CN114601193A - Preparation method and application of antioxidant nicotine salt - Google Patents

Preparation method and application of antioxidant nicotine salt Download PDF

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Publication number
CN114601193A
CN114601193A CN202210452249.0A CN202210452249A CN114601193A CN 114601193 A CN114601193 A CN 114601193A CN 202210452249 A CN202210452249 A CN 202210452249A CN 114601193 A CN114601193 A CN 114601193A
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antioxidant
nicotine salt
nicotine
parts
mixture
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CN202210452249.0A
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Inventor
杨鹏
苏磊
王一骑
邓益川
胡旺顺
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Shenzhen Aipu Biotechnology Co ltd
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Shenzhen Aipu Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/16Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A24B15/167Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The application provides a preparation method and application of an antioxidant nicotine salt, which comprises the following steps: adding nicotine, an antioxidant and an organic solvent into a reaction container according to a certain weight ratio, fully stirring under a first preset condition, and uniformly mixing to obtain a first mixed solution; and adding organic acid into the first mixed solution, placing the mixture under a second preset condition, fully stirring the mixture, and cooling the mixture to room temperature to obtain the nicotine salt. The nicotine salt with the oxidation resistance is prepared by mixing nicotine, an antioxidant, an organic solvent and an organic acid together under certain conditions, wherein the antioxidant adopts a tea seed green tangerine orange peel extract, and an oil-soluble antioxidant is extracted from the tea seed green tangerine orange peel, so that the oxidation stability of the nicotine salt can be obviously improved, and meanwhile, when the nicotine salt is applied to electronic tobacco tar, the oil-soluble antioxidant can also obviously improve the oxidation resistance of the tobacco tar, enhance the stability of the electronic tobacco tar and reduce the harm of the tobacco tar to human bodies.

Description

Preparation method and application of antioxidant nicotine salt
Technical Field
The application relates to the technical field of nicotine salt, in particular to a preparation method and application of antioxidant nicotine salt.
Background
Nicotine, 3- [ 1-methylpyrrolidin-2-yl ] pyridine, is a molecular alkaloid naturally produced by some solanaceous plants, commonly known as nicotine, which includes not only tobacco but also capsicum, tomato, potato, eggplant or petunia. Among these plants, tobacco is one of the most abundant plants with nicotine content, accounting for 8% -14%, which is also responsible for its use in cigarettes.
The emergence of electronic cigarettes has changed the fate of millions of smokers, and the emergence of nicotine salt tobacco tar has further promoted the healthy development of small smoke tides. Compared with the traditional nicotine tobacco tar extracted from tobacco, the nicotine salt tobacco tar has higher content of used nicotine salt, can be easily absorbed by human blood, can relieve the nicotine requirement of nicotine addicts, has more comfortable inhalation feeling and addiction relieving capability, can achieve the advantages of quick addiction relieving and no interference of small smoke to other people when being properly applied to low-power equipment, does not resemble the traditional tobacco tar, and can bring unacceptable throat hitting experience when pursuing high nicotine.
However, when the nicotine salt is applied to the electronic cigarette tobacco tar, the defect of low oxidation resistance exists as the nicotine tobacco tar, so that the electronic cigarette tobacco tar is poor in stability and extremely easy to oxidize, the taste of the electronic cigarette tobacco tar is affected, and meanwhile, oxidative decomposition substances generated after the electronic cigarette tobacco tar is inhaled into a human body have certain damage to human organs. Therefore, there is a need to develop a nicotine salt with improved antioxidant properties.
Disclosure of Invention
In view of the above, the present application is proposed to provide a method for preparing and use of an antioxidant nicotine salt that overcomes or at least partially solves the above mentioned problems, comprising:
a preparation method of an antioxidant nicotine salt comprises the following steps:
adding nicotine, an antioxidant and an organic solvent into a reaction container according to a certain weight ratio, fully stirring under a first preset condition, and uniformly mixing to obtain a first mixed solution;
and adding organic acid into the first mixed solution, placing the mixture under a second preset condition, fully stirring the mixture, and cooling the mixture to room temperature to obtain the antioxidant nicotine salt.
Preferably, before the step of adding nicotine, an antioxidant and an organic solvent into a reaction vessel according to a certain weight ratio, fully stirring and uniformly mixing under a first preset condition to obtain a first mixed solution, the method further comprises:
preparing an antioxidant, wherein the antioxidant is an extract of green tangerine orange peel of tea seeds.
