CN110236232B - Electronic tobacco tar prepared by using tobacco leaf extract Maillard reaction product - Google Patents
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Abstract
The application belongs to the technical field of novel tobacco products, and particularly relates to electronic tobacco tar prepared by utilizing a tobacco leaf extract Maillard reaction product. The main technical thought of the application is as follows: firstly, extracting tobacco leaves into extract, then adding amino acid to carry out Maillard reaction, finally carrying out thermal cracking on Maillard reaction products, and extracting to obtain tobacco leaf extract Maillard reaction cracking products with different odor types and fragrance characteristics, thereby laying a foundation for improving the smoking quality of the electronic cigarettes. The electronic cigarette oil prepared by using the Maillard reaction product of the tobacco leaf extract can obviously improve the aroma quality of the smoke of the electronic cigarette, improve the baking aroma and the smoke fineness of the electronic cigarette, reduce the dryness and enable the electronic cigarette to have the natural characteristic aroma of flue-cured tobacco, thereby being closer to the conventional cigarette in the prior art and having better practical value.
Description
Technical Field
The application belongs to the technical field of novel tobacco products, and particularly relates to electronic tobacco tar prepared by utilizing a tobacco leaf extract Maillard reaction product.
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 cigarettes and chewing cigarettes. 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. As one of the core of the electronic cigarette technology, the preparation method and specific components of the electronic cigarette liquid (tobacco tar) are key factors for determining the taste and harm of smoking.
The main components of the electronic cigarette liquid (tobacco oil) 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).
It has been found that Maillard reaction (browning reaction of amino acid and reducing sugar) is an important source of flavor of food, but also of tobacco. Tobacco contains a large number of amino acids and also contains a high content of carbohydrates. During the process of tobacco preparation, aging and fermentation (even during the process of tobacco processing), the two substances can react with each other, thereby endowing different tobaccos with specific aroma and fragrance characteristics and improving the quality of smoke.
Based on the characteristics of the Maillard reaction, in the existing research on the electronic cigarette liquid (tobacco tar), part of research works for improving the smoking quality by utilizing the Maillard reaction exist, but practical evaluation shows that the quality of the electronic cigarette liquid (tobacco tar) still has a further improvement space due to the fact that the Maillard reaction is relatively complex and the inevitable influence of chemical residual reagents in the existing treatment process on the smoking quality.
Disclosure of Invention
The application aims to provide the electronic cigarette oil prepared by utilizing the Maillard reaction product of the tobacco leaf extract, and the main technical idea is that certain kinds of amino acid are added into the tobacco leaf extract to promote the Maillard reaction of the tobacco leaf extract, and then the tobacco leaf extract after the Maillard reaction is subjected to thermal cracking, so that better fragrance and aroma characteristic components are obtained, and certain technical support is provided for improving the quality of the electronic cigarette liquid.
The technical solution adopted in the present application is detailed as follows.
An electronic cigarette oil prepared by using a tobacco leaf extract Maillard reaction product is prepared by the following steps:
(1) preparation of tobacco leaf extract
Shredding tobacco leaves, balancing (temperature 22 ℃, relative humidity 60 +/-2% RH) for 24h, and crushing;
heating and refluxing the tobacco powder crushed in the step (1) by using an organic solvent, and concentrating an extracting solution under reduced pressure to obtain a tobacco leaf extract;
the tobacco leaves are, for example, flue-cured tobacco leaves, burley tobacco leaves, aromatic tobacco leaves, sun-cured tobacco leaves and the like;
specific examples of the organic solvent include ethanol;
during the specific extraction operation, the tobacco powder: organic solvent =1g: 5-9 mL;
during the specific heating reflux operation, the voltage of the electric heating jacket is set to be 100-300V;
after extraction, the initial value of rotary evaporation temperature is 35 ℃, under the condition of no liquid dripping, the heating temperature is increased to 50 ℃, and under the condition of no liquid dripping, the heating temperature is kept for 20 min to ensure that the solvent is completely removed;
(2) carrying out a Maillard reaction
Adding amino acid into the tobacco extract obtained in the step (1) to carry out Maillard reaction, specifically:
