6-methylnicotine glycolate, preparation method thereof, atomization matrix, buccal product and electronic atomization device

By reacting and physical adsorbing treatment under the action of metal catalysts and ethanol acid, 6-methyldidine ethanol acid salt is prepared to solve the problem of high toxicity and spicy sensitivity of nicotine derivatives. Nicotine products with safer and better taste.

CN119371406AActive Publication Date: 2025-01-28HG INNOVATION LTD

Patent Information

Application Number
CN202411305954.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-19
Publication Date
2025-01-28
Estimated Expiration
2044-09-19

AI Technical Summary

Technical Problem

Among the existing nicotine derivatives, nicotine benzoate salt is more toxic, while 6-methyl nicotine has a strong sense of spicyness, making it difficult to meet safety and taste requirements.

Method used

By reacting 6-methyldine and ethanol acid under the action of metal catalysts, and physical adsorption treatment, 6-methyldidine ethanol acid salts are prepared to prepare atomized matrix or oral products.

Benefits of technology

This method effectively reduces the residual and heavy metal residues of the reactive substrate, enhances the safety and taste of the product, and reduces the spicy feeling.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to 6-methyl nicotine glycollate and a preparation method thereof, an atomization matrix, a buccal product and an electronic atomization device. The preparation method of the 6-methylnicotine glycollate comprises the following steps: mixing 6-methylnicotine, glycollic acid and a metal catalyst for reaction to obtain a reaction solution containing the 6-methylnicotine glycollate; and carrying out physical adsorption treatment on the reaction liquid to prepare the 6-methyl nicotine glycolate. 6-methylnicotine and glycollic acid react under the action of a metal catalyst, so that the conversion rate of a reaction substrate can be effectively promoted, and residues of the reaction substrate are effectively reduced; the obtained reaction liquid is further subjected to physical adsorption treatment, so that the residual catalyst in the reaction liquid can be effectively removed, and the prepared 6-methyl nicotine glycolate has less heavy metal residue.
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Description

Technical Field

[0001] The present application relates to the field of synthesis, and in particular to a 6-methylnicotine glycolate and a preparation method thereof, an atomization matrix, an oral product and an electronic atomization device. Background Art

[0002] Long-term smoking and exposure to nicotine will increase heart rate, raise blood pressure and reduce appetite. Large doses of nicotine can cause adverse reactions such as headaches and nausea. Currently, a series of nicotine derivatives have been produced by modifying the structure of nicotine to increase the biological efficacy of nicotine or reduce its toxicity. Among them, nicotine benzoate salt is widely used in nicotine derivatives, but benzoic acid is highly toxic; 6-methyl nicotine is less toxic and more active, but has a strong pungent taste.

[0003] Therefore, it is necessary to improve the traditional technology. Summary of the invention

[0004] Based on this, the present application provides a 6-methylnicotine glycolate with less toxicity and less pungency, and a preparation method thereof, an atomization matrix, an oral product and an electronic atomization device.

[0005] The technical solution of this application to solve the above technical problems is as follows.

[0006] In a first aspect, the present application provides a method for preparing 6-methylnicotine glycolate, comprising the following steps: mixing 6-methylnicotine, glycolic acid and a metal catalyst for reaction to obtain a reaction solution containing 6-methylnicotine glycolate; and subjecting the reaction solution to physical adsorption treatment to prepare 6-methylnicotine glycolate.

[0007] In some embodiments, in the method for preparing 6-methylnicotine glycolate, the metal catalyst includes nickel, and the physical adsorption treatment includes magnetic adsorption treatment.

[0008] In some embodiments, in the method for preparing 6-methylnicotine glycolate, the metal catalyst includes palladium, and the physical adsorption treatment includes activated carbon adsorption treatment.

[0009] In some embodiments, in the method for preparing 6-methylnicotine glycolate, the molar ratio of the glycolic acid to the 6-methylnicotine is 1-1.5:1.

[0010] In some embodiments, in the method for preparing 6-methylnicotine glycolate, the molar ratio of the metal catalyst to the 6-methylnicotine is 0.8-1.5:100.

[0011] In some of the embodiments, in the method for preparing 6-methylnicotine glycolate, the reaction temperature of the mixing reaction is 20° C. to 30° C., and the reaction time is 0.5 h to 2 h.