Preferably, the step of preparing the antioxidant comprises:
mixing the tea seed green tangerine peel particles and n-hexane according to a material-liquid ratio of 1: 1.2-1.4, soaking for 3 times at 50 ℃ for 2 hours each time, filtering and combining to obtain a leaching solution;
heating the combined leaching liquor to 60 ℃ to obtain a concentrated solution;
slowly cooling the concentrated solution to-5 to-7 ℃, controlling the cooling time to be 6 hours, and filtering and removing the wax in the oil after the wax in the concentrated solution is separated out to obtain a purified solution;
and (3) removing the residual solvent from the purified liquid by a molecular distillation method to obtain the antioxidant.
Preferably, the first preset condition is normal temperature, and the second preset condition is: the temperature is 60-150 ℃, the stirring speed is 200-.
Preferably, the organic acid is one or a combination of more of benzoic acid, glutamic acid, malic acid and citric acid.
Preferably, the organic solvent is one or both of propylene glycol and glycerol.
Preferably, the weight ratio of the nicotine, the antioxidant and the organic solvent is 1: 0.1-1: 0.1-1.
Preferably, the weight ratio of the first mixed solution to the organic acid is 1: 0.1-1.
Preferably, the weight ratio of the first mixed solution to the organic acid is 1: 0.3-1.
The application also provides an application of the antioxidant nicotine salt, wherein the antioxidant nicotine salt is used for the electronic cigarette oil, and the electronic cigarette oil comprises the following raw materials in parts by weight: 2-5 parts of antioxidant nicotine salt, 30-50 parts of glycerol, 3-6 parts of cooling agent and 40-60 parts of solvent.
The application has the following advantages:
in the embodiment of the application, nicotine, an antioxidant and an organic solvent are added into a reaction container according to a certain weight ratio, fully stirred under a first preset condition, and uniformly mixed to obtain a first mixed solution; and adding organic acid into the first mixed solution, placing the mixture under a second preset condition, fully stirring the mixture, and cooling the mixture to room temperature to obtain the antioxidant nicotine salt. The nicotine salt with the oxidation resistance is prepared by mixing nicotine, an antioxidant, an organic solvent and an organic acid together under certain conditions, wherein the antioxidant adopts a tea seed green tangerine orange peel extract, and an oil-soluble antioxidant is extracted from the tea seed green tangerine orange peel, so that the oxidation stability of the nicotine salt can be obviously improved, and meanwhile, when the nicotine salt is applied to electronic tobacco tar, the oil-soluble antioxidant can also obviously improve the oxidation resistance of the tobacco tar, enhance the stability of the electronic tobacco tar and reduce the harm of the tobacco tar to human bodies; meanwhile, the antioxidant is extracted from the tea seed green husks, so that the tea seed green husks are changed into valuable, and the production cost can be effectively reduced.
Detailed Description
In order to make the objects, features and advantages of the present application more comprehensible, the present application will be described in further detail with reference to the following embodiments. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
An embodiment of the application provides a preparation method of an antioxidant nicotine salt, which comprises the following steps:
adding nicotine, an antioxidant and an organic solvent into a reaction container according to a certain weight ratio, fully stirring under a first preset condition, and uniformly mixing to obtain a first mixed solution;
and adding organic acid into the first mixed solution, placing the mixture under a second preset condition, fully stirring the mixture, and cooling the mixture to room temperature to obtain the nicotine salt.
In the embodiment of the application, nicotine, an antioxidant and an organic solvent are added into a reaction container according to a certain weight ratio, fully stirred under a first preset condition, and uniformly mixed to obtain a first mixed solution; and adding organic acid into the first mixed solution, placing the mixture under a second preset condition, fully stirring the mixture, and cooling the mixture to room temperature to obtain the antioxidant nicotine salt. The nicotine salt with the oxidation resistance is prepared by mixing nicotine, an antioxidant, an organic solvent and an organic acid together under certain conditions, wherein the antioxidant adopts a tea seed green tangerine orange peel extract, and an oil-soluble antioxidant is extracted from the tea seed green tangerine orange peel, so that the oxidation stability of the nicotine salt can be obviously improved, and meanwhile, when the nicotine salt is applied to electronic tobacco tar, the oil-soluble antioxidant can also obviously improve the oxidation resistance of the tobacco tar, enhance the stability of the electronic tobacco tar and reduce the harm of the tobacco tar to human bodies; meanwhile, the antioxidant is extracted from the tea seed green husks, so that the tea seed green husks are changed into valuable, and the production cost can be effectively reduced.