the amino acid selection is as follows: one or a mixture of more of glycine, alanine, phenylalanine, histidine, proline, glutamic acid, lysine, leucine and arginine in any proportion;
in the Maillard reaction, propylene glycol is used as a reaction solvent, and the mass ratio of the reaction is as follows:
tobacco leaf extract: amino acids: the proportion of the propylene glycol to the propylene glycol is 3-12 g: 2 g: 30-120 g;
in the Maillard reaction, the reaction temperature is 50-100 ℃, the reaction pH = 7-10, and the reaction time is about 2-10 h;
concentrating under reduced pressure after the reaction, wherein the initial value of the heating temperature of the concentration under reduced pressure is 35 ℃, heating the temperature to 45 ℃ under the condition that no liquid drops, and keeping the temperature for 20 min under the condition that no liquid drops to ensure that the solvent is completely removed;
(3) microwave pyrolysis and extraction
Microwave cracking is carried out on the Maillard reaction product of the tobacco leaf extract obtained in the step (2), and the cracking product is extracted by using an organic solvent, specifically:
during microwave cracking operation, the microwave cracking power is 400W-1000W (preferably 700W-900W), and the microwave cracking time is not more than 200s (preferably 60-200 s, further set to 120s for example);
in the extraction, the organic solvent may be: one or a mixture of more of absolute ethyl alcohol, petroleum ether and dichloromethane in any proportion;
in the extraction operation, the mass volume ratio of the cracking product: organic solvent (extractant) =1:10 g-15 mL;
after extraction, the extract can be further concentrated under reduced pressure for storage and use, and the temperature is 30-50 ℃ during the concentration under reduced pressure.
The electronic cigarette liquid prepared by using the tobacco leaf extract Maillard reaction product comprises electronic cigarette oil prepared by using the tobacco leaf extract Maillard reaction product and an atomizing agent; the electronic tobacco tar is the product of the maillard reaction of the tobacco extract in terms of volume ratio: an atomizing agent =1: 10-20 (V: V);
the atomization agent comprises propylene glycol, glycerol and distilled water = 3-8: 1:1(V: V: V) in volume ratio.
In specific application, the addition amount of the electronic cigarette liquid in the electronic cigarette cartridge (namely, the usage amount of the electronic cigarette liquid in each time) is 0.3-0.6 g.
The main technical thought of the application is as follows: firstly, extracting tobacco leaves into extract, then adding amino acid to carry out Maillard reaction, finally carrying out thermal cracking on Maillard reaction products, and extracting to obtain tobacco leaf extract Maillard reaction cracking products with different odor types and fragrance characteristics, thereby laying a foundation for improving the smoking quality of the electronic cigarettes.
In general, the electronic cigarette oil prepared by using the maillard reaction product of the tobacco leaf extract can obviously improve the aroma of the smoke of the electronic cigarette, improve the baking aroma and the smoke fineness of the electronic cigarette, reduce the dryness and ensure that the electronic cigarette has the natural characteristic aroma of the flue-cured tobacco, thereby being closer to the conventional cigarette in the prior art and having better practical value.
Drawings
FIG. 1 is a graph showing the effect of microwave lysis time on volatile fragrance components;
FIG. 2 shows the effect of microwave pyrolysis power on volatile fragrance 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: northhuche B1F.
Experimental equipment:
CM-02S type microwave pyrolysis furnace, Nanjing zemu microwave science and technology Co., Ltd;
agilent 7890B/5977A GC-MS, Agilent Inc., USA.
Example 1
In this embodiment, flue-cured tobacco leaves of schchang B011 in the south of the river are taken as an example, tobacco leaf extract is specifically prepared, maillard reaction is performed, and electronic tobacco tar is prepared, and the specific process is described as follows.
(1) Preparation of tobacco leaf extract
Shredding cured tobacco leaves of Schchang B011 from Henan, balancing (temperature 22 ℃, relative humidity 60 +/-2% RH) for 24h, and crushing;
weighing 50g of tobacco powder, placing the tobacco powder into a 1000mL round-bottom flask, adding anhydrous ethanol twice (350 mL is added in the two times), heating and refluxing for 3h for extraction, combining the extract, and concentrating under reduced pressure at 40 ℃ to obtain tobacco leaf extract.
(2) Maillard reaction
Weighing 10g of tobacco leaf extract obtained in the step (1), placing the tobacco leaf extract in a 250 mL three-neck flask, and sequentially adding 2g of glycine and 100g of propylene glycol;
putting the three-neck flask into a constant-temperature heating magnetic stirrer to react for 6 hours at the temperature of 60 ℃ and under the condition of pH = 8; after the reaction is finished, carrying out reduced pressure concentration at 40 ℃ to obtain a tobacco extract Maillard reaction product.