[0012] On the other hand, the present application provides 6-methyl nicotine glycolate, which is prepared by the above-mentioned preparation method of 6-methyl nicotine glycolate.

[0013] On the other hand, the present application provides a 6-methyl nicotine glycolate, the structural formula of the 6-methyl nicotine glycolate is shown in formula (I):

[0014] .

[0015] On the other hand, the present application provides an aerosolized matrix, comprising the above-mentioned methyl nicotine glycolate.

[0016] On the other hand, the present application provides an oral product comprising the above-mentioned methyl nicotine glycolate.

[0017] On the other hand, the present application provides an electronic atomization device, including the above-mentioned atomization matrix.

[0018] Compared with the prior art, the preparation method of 6-methylnicotine glycolate of the present application has the following beneficial effects:

[0019] The preparation method of 6-methylnicotine glycolate provided in the present application comprises reacting 6-methylnicotine and glycolic acid under the action of a metal catalyst, which can effectively promote the conversion rate of the reaction substrate, thereby effectively reducing the residue of the reaction substrate; further, the obtained reaction liquid is subjected to physical adsorption treatment, which can effectively remove the residual catalyst in the reaction liquid without affecting the reaction product, so that the heavy metal residue in the prepared 6-methylnicotine glycolate is less.

[0020] Using 6-methylnicotine glycolate to prepare an atomized base or an oral preparation can effectively improve the safety of the atomized base or the oral preparation, and effectively reduce the spiciness of the atomized base or the oral preparation. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the specific implementation methods of the present application or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0022] Figure 1 The IC50 curve of the aerosolized matrix prepared in Example 1;

[0023] Figure 2 This is the IC50 curve of the aerosolized matrix prepared in Comparative Example 4. DETAILED DESCRIPTION

[0024] References to embodiments of the present invention will now be provided in detail, one or more examples of which are described below. Each example is provided as an explanation rather than a limitation of the present invention. In fact, it will be apparent to those skilled in the art that various modifications and variations may be made to the present invention without departing from the scope or spirit of the present invention. For example, a feature illustrated or described as part of one embodiment may be used in another embodiment to produce a further embodiment.

[0025] Therefore, it is intended that the present invention covers such modifications and variations that fall within the scope of the appended claims and their equivalents. Other objects, features and aspects of the present invention are disclosed in or are obvious from the following detailed description. Those of ordinary skill in the art will appreciate that this discussion is only a description of exemplary embodiments and is not intended to limit the broader aspects of the present invention.

[0026] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0027] The term "comprises", "comprising" or any other variant thereof is intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements includes not only those elements, but also includes other elements not explicitly listed, or also includes elements inherent to such process, method, article or equipment. In the absence of more restrictions, the elements defined by the sentence "comprising one..." do not exclude the presence of other identical elements in the process, method, article or equipment including the elements. The indefinite articles "a kind of" and "an" before the elements or components of the present invention are not restrictive to the quantity requirements (i.e., the number of occurrences) of the elements or components. Therefore, "a" or "a kind of" should be interpreted as including one or at least one, and the elements or components in the singular form also include the plural form, unless the number clearly refers only to the singular form. The meaning of "multiple" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0028] The weight of the relevant components mentioned in the description of the embodiments of the present invention may not only refer to the specific content of each component, but also indicate the weight ratio between the components. Therefore, as long as the content of the relevant components is proportionally enlarged or reduced according to the description of the embodiments of the present invention, it is within the scope disclosed in the description of the embodiments of the present invention. Specifically, the weight described in the description of the embodiments of the present invention may be a mass unit known in the chemical industry such as μg, mg, g, kg, etc.

[0029] Except as shown in the operating examples or otherwise indicated, all numbers used in the specification and claims to indicate the amount of ingredients, physicochemical properties, etc. are understood to be adjusted by the term "about" in all cases. For example, therefore, unless otherwise indicated, the numerical parameters listed in the above specification and the attached claims are approximate values, and those skilled in the art can use the teachings disclosed herein to seek to obtain the desired properties and appropriately change these approximate values. The use of numerical ranges expressed as endpoints includes all numbers within the range and any range within the range, for example, 1 to 5 includes 1, 1.1, 1.3, 1.5, 2, 2.75, 3, 3.80, 4 and 5, etc.