Hereinafter, a method for preparing an antioxidant nicotine salt and its use in the present exemplary embodiment will be further described.
In an embodiment of the application, the antioxidant is an extract of tea seed green tangerine peels, the used raw material is the waste tea seed green tangerine peels, the raw material source is wide, the antioxidant is prepared from the waste extract of the tea seed green tangerine peels, waste materials are changed into things of value, and the cost can be effectively reduced.
Specifically, the preparation process of the antioxidant comprises the following steps:
collecting ripe tea fruits, drying in the sun to crack the peel, and separating green husks and seeds of tea seeds; taking green tea seed husks, and continuing airing until the water content is reduced to below 15%; crushing the dried green tea seed peel by using a crusher, sieving by using a sieve of 10 meshes to obtain green tea seed peel granules, sealing, bagging and storing; weighing 20kg of the tea seed green tangerine peel particles, adding 24L of n-hexane, soaking at 50 ℃ for 3 times, each time for 2 hours, filtering and combining the leaching liquor; heating the leaching liquor to 60 ℃ to evaporate 80% of the solvent in the leaching liquor to obtain a concentrated solution, and cooling and recycling the evaporated solvent through a condenser; slowly cooling the concentrated solution to-5 to-7 ℃, controlling the cooling time to be 6 hours, and filtering and removing wax in the oil after the wax in the concentrated solution is separated out to obtain a purified solution; the purified solution was subjected to molecular distillation to remove the remaining solvent, and 50g of an oil-soluble antioxidant was obtained.
In one embodiment of the present application, a method for preparing an antioxidant nicotine salt comprises the following steps:
adding nicotine, tea seed green tangerine peel extract and organic solvent into a reaction container according to a certain weight ratio, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution;
adding organic acid into the transparent solution, stirring at 60-150 ℃ at a stirring speed of 200-.
In one embodiment of the present application, the organic acid is one or a combination of several of benzoic acid, glutamic acid, malic acid, and citric acid, preferably benzoic acid; the organic solvent is one or two of propylene glycol or glycerol, and is preferably propylene glycol.
Example 1
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.7:0.5, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: benzoic acid is 1: adding benzoic acid at a ratio of 0.4, heating and stirring at 130 deg.C with stirring speed of 400r/min and reflux ratio of 2:1, refluxing for 2h, and cooling to room temperature to obtain nicotine salt.
Example 2
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.3:0.35, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: benzoic acid is 1: adding benzoic acid at a ratio of 0.7, heating and stirring at 110 deg.C with stirring speed of 400r/min and reflux ratio of 2:1, refluxing for 1h, and cooling to room temperature to obtain nicotine salt.
Example 3
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.6:0.9, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: benzoic acid is 1: adding benzoic acid at a ratio of 0.4, heating and stirring at 90 deg.C with stirring speed of 300r/min and reflux ratio of 2:1, refluxing for 5h, and cooling to room temperature to obtain nicotine salt.
Example 4
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.9:0.2, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: benzoic acid is 1: adding benzoic acid at a ratio of 0.3, heating at 60 deg.C under stirring at a speed of 200r/min and reflux ratio of 2:1, refluxing for 3.6h, and cooling to room temperature to obtain nicotine salt.
Example 5
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.5:0.5, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: benzoic acid is 1: adding benzoic acid at a ratio of 0.7, heating at 70 deg.C under stirring at a speed of 500r/min and reflux ratio of 2:1, refluxing for 1.5h, and cooling to room temperature to obtain nicotine salt.
Example 6
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.8:0.9, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: citric acid is 1: adding citric acid at a ratio of 0.2, heating at 105 deg.C under stirring at 400r/min under reflux ratio of 2:1 for 1 hr, and cooling to room temperature to obtain nicotine salt.
Example 7
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.9:0.1, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: malic acid is 1: adding malic acid at a ratio of 0.2, heating and stirring at 100 deg.C with stirring speed of 300r/min and reflux ratio of 2:1, refluxing for 2.8h, and cooling to room temperature to obtain nicotine salt.