(3) Microwave pyrolysis
Weighing 2g of the Maillard reaction product of the tobacco leaf extract obtained in the step (2), placing the weighed product in a 50mL triangular flask, performing microwave pyrolysis, and extracting the pyrolysis product by using an organic solvent, specifically:
during microwave cracking operation, the microwave cracking power is 900W, and the microwave cracking time is 120 s;
during extraction, the organic solvent is absolute ethyl alcohol;
in the extraction operation, the mass volume ratio of the cracking product: organic solvent (extractant) =1g:10 mL;
after the extraction is finished, the extract is further concentrated under reduced pressure for storage and use, and the temperature is 40 ℃ when the extract is concentrated under reduced pressure.
And (3) performing gas-phase mass spectrometry detection on the tobacco extract in the step (1) and the product components of the finally prepared electronic cigarette oil, wherein the results are shown in the following table 1.
The electronic cigarette liquid prepared by using the tobacco leaf extract Maillard reaction product comprises electronic cigarette oil and an atomizing agent; the maillard reaction product of the tobacco leaf extract is calculated according to the volume ratio: nebulizer =1:15 (V: V);
the atomizing agent comprises the following components in percentage by volume, propylene glycol, glycerol and distilled water =5: 1:1(V: V: V).
In specific application, the addition amount of the electronic cigarette liquid is 0.5g, sensory evaluation is performed, and specific results are shown in table 2.
It should be noted that, in step (3), the inventors partially optimize the microwave cracking time and microwave cracking power, and the specific optimization is briefly described as follows.
(1) Microwave pyrolysis time
Referring to the above operation, microwave cracking is performed on the maillard reaction product obtained in the step (2), the microwave cracking power is 900W, statistics is performed on the types and total material content of the cracking products after different cracking time, and the result is shown in fig. 1.
As can be seen from FIG. 1, as the cracking time is prolonged, the amount and content of volatile components obtained from the cracking product both show a trend of increasing first and then decreasing, and in summary, 60-200 s of cracking is a more reasonable cracking time range, and the optimal cracking time is 120 s.
(2) Microwave cracking power
Referring to the above operation, microwave cracking is performed on the maillard reaction product obtained in the step (2), the cracking time is set to 120s, but different microwave cracking powers are set, and the types and total material contents of the cracking products obtained by different cracking powers are counted, and the result is shown in fig. 2.
As can be seen from FIG. 2, with respect to the amount of volatile aroma substances of the cleavage product (i.e., the type of aroma substance), the amount of aroma substances continues to increase with increasing cleavage power, but no more at 900W; and as for the content of the volatile aroma substances of the cracking products, the content of the volatile aroma substances of the cracking products tends to increase and then decrease along with the increase of the cracking power, reaches the highest value at 900W and then gradually decreases. Generally, when the cracking power is 700-900W, the content and the type of the aromatic substances can be better ensured, wherein the quantity and the content of the aromatic substances are better results when the cracking power is 900W. It should be noted that when the cracking power reaches 1000W, the extract will generate burnt smell, so the amount of the aroma substances should be different from the actual amount of the aroma substances, and therefore, the highest power of microwave cracking should be controlled.
Example 2
In this example, schchang C076 tobacco leaves are taken as an example to prepare tobacco leaf extract and electronic tobacco tar respectively, the preparation process is the same as that in example 1, but some operation parameters are adjusted as follows:
in the step (2), during the Maillard reaction, alanine is added for the Maillard reaction, and the material dosage is as follows: 10g of tobacco extract, 2g of alanine and 100g of propylene glycol; the Maillard reaction conditions are as follows: reacting for 4h at 80 ℃ and pH = 7;
in the step (3), during cracking, the microwave cracking power is 900W, and the microwave cracking time is 120 s.
The electronic cigarette liquid prepared by using the tobacco leaf extract Maillard reaction product electronic cigarette oil comprises electronic cigarette oil and an atomizing agent; the electronic tobacco tar is the product of the maillard reaction of the tobacco extract in terms of volume ratio: nebulizer =1:15 (V: V);
the atomizing agent comprises the following components in percentage by volume, propylene glycol, glycerol and distilled water =5: 1:1(V: V: V).