[0030] An embodiment of the present application provides a method for preparing 6-methylnicotine glycolate, comprising the following steps:

[0031] Mixing 6-methylnicotine, glycolic acid and a metal catalyst to react to obtain a reaction solution containing 6-methylnicotine glycolate;

[0032] The reaction solution is subjected to physical adsorption treatment to prepare 6-methylnicotine glycolate.

[0033] The preparation method of 6-methylnicotine glycolate provided in the present application comprises reacting 6-methylnicotine and glycolic acid under the action of a metal catalyst, which can effectively promote the conversion rate of the reaction substrate, thereby effectively reducing the residue of the reaction substrate; further, the obtained reaction liquid is subjected to physical adsorption treatment, which can effectively remove the residual catalyst in the reaction liquid without affecting the reaction product, so that the heavy metal residue in the prepared 6-methylnicotine glycolate is less.

[0034] The preparation method of 6-methylnicotine glycolate provided in the present application does not require the use of solvents, can effectively save the use of reagents, and has simple post-processing.

[0035] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the metal catalyst includes at least one of nickel and palladium.

[0036] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the metal catalyst includes nickel, and the physical adsorption treatment includes magnetic adsorption treatment.

[0037] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the metal catalyst includes palladium, and the physical adsorption treatment includes activated carbon adsorption treatment.

[0038] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the molar ratio of glycolic acid to 6-methylnicotine is 1~1.5:1.

[0039] It can be understood that the molar ratio of glycolic acid to 6-methylnicotine includes but is not limited to 1:1, 1.1:1, 1.2:1, 1.3:1, and 1.4:1; in some examples, it can be within a range consisting of any two of these point values ​​as end values, the same below.

[0040] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the molar ratio of glycolic acid to 6-methylnicotine is 1~1.2:1.

[0041] In some of these examples, in the method for preparing 6-methylnicotine glycolate, the molar ratio of glycolic acid to 6-methylnicotine is 1:1.

[0042] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the molar ratio of the metal catalyst to 6-methylnicotine is 0.8~1.5:100.

[0043] It is understood that the molar ratio of the metal catalyst to 6-methylnicotine includes but is not limited to 0.8:100, 1:100, 1.2:100, and 1.5:100.

[0044] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the temperature of the mixing reaction is 20°C~30°C, and the time is 0.5 h~2 h.

[0045] It will be appreciated that the reaction temperature of the mixed reaction includes but is not limited to 20°C, 21°C, 22°C, 23°C, 24°C, 25°C, 26°C, 27°C, 28°C, 29°C, and 30°C, and the reaction time includes but is not limited to 0.5 h, 0.6 h, 0.7 h, 0.8 h, 0.9 h, 1 h, 1.1 h, 1.2 h, 1.3 h, 1.4 h, 1.5 h, 1.6 h, 1.7 h, 1.8 h, 1.9 h, and 2 h.

[0046] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the reaction temperature of the mixing reaction is 22°C~28°C, and the reaction time is 0.8 h~1.5 h.

[0047] In some of the examples, in the method for preparing 6-methylnicotine glycolate, the reaction temperature of the mixing reaction is 25° C. and the reaction time is 1 h.

[0048] One embodiment of the present application provides a 6-methyl nicotine glycolate, which is prepared by the above-mentioned preparation method of 6-methyl nicotine glycolate.

[0049] The 6-methylnicotine glycolate provided by the present application has less heavy metal residues.

[0050] Another embodiment of the present application provides a 6-methyl nicotine glycolate, and the structural formula of 6-methyl nicotine glycolate is shown in formula (I):

[0051] .

[0052] 6-Methylnicotine glycolate is used to prepare nicotine products, which has low toxicity and can effectively improve the safety of nicotine products.

[0053] One embodiment of the present application provides a nicotine product, comprising the above-mentioned 6-methylnicotine glycolic acid.

[0054] The nicotine product includes 6-methyl nicotine glycolate prepared by the preparation method of 6-methyl nicotine glycolate, which can effectively improve the safety of the nicotine product and effectively reduce the spiciness of the nicotine product; and has a better aroma performance, less odor, and a stronger sense of satisfaction.

