CN104621709B - Flue-cured tobacco extract and electronic cigarette liquid - Google Patents

Abstract

The invention discloses a flue-cured tobacco extract and an electronic cigarette liquid. The flue-cured tobacco extract uses tobacco leaves, shredded tobacco, tobacco powder and/or soot as raw materials, and adds an extraction solvent in a Soxhlet extractor to carry out Soxhlet extraction of the raw materials. The improvement is to connect a vacuum pump to the condenser tube of the Soxhlet extractor , so that the vacuum in the Soxhlet extractor is maintained at 20-80mmHg; the temperature of the condensate in the condensation tube is below -5°C; after the Soxhlet extraction is completed, the extract is collected, and the extract is concentrated to obtain flue-cured tobacco extraction things. The invention puts the whole Soxhlet extraction system in a negative pressure state, lowers the boiling point of the extraction solvent, lowers the extraction temperature, accelerates the solvent circulation during the extraction process, accelerates the extraction frequency, and has higher efficiency. At the same time, due to the lower heating temperature of the solvent and milder extraction conditions, the excessive chemical reaction between the aroma components in the extract caused by the high temperature heating of the solvent is avoided, and the extract has less miscellaneous gas.

Description

A flue-cured tobacco extract and electronic cigarette liquid

technical field

The invention belongs to the technical field of electronic cigarettes, in particular to a flue-cured tobacco extract and electronic cigarette liquid.

Background technique

As a new type of tobacco product, electronic cigarette liquid determines the sensory style characteristics of electronic cigarette, so the preparation of electronic cigarette liquid becomes the key to electronic cigarette products. The basic technical principle of the electronic cigarette is that when smoking the electronic cigarette, the battery of the electronic cigarette supplies power to the atomizer of the electronic cigarette, the atomizer starts to work, and atomizes the liquid stored in the electronic cigarette to generate smoke. The smoke liquid in electronic cigarettes, also known as "smoke oil", is stored in absorbent materials, commonly known as "adsorbent cotton". The liquid in the e-cigarette is actually a formula essence, which is atomized into "smoke" when smoking the e-cigarette. The smoke includes glycerin, propylene glycol and other substances volatilized from the essence, as well as the aroma substances volatilized from the essence. E-cigarette liquid is the source of the aroma of e-cigarettes, which determines the taste and style of e-cigarettes and whether the products are accepted by consumers. Therefore, the liquid formulation technology of electronic cigarettes is one of the key technologies of electronic cigarettes. The e-cigarette liquid mainly includes two parts, one is the aromatizer, and the other is the basic solvent for dissolving the aromatizer. In addition, some auxiliary materials can be added to meet the needs of different groups of people. Among them, the aroma of the e-cigarette is mainly provided by the aromatizer. The fragrance-inducing substance is a mixture of various spices, and tobacco extract is mostly used.

At present, tobacco extraction methods in a broad sense include high-temperature extraction methods such as high-temperature dry distillation or distillation or steam distillation, and solvent heating and reflux methods. Among the many tobacco extraction methods, high-temperature extraction methods such as dry distillation or distillation, while obtaining the aroma components of tobacco, because high-temperature heating will inevitably destroy the aroma of the tobacco itself, and high-temperature heating will also bring about deep reactions. It will bring unnecessary miscellaneous gas to the extract and affect the sensory quality evaluation of the extract. Traditional solvent extraction methods mostly use organic solvents mixed with tobacco and placed in a flask to heat, or until boiling, to increase the solubility of the organic solvent, dissolve the spices in the tobacco, then filter, and concentrate the filtrate to obtain the extract. This traditional method, 1. The extraction efficiency is not high, because a certain solvent is easy to reach saturation, and the required aroma components can no longer be extracted from the tobacco; 2. In order to improve the extraction efficiency, it will be heated until reflux, and the temperature will rise to the solvent. The boiling point will also bring unnecessary miscellaneous gases to the extracted product; 3. Filtration is required after extraction, especially for the filtration after soot extraction, which is very time-consuming.

