavor component of Canadian tobacco leaf with 9.9ml of 95% ethanol by volume fraction to 1% concentration, adding 5 μ L into cigarette, and performing smoking comparison by a smoking panel mainly composed of industry smoking experts. According to evaluation, compared with a blank cigarette (not added), the cigarette has the advantages that the cigarette is outstanding in baking aroma, fine in smoke and reduced in miscellaneous gas due to the addition of the characteristic alkaline aroma component, the aroma style of Canadian tobacco leaves can be well reproduced, and the sensory quality of the cigarette is improved.

Example 6

The preparation method is the same as that of example 1 except that the aqueous phase is adjusted to pH =12 with 12% sodium hydroxide solution in step (2), and the process is cooled with ice water bath, and finally the alkaline flavor component characteristic to the canadian tobacco leaves is obtained. Diluting obtained 0.1ml of characteristic alkaline flavor component of Canadian tobacco leaf with 9.9ml of 95% ethanol by volume fraction to 1% concentration, adding 5 μ L into cigarette, and performing smoking comparison by a smoking panel mainly composed of industry smoking experts. The evaluation shows that compared with a blank cigarette (not added), the cigarette has outstanding baking aroma, fine smoke and reduced offensive odor due to the addition of the characteristic alkaline aroma components, can better reproduce the aroma style of Canadian tobacco leaves, and improves the sensory quality of the cigarette.

Comparative example 1

Except that the composition of the eluent in the step (3) was n-hexane-diethyl ether, the volume ratio was the same as in table 1, and the other preparation methods were the same as in example 1, and the compositions of characteristic basic flavor components B3 and B5 of the finally obtained canadian tobacco leaves are shown in tables 5 and 6. Diluting 0.1ml of alkaline flavor component with volume fraction of 95% ethanol 9.9ml to 1% concentration, adding 5 μ L into cigarette, and performing smoking comparison by a smoking panel mainly composed of industry smoking experts. The evaluation shows that compared with a blank cigarette (not added), the cigarette has the advantages that the cigarette smoke is fine and smooth, the baking aroma is prominent, the scorching aroma is slightly insufficient, the smoke amount is slightly reduced, and the aroma style of the Canadian tobacco can be reproduced to a certain degree.

TABLE 5 GC-MS qualitative analysis of the B3 fraction

TABLE 6 GC-MS qualitative analysis of the B5 fraction

Comparative example 2

The preparation method is the same as that in example 1 except that the composition of the eluent in the step (4) is dichloromethane-methanol, the volume ratio is consistent with that in table 2, 0.1ml of the finally obtained alkaline flavor components with the characteristics of the Canadian tobacco leaves is diluted to 1% concentration by 9.9ml of ethanol with the volume fraction of 95%, 5 microlitres of the diluted alkaline flavor components is added into cigarettes, and a smoking panel mainly composed of smoking experts in the industry carries out smoking evaluation comparison. The evaluation shows that compared with a blank cigarette (not added), the cigarette has fine smoke and prominent baking aroma due to the addition of the characteristic alkaline aroma component, but has slightly insufficient scorched aroma, the sensory quality of the cigarette is improved to a certain extent, and the aroma style of the Canadian tobacco can be basically reproduced.

Claims

1. A preparation method of alkaline flavor components characteristic to Canadian tobacco smoke is characterized by comprising the following steps:

(1) Extraction: the method comprises the following steps that a Cambridge filter disc is installed on a rotary smoking machine, and two absorption bottles which are connected in series are connected behind a catcher of the rotary smoking machine; the absorption bottle is filled with methanol and is placed below 70 ℃ below zero; smoking Canadian tobacco cigarettes in the rotary smoking machine, wherein smoke particulate matters are collected by the Cambridge filter disc to obtain a Cambridge filter disc containing the smoke particulate matters, and smoke gaseous matters are collected by the methanol to obtain a methanol solution containing the smoke gaseous matters; extracting the smoke particulate matter in the Cambridge filter containing the smoke particulate matter by using an organic solvent A to obtain an organic solution containing the smoke particulate matter; combining the organic solution containing the smoke particle phase substances with the methanol solution containing the smoke gas phase substances to obtain a mixed solution, and concentrating under reduced pressure to one twentieth of the volume of the mixed solution to obtain a crude extract, namely the smoke components of the Canadian tobacco leaves; the organic solvent A is isopropanol, methyl tert-butyl ether or diethyl ether;