[0055] Compared with traditional nicotine benzoate salt, the 6-methylnicotine glycolate prepared by the above-mentioned preparation method of 6-methylnicotine glycolate in nicotine products has less toxicity and can effectively improve the safety of nicotine products; compared with traditional 6-methylnicotine or other types of 6-methylnicotine salts, the spiciness is weaker.

[0056] The study found that the 6-methylnicotine salt prepared by reacting 6-methylnicotine with citric acid, tartaric acid or malic acid has a strong off-flavor and severe suppressed aroma; the 6-methylnicotine salt prepared by reacting 6-methylnicotine with levulinic acid has poor stability; the 6-methylnicotine salt prepared by reacting 6-methylnicotine with lactic acid is highly corrosive and not friendly to the heating wire.

[0057] In some examples, nicotine products include but are not limited to at least one of an atomized substrate and an oral product. The atomized substrate is atomized into an aerosol by heating or high-pressure air jet spraying for inhalation by the user. The oral product is placed in the user's mouth and consumed by the user by dissolving or melting.

[0058] One embodiment of the present application provides an oral product, comprising the above-mentioned 6-methylnicotine glycolate.

[0059] It can be understood that oral products include but are not limited to oral cigarettes; further, the specific forms of oral cigarettes include but are not limited to: at least one of nicotine bags, orodispersible films, oral tablets and chewing gum.

[0060] Another embodiment of the present application provides an aerosolized matrix, comprising the above-mentioned 6-methylnicotine glycolic acid.

[0061] In some of these examples, the aerosolized matrix includes the following components by weight:

[0062] 3-10 parts of 6-methylnicotine glycolic acid, 30-50 parts of additives and 40-60 parts of organic solvents.

[0063] It can be understood that in the atomized matrix, by mass, 6-methylnicotine glycolic acid includes but is not limited to 3, 4, 5, 6, 7, 8, 9, and 10 parts; additives include but are not limited to 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, and 50 parts; organic solvents include but are not limited to 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, and 60 parts.

[0064] In some of these examples, the aerosolized matrix includes the following components by weight:

[0065] 3-8 parts of 6-methylnicotine glycolic acid, 35-45 parts of additives and 50-60 parts of organic solvents.

[0066] In some of these examples, the aerosolized matrix includes the following components by weight:

[0067] 4-6 parts of 6-methylnicotine glycolic acid, 36-42 parts of additives and 52-58 parts of organic solvents.

[0068] In some of the examples, in the aerosol base, the organic solvent is selected from at least one of propylene glycol and glycerol (glycerin).

[0069] In some of these examples, the organic solvents in the aerosol base include propylene glycol and glycerol.

[0070] In some of the examples, the mass ratio of propylene glycol to glycerol in the aerosol matrix is ​​0.3~0.8:1.

[0071] It will be appreciated that the mass ratio of propylene glycol to glycerol includes, but is not limited to, 0.3:1, 0.4:1, 0.5:1, 0.6:1, 0.7:1, and 0.8:1.

[0072] In some of the examples, the mass ratio of propylene glycol to glycerol in the aerosol matrix is ​​0.3~0.5:1.

[0073] In some of these examples, the additive in the atomized base includes at least one of a flavor, a sweetener, and a cooling agent.

[0074] It can be understood that the present application does not limit the types of flavors, sweeteners and cooling agents; further, the atomized matrix of the present application may also include other commonly used additives.

[0075] In some of the examples, the flavor in the atomized matrix includes at least one of various edible flavors including but not limited to fruit flavor, tobacco flavor, cooking flavor, etc.

[0076] In some of these examples, the aerosolized matrix includes the following components by weight:

[0077] 3-10 parts of 6-methylnicotine glycolic acid, 15-25 parts of strawberry flavor, 5-15 parts of green strawberry flavor, 2-5 parts of sweetener, 4-8 parts of cooling agent, 30-50 parts of glycerol and 10-20 parts of propylene glycol.

[0078] In some of these examples, the e-liquid in the atomized matrix includes the following components by weight:

[0079] 3-8 parts of 6-methylnicotine glycolic acid, 18-22 parts of strawberry flavor, 8-12 parts of green strawberry flavor, 2-4 parts of sweetener, 5-7 parts of cooling agent, 35-45 parts of glycerol and 12-18 parts of propylene glycol.