At present, a common problem with e-cigarette products is that e-cigarette liquids lack or have weak tobacco flavor characteristics, and some are even closer to food such as chewing gum. There is a large deviation in style from smoking cigarettes, and the overall style is close to food . Therefore, it is necessary to explore the extracts of different types of tobacco leaf raw materials to improve the basic taste, richness, delicateness and satisfaction of electronic cigarettes.

Contents of the invention

The technical problem solved by the present invention is that the e-cigarette liquid lacks or has weak tobacco flavor characteristics.

One of the technical schemes of the present invention is to provide a flue-cured tobacco extract, using tobacco leaves, shredded tobacco, tobacco powder and/or soot as raw materials, adding an extraction solvent in a Soxhlet extractor to carry out Soxhlet extraction of the raw materials. The condensate tube of the extractor is connected to a vacuum pump so that the vacuum in the Soxhlet extractor is maintained at 20 to 80 mmHg; the temperature of the condensate in the condensate tube is below -5°C; after the Soxhlet extraction is completed, collect and extract liquid, and concentrate the extract to obtain flue-cured tobacco extract.

Further, the extraction solvent is ethanol, n-hexane, cyclohexane or petroleum ether.

Further, the condensing tube used in the Soxhlet extraction is a serpentine condensing tube.

Further, the extraction time of the Soxhlet extraction is 3-8 hours.

Further, the volume of the extraction solvent is 14-30 times the volume of the raw material.

Further, before the Soxhlet extraction, the raw material is soaked in an extraction solvent for 4-8 hours.

Further, ultrasonic or microwave extraction is performed on the soaked raw materials for 0.5-1 h.

Another technical solution of the present invention is to provide an electronic cigarette liquid, which is obtained by dissolving the above-mentioned flue-cured tobacco extract in a base solvent. The base solvent is a mixture of glycerin, propylene glycol, ethanol, water or three of them. Wherein, the distribution of mass percentage is as follows: 0-20% of water, 60-70% of glycerin, 0-20% of ethanol, and 0-20% of propylene glycol.

Flue-cured tobacco has a special roasted aroma, strong strength and good aroma retention. The invention extracts the flue-cured tobacco, prepares the flue-cured tobacco extract as the e-cigarette liquid, and increases the special flavor of the e-cigarette.

The present invention aims to provide a raw material extract of flue-cured tobacco. According to the formula requirements, flue-cured tobacco leaves from different production areas and different parts, or cut into shredded tobacco, or ground into tobacco powder are used as raw materials, and ethanol, n-hexane, cyclohexane or petroleum Repeated extraction at low temperature with non-toxic or slightly toxic organic solvents such as ether. In order to achieve low-temperature repeated extraction, the Soxhlet extraction device was improved, and a glass three-way valve was connected to the vacuum pump at the upper end of the condenser tube of the Soxhlet extractor to maintain the vacuum at 20-80mmHg, so that the solvent can be used at a lower temperature. Boiling avoids side reactions caused by excessive temperature. The condensing tube is a serpentine condensing tube, and the size of the condensing tube can be lengthened. The condensing tube is fed with low-temperature circulating condensate, and the temperature of the condensate is below -5°C to improve the condensation effect and prevent the solvent from being sucked away by the vacuum pump. After reducing the boiling point of the solvent under reduced pressure, the cycle speed of solvent evaporation and cooling is accelerated, and the extraction frequency is accelerated. The extraction is carried out under milder temperature conditions, which avoids excessive chemical reactions between the aroma components in the extract caused by high temperature heating of the solvent. Sensory evaluation It is believed that the extract under mild conditions has less miscellaneous gas and the taste of smoke is purer.