(2) Acid washing: cooling in ice water bath, and adding 2-10wt% of H into the crude extract obtained in step (1) ₂ SO ₄ Extracting with water solution, mixing water phases, adjusting pH to 11-12, adding organic solvent B for extraction, mixing organic phases, and concentrating under reduced pressure to obtain organic phase extract; said H ₂ SO ₄ The volume of the aqueous solution is 1-2 times of the volume of the crude extract; the organic solvent B is petroleum ether;

a mixture of petroleum ether and ethyl acetate in a volume ratio of 40:1, representing 7 column volumes, was recorded as fractions A1-A7

8 column volumes of a mixture of petroleum ether and ethyl acetate in a volume ratio of 10

3 column volumes of a mixture of petroleum ether and ethyl acetate in a volume ratio of 3

Mixing a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 1:1 for 6 column volumes, recording as fractions A19-A24, combining fractions A9, A10, A11, A22 and A23, and removing a solvent to obtain an alkaline component primary isolate;

(4) And (3) gel chromatography separation: and (3) separating the primary alkaline component isolate obtained in the step (3) by using an LH-20 gel chromatographic column, eluting by using the following solvents in sequence, collecting the eluate as one fraction by eluting one column volume, and numbering the fractions as fractions B1-B7 in sequence according to the collection sequence:

1 column volume of dichloromethane, noted B1

1 column volume of a mixed solution of dichloromethane and ethanol with a volume ratio of 80

1 column volume of a mixture of dichloromethane and ethanol with a volume ratio of 60

The volume ratio of dichloromethane to ethanol mixed solution is 40

1 column volume of a mixed solution of dichloromethane and ethanol with a volume ratio of 20

Ethanol 1 column volume, denoted B7

2. The process of claim 1, wherein the process comprises the steps of: the volume of the methanol in the step (1) is 1/3-1/2 of the volume of the absorption bottle.

3. The method for preparing alkaline flavor components characteristic of Canadian tobacco smoke according to claim 1, comprising: the volume of the organic solvent A in the step (1) is 20-40 mL/piece based on the number of the Cambridge filter pieces.

4. The method of preparing the alkaline flavor components characteristic of Canadian tobacco smoke according to claim 3, comprising: the volume of the organic solvent A in the step (1) is 30 mL/sheet based on the number of the Cambridge filter sheets.

5. The process of claim 1, wherein the process comprises the steps of: the volume of the added organic solvent B in the step (1) is 0.5-1 time of that of the water phase.

6. The method of preparing alkaline flavor components characteristic of the flue gas of canadian tobacco leaves according to claim 5, wherein: the volume of the added organic solvent B in the step (1) is 1 time of that of the water phase.

7. The process of claim 1, wherein the process comprises the steps of: said H in step (2) ₂ SO ₄ The volume of the aqueous solution was 2 times the volume of the crude extract.

8. The process of claim 1, wherein the process comprises the steps of: the silica gel used by the normal phase silica gel column in the step (3) is 200-300 meshes, and the volume mass ratio of the organic phase extract to the silica gel is 1mL.

9. The method for preparing alkaline flavor components characteristic of Canadian tobacco smoke according to claim 1, comprising: the solvent removal in step (3) is carried out by concentration under reduced pressure.

10. The method for preparing alkaline flavor components characteristic of Canadian tobacco smoke according to claim 1, comprising: the solvent is removed in step (4) by concentration under reduced pressure.