[0080] In some of the examples, the aerosolized matrix includes the following components by weight:

[0081] 5 parts of 6-methylnicotine glycolic acid, 20 parts of strawberry flavor, 10 parts of green strawberry flavor, 3 parts of sweetener, 6 parts of cooling agent, 40 parts of glycerol and 16 parts of propylene glycol.

[0082] One embodiment of the present application provides the use of the above-mentioned atomizing matrix in preparing an electronic atomizing device. Another embodiment of the present application provides an electronic atomizing device, comprising the above-mentioned atomizing matrix.

[0083] It is understood that the electronic atomization device includes but is not limited to an electronic cigarette. It is further understood that the atomization matrix serves as the e-liquid in the electronic cigarette.

[0084] The present application is further described in detail below in conjunction with specific implementation methods, but the implementation methods of the present application are not limited thereto.

[0085] Preparation of 6-methylnicotine salt:

[0086] 6-Methylnicotine azelaic acid: Wash a 500 mL three-necked flask, add 176 g (1 mol) of 6-methylnicotine, add 188.22 g (1 mol) of azelaic acid while stirring, and stir at 25°C for 1 h to prepare 6-methylnicotine azelaic acid.

[0087] No. 1 6-methylnicotine glycolate: Wash a 500 mL three-necked flask, add 176 g (1 mol) of 6-methylnicotine, add 75.05 g (1 mol) of glycolic acid while stirring, stir at 25°C for 1 h, and prepare No. 1 6-methylnicotine glycolate.

[0088] No. 2 6-methylnicotine glycolate: Wash a 500 mL three-necked flask, add 176 g (1 mol) of 6-methylnicotine, add 112.58 g (1.5 mol) of glycolic acid while stirring, stir at 25°C for 1 h to prepare No. 2 6-methylnicotine glycolate.

[0089] No. 3 6-methylnicotine glycolate: Wash a 500 mL three-necked flask, add 176 g (1 mol) of 6-methylnicotine, add 75.05 g (1 mol) of glycolic acid while stirring, add 1.06 g (0.01 mol) of palladium catalyst, and stir at 25°C for 1 h; remove palladium from the reaction solution by activated carbon adsorption to prepare No. 3 6-methylnicotine glycolate.

[0090] No. 4 6-methylnicotine glycolate: Wash a 500 mL three-necked flask, add 176 g (1 mol) of 6-methylnicotine, add 75.05 g (1 mol) of glycolic acid while stirring, add 0.58 g (0.01 mol) of nickel catalyst, and stir at 25°C for 1 h; use a magnet to remove nickel from the reaction solution to prepare No. 4 6-methylnicotine glycolate.

[0091] Example 1

[0092] Calculated by mass, 5 parts of No. 4 6-methylnicotine glycolic acid, 20 parts of strawberry flavor, 10 parts of green strawberry flavor, 3 parts of sweetener, 6 parts of cooling agent, 40 parts of glycerol and 16 parts of propylene glycol are mixed to prepare the atomization matrix - smoke oil.

[0093] In the e-liquid prepared in Example 1, the 6-methyl nicotine content is 20 mg / g, the density is 1.2 g / cm³, and the pH value is 7.4.

[0094] Example 2

[0095] The method is basically the same as Example 1, except that the No. 4 6-methyl nicotine glycolate in Example 1 is replaced with an equal mass of No. 3 6-methyl nicotine glycolate, as follows:

[0096] Calculated by weight, No. 3 6-methylnicotine glycolate, 20 parts of strawberry flavor, 10 parts of green strawberry flavor, 3 parts of sweetener, 6 parts of cooling agent, 40 parts of glycerol and 16 parts of propylene glycol are mixed to prepare an atomization matrix - e-liquid.

[0097] Comparative Example 1

[0098] The method is basically the same as Example 1, except that the 6-methylnicotine glycolate No. 4 in Example 1 is replaced with 6-methylnicotine azelaic acid salt of equal mass, as follows:

[0099] Calculated by mass, 5 parts of nicotine azelaate, 20 parts of strawberry flavor, 10 parts of green strawberry flavor, 3 parts of sweetener, 6 parts of cooling agent, 40 parts of glycerol and 16 parts of propylene glycol are mixed to prepare an atomization matrix - smoke oil.