The preferred extraction solvent of the present invention is ethanol or n-hexane or cyclohexane or petroleum ether. For the same tobacco leaf raw material, based on the polarity and boiling point of the solvent, the content of each aroma component in the final extract is different. For example, the content of polar aroma components in aroma substances extracted from strong polar solvents will increase; similarly, the content of non-polar aroma components in aroma substances extracted from weak polar solvents will increase. According to the extracts obtained by extraction with different polar solvents, according to the needs of the formula, different formula requirements can be met. For example, the advantage of ethanol extract is that ethanol solvent will not bring solvent miscellaneous gas, and has obvious advantages in sensory evaluation. In addition, it is a polar solvent, and it is easy to extract polar aroma components in tobacco leaves. Compared with ethanol, n-hexane has less polarity, and its extraction effect on non-polar aroma components in tobacco leaves is better than that of ethanol. Therefore, n-hexane tobacco leaf extracts are often strong and satisfying, but the disadvantage is that the extracts are slightly miscellaneous.

The volume of the extraction solvent is 14 to 30 times the volume of the raw material, which can fully dissolve the spices in the tobacco without wasting the solvent. The extraction time is 4 to 8 hours, which can ensure the full dissolution of the spices and avoid the generation of miscellaneous gases by heating for a long time. After the extraction is completed, the extract is collected, concentrated under reduced pressure, and dissolved in the base solvent to be used as e-cigarette liquid. The electronic cigarette made of the electronic cigarette liquid can improve the smoke quality of the electronic cigarette, improve the flavor, and increase the sense of satisfaction.

The described extraction experimental device is optimized and improved on the basis of the Soxhlet extraction device. The important improvement is to connect a vacuum pump to the top of the Soxhlet extraction, so that the entire extraction system is in a negative pressure state, so as to reduce the boiling point of the extraction solvent and make the extraction The lower the temperature, the faster the solvent circulation during the extraction process, the faster the extraction frequency, and the higher the extraction efficiency at the same time. For example, if ethanol is used as the extraction solvent and Soxhlet extraction is performed under normal pressure, the water bath heating needs to be set at 90°C to allow the solvent to boil and circulate to cool down to meet the extraction requirements; while under reduced pressure, when the negative pressure reaches -0.090Mpa (vacuum degree is about 76mmHg ), the set temperature of the water bath at 55°C can meet the requirements. In the negative pressure state, the solvent has the risk of being sucked away by the vacuum pump. In order to ensure that the solvent can be effectively cooled and recycled repeatedly, the present invention adopts two improvement measures: firstly, extract the condensing pipe and select a serpentine condensing pipe and lengthen the length of the condensing pipe 50%, to increase the solvent condensation distance, so that the condensate can cool the extraction solvent more fully; secondly, feed the low-temperature cooling circulating fluid into the condensation pipe, and the temperature of the condensate is below -5°C, between -10 and -5°C Can basically meet the condensation requirements.

In addition, soaking the raw materials (tobacco leaves or shredded tobacco or tobacco powder or soot) in corresponding solvents for 4-8 hours before extraction can improve the extraction effect. Furthermore, it is better to extract the raw materials soaked in the solvent by ultrasonic or microwave for 0.5-1 hour first, and then to extract them.

The present invention proposes an improved Soxhlet extraction method. The major improvement is that a vacuum pump is connected to the condenser tube of the Soxhlet extraction, so that the whole extraction is in a negative pressure state. Under negative pressure, the boiling temperature of the solvent is significantly reduced, the circulation of fresh solvent is accelerated, the extraction frequency is accelerated, and the extraction efficiency is higher. At the same time, due to the lower heating temperature of the solvent and milder extraction conditions, the excessive chemical reaction between the aroma components in the extract caused by the high temperature heating of the solvent is avoided, and the extract has less miscellaneous gas. Compared with the high-temperature extraction method and the traditional solvent extraction method, the extract obtained in the present invention is obtained at a lower extraction temperature, so the extracted product can better reflect the original taste, and avoids the high-temperature extraction method due to the high temperature in the extraction process. Unnecessary in-depth chemical reactions occur to provide the base flavor of tobacco for e-liquid. The advantage of tobacco extraction method of the present invention is:

(1) The solvent extraction temperature is low, does not destroy the inherent aroma components of tobacco, avoids the excessive chemical reaction between the aroma components in the extract caused by the high temperature heating of the solvent, and the extraction product well maintains the original flavor of the tobacco. Less miscellaneous gas;

(2) The extraction efficiency is high, the boiling temperature of the solvent is reduced under negative pressure, the fresh solvent circulation is accelerated, the extraction frequency is accelerated, the extraction efficiency is increased, and the extraction is complete.