In specific application, the addition amount of the electronic cigarette liquid in the electronic cigarette cartridge is 0.5 g.
The results of the detection of the components of the electronic cigarette liquid and the results of the smoking evaluation of the electronic cigarette liquid prepared in this example are shown in tables 1 and 2 below.
Example 3
In this example, taking the tobacco leaf of hao bei engshi B1F as an example, the tobacco leaf extract and the electronic tobacco tar are prepared separately, the preparation process is the same as that of example 1, but some operation parameters are adjusted as follows:
in the step (2), during the Maillard reaction, alanine is added for the Maillard reaction, and the material dosage is as follows: 10g of tobacco extract, 1g of proline, 1g of glutamic acid and 100g of propylene glycol; the Maillard reaction conditions are as follows: reacting for 4h at 100 ℃ and pH = 7;
in the step (3), during cracking, the microwave cracking power is 900W, and the microwave cracking time is 120 s.
The electronic cigarette liquid prepared by using the tobacco leaf extract Maillard reaction product electronic cigarette oil comprises electronic cigarette oil and an atomizing agent; the electronic tobacco tar is the product of the maillard reaction of the tobacco extract in terms of volume ratio: nebulizer =1:15 (V: V);
the atomizing agent comprises the following components in percentage by volume, propylene glycol, glycerol and distilled water =5: 1:1(V: 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 carried out by using an electronic cigarette gun.
The results of the detection of the components of the electronic cigarette liquid and the results of the smoking evaluation of the electronic cigarette liquid prepared in this example are shown in tables 1 and 2 below.
TABLE 1 comparison of the partial main products after the cracking of tobacco leaf extract after Maillard reaction and the direct cracking of tobacco leaf extract
The analysis and comparison of the results in the table 1 show that after the tobacco extract is subjected to Maillard reaction, the important tobacco flavor components obtained by cracking are obviously higher than the content of the tobacco extract obtained by direct microwave cracking, and the caramel flavor of the smoke can be obviously improved by heterocyclic substances such as DDMP, methyl cyclopentenolone and the like, so that the cavity feeling of the smoke is compensated, and the quality of the existing electronic cigarette liquid can be better improved.
TABLE 2 sensory evaluation results of electronic cigarette liquid prepared by cracking products after Maillard reaction of tobacco leaf extract and electronic cigarette liquid prepared by direct cracking of extract (preparation method and component ratio are the same)
As can be seen from the above table, the sensory evaluation score obtained after the Maillard reaction of the tobacco extract is obviously higher than the sensory evaluation score of the tobacco extract by direct microwave pyrolysis, which indicates that the sensory quality of the electronic cigarette can be improved by adding the Maillard reaction pyrolysis product of the tobacco extract into the electronic cigarette, so that the tobacco fragrance of the electronic cigarette is more prominent, the dry feeling is relatively lower, and the aftertaste is more comfortable.
Claims (9)
1. The electronic cigarette oil prepared by using the Maillard reaction product of the tobacco leaf extract is characterized by being prepared by the following steps:
(1) preparation of tobacco leaf extract
Shredding tobacco leaves, balancing and crushing; heating and refluxing the crushed tobacco powder by adopting an organic solvent, and concentrating the extracting solution under reduced pressure to obtain a tobacco leaf extract;
the tobacco leaves are one or a mixture of more of flue-cured tobacco leaves, burley tobacco leaves, aromatic tobacco leaves and air-cured tobacco leaves in any proportion;
(2) carrying out a Maillard reaction
Adding amino acid into the tobacco extract obtained in the step (1) to carry out Maillard reaction, specifically:
the amino acid selection is as follows: one or a mixture of more of glycine, alanine, phenylalanine, histidine, proline, glutamic acid, lysine, leucine and arginine in any proportion;
in the Maillard reaction, the reaction temperature is 50-100 ℃, the reaction pH = 7-10, and the reaction time is 2-10 h;
after the reaction is finished, carrying out reduced pressure concentration to obtain a tobacco leaf extract Maillard reaction product;
(3) microwave pyrolysis and extraction
And (3) cracking the Maillard reaction product of the tobacco leaf extract obtained in the step (2), and extracting the cracked product by using an organic solvent.
2. The electronic cigarette oil prepared by using the maillard reaction products of the tobacco leaf extract according to the claim 1, wherein in the step (2), during the maillard reaction, propylene glycol is used as a reaction solvent, and the mass ratio during the reaction is as follows:
tobacco leaf extract: amino acids: propylene glycol = 3-12 g: 2 g: 30-120 g.