[0100] After tasting, 6-methylnicotine azelaic acid salt has a distinct odor.

[0101] Comparative Example 2

[0102] The method is basically the same as Example 1, except that the No. 4 6-methyl nicotine glycolate in Example 1 is replaced with an equal mass of No. 1 6-methyl nicotine glycolate, as follows:

[0103] By mass, 5 parts of No. 1 6-methylnicotine glycolate, 20 parts of strawberry flavor, 10 parts of green strawberry flavor, 3 parts of sweetener, 6 parts of cooling agent, 40 parts of glycerol and 16 parts of propylene glycol are mixed to prepare an atomization matrix - e-liquid.

[0104] Comparative Example 3

[0105] The method is basically the same as Example 1, except that the No. 4 6-methyl nicotine glycolate in Example 1 is replaced with an equal mass of No. 2 6-methyl nicotine glycolate, as follows:

[0106] Calculated by mass, 5 parts of No. 2 6-methylnicotine glycolate, 20 parts of strawberry flavor, 10 parts of green strawberry flavor, 3 parts of sweetener, 6 parts of cooling agent, 40 parts of glycerol and 16 parts of propylene glycol are mixed to prepare an atomization matrix - e-liquid.

[0107] Comparative Example 4

[0108] The method is basically the same as Example 1, except that the 6-methylnicotine glycolic acid No. 4 in Example 1 is replaced with 6-methylnicotine benzoate of equal mass, as follows:

[0109] Calculated by weight, 6-methylnicotine benzoate, 20 parts of strawberry flavor, 10 parts of green strawberry flavor, 3 parts of sweetener, 6 parts of cooling agent, 40 parts of glycerol and 16 parts of propylene glycol are mixed to prepare an atomization matrix - e-liquid.

[0110] Taste test:

[0111] The taste was evaluated by 6 people, and the average score of the 6 people was taken. The evaluation dimensions include: throat hit (1~10 points, the higher the score, the stronger the impact on the throat); satisfaction (1~10 points, the higher the score, the better the satisfaction); odor (1~10 points, the lower the score, the less odor); spiciness (1~10 points, the higher the score, the lower the spiciness); overall aroma performance (1~10 points, the higher the score, the better the aroma performance). The evaluation results are shown in Table 1:

[0112] Table 1

[0113]

[0114] By comparing the evaluation results in Table 1, it can be seen that: from the comparison of the three dimensions of throat hit, reduction of spiciness, and satisfaction, the e-liquids prepared in Examples 1 and 2 are better than the e-liquids prepared in Comparative Examples 2 and 3; among them, the spiciness of Comparative Example 2 is stronger, and Comparative Example 3 has an overall sour taste, which is not conducive to commercial sale; from the overall aroma performance, the e-liquid prepared in Example 1 is better than the e-liquid prepared in Example 2; the possible reason is that the activated carbon adsorbs more small molecular ester substances, resulting in a weaker aroma of the e-liquid prepared in Example 2.

[0115] Stability test:

[0116] According to the results of the oral evaluation, the e-liquid prepared in Example 1 and the e-liquid prepared in Comparative Example 4 were selected for stability comparison:

[0117] After 6 months of room temperature comparison, the content of 6-methyl nicotine salt (mg / g) in the e-liquid was tested by gas phase mass spectrometry every 2 weeks. The results are shown in Table 2:

[0118] Table 2

[0119]

[0120] It can be seen from Table 2 that the degradation rate of No. 4 6-methyl nicotine salt is slower than that of 6-methyl nicotine benzoate and has better stability.

[0121] Toxicity test:

[0122] Beas-2B cells were selected for in vitro cytotoxicity testing. Beas-2B cells are a normal human lung epithelial cell line, whose survival rate directly affects the physiological function of the lungs and are commonly used for toxicity detection and analysis of electronic cigarette components. The IC50 curves of the atomized matrix-cigarette oil prepared in Example 1 and Comparative Example 4 are shown in Figure 2. Figure 1 and Figure 2 shown.