Compared with other tobacco extraction techniques, the present invention has the following technical effects. The present invention inherits the advantages of the Soxhlet extraction method. Firstly, the fresh solvent that circulates repeatedly extracts the aroma components in the raw material of tobacco leaves continuously, and the extraction efficiency is high. The top of the Soxhlet extraction is connected to a vacuum pump, so that the entire extraction system is in a negative pressure state, lowering the boiling point of the extraction solvent, lowering the extraction temperature, accelerating the solvent circulation during the extraction process, increasing the extraction frequency, and the extraction efficiency is higher at the same time. At the same time, due to the lower heating temperature of the solvent and milder extraction conditions, the excessive chemical reaction between the aroma components in the extract caused by the high temperature heating of the solvent is avoided, and the sensory evaluation shows that the extract under mild conditions has less miscellaneous gas.

Description of drawings

Fig. 1 is the schematic diagram of the Soxhlet extraction experimental device used in the present invention.

Fig. 2 is the GC-MS graph of the extract components obtained in Example 1 of the present invention.

Fig. 3 is a GC-MS comparison chart of the extract components obtained in Example 1 and Example 2 of the present invention.

detailed description

The present invention will be further described below in conjunction with specific embodiments. The following examples are intended to illustrate the present invention without further limiting the invention.

The Soxhlet extraction device used in the embodiment is as shown in Figure 1. It is mainly to connect a vacuum pump to the top of the commonly used Soxhlet extraction device to make the Soxhlet extraction under a certain negative pressure. Extractors are used for extraction.

comparative example

Soak 10g of Zimbabwean L10F in 200mL of absolute ethanol for 4h, heat in a water bath for conventional Soxhlet extraction for 4h, set the temperature of the water bath at 90°C, concentrate the extract under reduced pressure until the solvent is dry, and the concentrate is mixed with (5mL of water + 5mL of absolute ethanol +20mL glycerol) dissolved. As an e-cigarette liquid flavoring, the evaluation results are: it has the characteristics of Zimbabwean smoke, and the smoke is full and mellow.

Example 1

Soak 110g of Zimbabwean L10F shredded tobacco in 200mL of absolute ethanol for 4h, and extract it with the improved Soxhlet extraction device of the present invention for 3h, the vacuum degree is 40mmHg, the heating temperature of the water bath is 50°C, the extract is concentrated under reduced pressure until the solvent is dry, and the concentrate is obtained by (5mL water + 5mL absolute ethanol + 20mL glycerin) was dissolved, flavored as e-cigarette liquid, and prepared as a test sample. The e-cigarette produced in the comparative example was used as a control, and the sensory evaluation was carried out. The result of the evaluation and evaluation was: it has obvious characteristics of Zimbabwean smoke, and the smoke is fuller and more mellow. Compared with the control, the flue gas of the test sample is purer. The GC-MS diagram of the obtained flue-cured tobacco extract is shown in Figure 2. Because the peak of nicotine is too large, in order to clearly show other components, the peak that is too high is not completely drawn. In the GC-MS chart of the aroma components in the obtained e-cigarette liquid: 1 is furfural; 2 is 1-(3-pyridine)-ethanone; 3 is DDMP; 4 is 5-hydroxymethylfurfural; 5 is nicotine; 6 For 2,3'-bipyridine; 7 for large column trienone; 8 for N-methoxy-formamide; 9 for pinane. It can be seen from Fig. 2 that the extract of flue-cured tobacco has more furanone compounds and terpene compounds, which are the aroma characteristics of flue-cured tobacco.