3. The electronic cigarette oil prepared by using the maillard reaction product of the tobacco leaf extract according to claim 2, wherein in the step (2), during the maillard reaction: tobacco leaf extract: amino acids: propylene glycol =10 g: 2 g: 100 g.
4. The electronic cigarette oil prepared by using the maillard reaction product of the tobacco leaf extract according to the claim 1, wherein in the step (3), microwave cracking is selected for cracking, the microwave cracking power is 400W-1000W, and the microwave cracking time is not more than 200 s.
5. The electronic cigarette oil prepared by using the maillard reaction product of the tobacco leaf extract according to claim 1, wherein the microwave cracking power is 700W-900W, and the microwave cracking time is 60-120 s.
6. The method for preparing electronic cigarette oil by using maillard reaction products of tobacco leaf extract according to claim 1, which is characterized by comprising the following steps:
(1) preparation of tobacco leaf extract
Shredding tobacco leaves, balancing and crushing; heating and refluxing the crushed tobacco powder by adopting an organic solvent, and concentrating the extracting solution under reduced pressure to obtain a tobacco leaf extract;
the tobacco leaves are one or a mixture of more of flue-cured tobacco leaves, burley tobacco leaves, aromatic tobacco leaves and air-cured tobacco leaves in any proportion;
(2) carrying out a Maillard reaction
Adding amino acid into the tobacco extract obtained in the step (1) to carry out Maillard reaction, specifically:
the amino acid selection is as follows: one or a mixture of more of glycine, alanine, phenylalanine, histidine, proline, glutamic acid, lysine, leucine and arginine in any proportion;
in the Maillard reaction, the reaction temperature is 50-100 ℃, the reaction pH = 7-10, and the reaction time is 2-10 h;
after the reaction is finished, carrying out reduced pressure concentration to obtain a tobacco leaf extract Maillard reaction product;
(3) microwave pyrolysis and extraction
And (3) cracking the Maillard reaction product of the tobacco leaf extract obtained in the step (2), and extracting the cracked product by using an organic solvent.
7. The electronic cigarette liquid prepared by using the electronic cigarette oil of the tobacco leaf extract Maillard reaction product of claim 1, is characterized by comprising the electronic cigarette oil prepared by the tobacco leaf extract Maillard reaction product and an atomizing agent; the electronic tobacco tar is the product of the maillard reaction of the tobacco extract in terms of volume ratio: the atomizing agent is =1: 10-20.
8. The electronic cigarette liquid of claim 7, wherein the atomizing agent comprises propylene glycol, glycerol and distilled water in a volume ratio of 3-8: 1: 1.
9. The application of the electronic cigarette liquid of claim 7 in an electronic cigarette, wherein the usage amount of the electronic cigarette liquid is 0.3-0.6 g each time.
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| CN112322663A (en) * | 2020-11-19 | 2021-02-05 | 河南中烟工业有限责任公司 | Tobacco flavor prepared by fermenting glucose and phenylalanine and application thereof |
| CN112956732A (en) * | 2021-04-02 | 2021-06-15 | 河南中烟工业有限责任公司 | Tobacco lysate and preparation method thereof |
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| CN101204249A (en) * | 2007-12-11 | 2008-06-25 | 广东中烟工业公司 | Preparation method for tobacco extracting |
| CN104017646A (en) * | 2014-06-13 | 2014-09-03 | 广西中烟工业有限责任公司 | Preparation method and application of malliard reaction product of waste and inferior tobacco leaf concentrate |
| CN104522878A (en) * | 2014-12-26 | 2015-04-22 | 郑州轻工业学院 | Glucose microwave pyrolysis product and application of same in tobacco products as aromatizing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101204249A (en) * | 2007-12-11 | 2008-06-25 | 广东中烟工业公司 | Preparation method for tobacco extracting |
| CN104017646A (en) * | 2014-06-13 | 2014-09-03 | 广西中烟工业有限责任公司 | Preparation method and application of malliard reaction product of waste and inferior tobacco leaf concentrate |
| CN104522878A (en) * | 2014-12-26 | 2015-04-22 | 郑州轻工业学院 | Glucose microwave pyrolysis product and application of same in tobacco products as aromatizing agent |
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