[0123] IC50 (half maximal inhibitory concentration) refers to the concentration at which a substance can reduce the activity of a biological process by 50% under experimental conditions. IC50 is a unit of measurement used to measure the effectiveness of a drug, compound or other biologically active molecule in inhibiting a specific biological process. The smaller the IC50 value, the greater the effectiveness of the substance in inhibiting a biological process.

[0124] according to Figure 1 and Figure 2 It can be seen that the IC50 of Example 1 is 1.128 mg / mL, and the IC50 of Comparative Example 4 is 0.8219 mg / mL. This indicates that the toxicity of No. 4 6-methylnicotine glycolate used in Example 1 is less than that of 6-methylnicotine benzoate in Comparative Example 4; using No. 4 6-methylnicotine glycolate instead of 6-methylnicotine benzoate can achieve the purpose of reducing toxicity and harm.

[0125] Flue gas heavy metal test:

[0126] ICP-MS was used to test the heavy metal content of the e-liquids prepared in Example 1 and Comparative Example 4. The test results are shown in Table 3:

[0127] Table 3

[0128]

[0129] It can be seen from Table 3 that the heavy metal contents in the flue gas of Example 1 and Comparative Example 4 are both within the TPD reference limit. Among them, the contents of chromium, iron, nickel and antimony in the flue gas of Example 1 are less than those of Comparative Example 4.

[0130] Smoke aldehyde and ketone test:

[0131] The aldehyde and ketone tests were performed on the e-liquids prepared in Example 1 and Comparative Example 4 using HPLC. The test results are shown in Table 4:

[0132] Table 4

[0133]

[0134] It can be seen from Table 4 that the content of formaldehyde, acetaldehyde, acrolein and crotonaldehyde in the flue gas of Example 1 and Comparative Example 4 is not much different, and both are within the TPD reference limit.

[0135] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0136] The above-described embodiments only express several implementation methods of the present application, which is convenient for understanding the technical solution of the present application in detail, but it cannot be understood as limiting the scope of protection of the invention patent. It should be pointed out that for ordinary technicians in this field, without departing from the concept of the present application, several modifications and improvements can be made, which all belong to the scope of protection of the present application. It should be understood that the technical solutions obtained by those skilled in the art through logical analysis, reasoning or limited experiments on the basis of the technical solutions provided in the present application are all within the scope of protection of the claims attached to the present application. Therefore, the scope of protection of the patent of this application shall be based on the contents of the attached claims, and the description and drawings can be used to explain the contents of the claims.

Claims

1. A method for preparing 6-methylnicotine glycolate, characterized in that: The following steps are involved: Mixing 6-methylnicotine, glycolic acid and a metal catalyst to react to obtain a reaction solution containing 6-methylnicotine glycolate; The reaction solution is subjected to physical adsorption treatment to prepare 6-methylnicotine glycolate.

2. The method for preparing 6-methylnicotine glycolate according to claim 1, characterized in that: The metal catalyst includes nickel, and the physical adsorption treatment includes magnetic adsorption treatment.

3. The method for preparing 6-methylnicotine glycolate according to claim 1, characterized in that: The metal catalyst includes palladium, and the physical adsorption treatment includes activated carbon adsorption treatment.

4. The method for preparing 6-methylnicotine glycolate according to claim 1, characterized in that: The preparation method includes at least one of the following features: (1) The molar ratio of the glycolic acid to the 6-methylnicotine is 1 to 1.5:1; (2) The molar ratio of the metal catalyst to the 6-methylnicotine is 0.8-1.5:

100.

5. The method for preparing 6-methylnicotine glycolate according to any one of claims 1 to 4, characterized in that: The reaction temperature of the mixed reaction is 20°C to 30°C, and the reaction time is 0.5 h to 2 h.

6. A 6-methylnicotine glycolate, characterized in that The 6-methylnicotine glycolate is prepared by the preparation method of any one of claims 1 to 5.

7. A 6-methylnicotine glycolate, characterized in that The structural formula of the 6-methylnicotine glycolate is shown in formula (I): 。 8. An atomized substrate, characterized in that Comprising 6-methylnicotine glycolate as described in claim 6 or 7.

9. An oral product, characterized in that: Comprising 6-methylnicotine glycolate as described in claim 6 or 7.

10. An electronic atomization device, characterized in that: Comprising the atomized substrate as described in claim 8.

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