Example 2

Soak 10g of Zimbabwe L10F with 200mL of n-hexane for 4h, extract with the improved Soxhlet extraction device of the present invention for 3h, the vacuum degree is 80mmHg, the water bath heating temperature is 45°C, the extract is concentrated under reduced pressure until the solvent is dry, and the concentrate is extracted with (5mL Water + 5mL absolute ethanol + 20mL glycerin) dissolved, flavored as e-cigarette liquid, and tested. Taking the e-liquid prepared in Example 1 as a control, the sensory evaluation and smoking evaluation results are as follows: Compared with the control, the test sample has more energy, a stronger sense of satisfaction, and a little miscellaneous gas.

Fig. 3 is the overlay of the GC-MS diagram of the aroma components in the electronic cigarette liquid obtained in Example 2 and Fig. 2 . It can be seen from Figure 3 that ethanol is a polar solvent, while n-hexane is a non-polar solvent. The aroma components extracted by the non-polar solvent n-hexane are densely distributed in the area with short retention time, that is, the left end of the GC-MS diagram (Note: GC-MS column is a polar column). For example, nicotine in the extract is a polar substance, and it can be seen from Figure 3 that the extraction effect of n-hexane is obviously much weaker than that of the polar solvent ethanol. Figure 3 shows that there are differences in the aroma components extracted by solvents of different polarities. Therefore, the present invention proposes to select different solvents to obtain e-liquid with a particular style to meet the requirements of e-cigarette formulations.

Example 3

Soak Sangzhi B3F Zimbabwe L10F in 200mL of n-hexane for 4h, extract for 3h with the improved Soxhlet extraction device of the present invention, vacuum degree is 80mmHg, water bath heating temperature is 45°C, the extract is concentrated under reduced pressure until the solvent is dry, and the concentrate is (5mL water + 5mL absolute ethanol + 20mL glycerin) is dissolved and used as the e-cigarette liquid for flavoring. Make two samples, one with 0.5ml of commercially available e-cigarette liquid as a control sample; the other as an experimental sample, add 0.5ml of the same commercially available e-cigarette liquid as the control sample, and add another 0.25ml prepared in this example The smoke liquid was extracted from the flue-cured tobacco, and the results of the comparative evaluation and smoking evaluation are as follows: Compared with the control sample, the experimental sample has obvious characteristics of tobacco aroma, strong vigor and strong sense of satisfaction.

Claims (5)

1. a kind of flue-cured tobacco extract, it is characterised in that with the Nicotiana tabacum L. of flue-cured tobacco, tobacco shred, offal and/or flue dust as raw material, in Soxhlet Adding Extraction solvent in extractor carries out surname extraction to raw material, connects vacuum pump, make institute on the condensing tube of apparatus,Soxhlet'ses State the vacuum in apparatus,Soxhlet'ses and maintain 20～80 mmHg, water bath heating temperature is 45-50 DEG C；It is cold in the condensing tube The temperature of lime set is less than -5 DEG C；After the completion of surname extraction, extracting solution is collected, extracting solution is concentrated to give into flue-cured tobacco extract；Institute Condensing tube is stated for serpentine condenser；The extraction time of the surname extraction is 3～8 h；The volume of the Extraction solvent is raw material 14～30 times of volume.

2. flue-cured tobacco extract as claimed in claim 1, it is characterised in that the Extraction solvent is ethanol, normal hexane, hexamethylene Or petroleum ether.

3. flue-cured tobacco extract as claimed in claim 1, it is characterised in that before the surname extraction, raw material is placed in and is carried 4～8 h are soaked in taking solvent.

4. flue-cured tobacco extract as claimed in claim 3, it is characterised in that the raw material after the immersion is carried out ultrasonic or micro- Ripple extracts 0.5～1 h.

5. a kind of electronic cigarette liquid, it is characterised in that the flue-cured tobacco extract described in one of Claims 1 to 4 is dissolved in into base solvent Obtain.