Example 8
Weighing nicotine, a tea seed green tangerine peel extract and propylene glycol according to a weight ratio of 1:0.8:0.8, respectively, fully stirring at normal temperature, and uniformly mixing to obtain a transparent solution; in the obtained transparent solution, the weight ratio of the transparent solution is as follows: malic acid is 1:0.1 of glutamic acid, and adding the transparent solution according to the weight ratio: distilled water is 1: adding water at a ratio of 0.01, heating and stirring at 112 deg.C with stirring speed of 200r/min and reflux ratio of 2:1, refluxing for 5 hr, and cooling to room temperature to obtain nicotine salt.
In the embodiment of the application, the antioxidant nicotine salt prepared by the preparation method is applied to electronic cigarette oil to obtain antioxidant electronic cigarette oil, and the antioxidant electronic cigarette oil comprises the following raw materials in parts by weight: 2-5 parts of antioxidant nicotine salt, 30-50 parts of glycerol, 3-6 parts of cooling agent and 40-60 parts of solvent; wherein the cooling agent is peppermint oil or N-ethyl-p-menthane-3-formamide, preferably peppermint oil, and the solvent is propylene glycol or glycerol, preferably glycerol.
Example 9
The antioxidant electronic cigarette oil comprises the following raw materials in parts by weight: 5 parts of antioxidant nicotine salt, 30 parts of glycerol, 3 parts of peppermint oil and 40 parts of glycerol.
Example 10
The antioxidant electronic cigarette oil comprises the following raw materials in parts by weight: 4 parts of antioxidant nicotine salt, 35 parts of glycerin, 4 parts of peppermint oil and 45 parts of glycerol.
Example 11
The antioxidant electronic cigarette oil comprises the following raw materials in parts by weight: 3 parts of antioxidant nicotine salt, 40 parts of glycerin, 5 parts of peppermint oil and 50 parts of glycerol.
Example 12
The antioxidant electronic cigarette oil comprises the following raw materials in parts by weight: 2 parts of antioxidant nicotine salt, 50 parts of glycerin, 6 parts of peppermint oil and 60 parts of glycerol.
Experiment on Oxidation resistance
The antioxidant electronic cigarette oil prepared by the invention is compared with common electronic cigarette oil without antioxidant, a grease oxidation stability tester is used for measurement, the experimental conditions are that the temperature is 110 ℃/120 ℃, the air flow rate is 20L/h, and the measurement result evaluates the antioxidant performance according to the induction time.
The experimental groups used were the groups of example 9 and example 12.
Comparative example 9
The electronic cigarette oil comprises the following raw materials in parts by weight: 5 parts of nicotine, 30 parts of glycerol, 3 parts of peppermint oil and 40 parts of glycerol.
Comparative example 12
The electronic cigarette oil comprises the following raw materials in parts by weight: 2 parts of nicotine, 50 parts of glycerol, 6 parts of peppermint oil and 60 parts of glycerol.
The experimental data are shown in table one.
Figure BDA0003619152090000071
Watch 1
Experimental results show that the antioxidant electronic tobacco tar prepared by the method can obviously improve the oxidation stability of the tobacco tar, so that the nicotine salt prepared by the method has higher antioxidant stability.
While preferred embodiments of the present application have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including the preferred embodiment and all such alterations and modifications as fall within the true scope of the embodiments of the application.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or article that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, or article. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, or article that comprises the element.
The preparation method and the application of the antioxidant nicotine salt provided by the application are described in detail above, and the principle and the implementation mode of the application are explained in the present application by using specific examples, and the description of the above examples is only used to help understand the method and the core idea of the application; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.

Claims (10)

1. The preparation method of the antioxidant nicotine salt is characterized by comprising the following steps:
adding nicotine, an antioxidant and an organic solvent into a reaction container according to a certain weight ratio, fully stirring under a first preset condition, and uniformly mixing to obtain a first mixed solution;
and adding organic acid into the first mixed solution, placing the mixture under a second preset condition, fully stirring the mixture, and cooling the mixture to room temperature to obtain the antioxidant nicotine salt.
2. The method for preparing an antioxidant nicotine salt as claimed in claim 1, wherein the step of adding nicotine, an antioxidant and an organic solvent into a reaction vessel according to a certain weight ratio, stirring the mixture fully under a first preset condition, and mixing the mixture uniformly to obtain a first mixed solution further comprises:
preparing an antioxidant, wherein the antioxidant is an extract of green tangerine orange peel of tea seeds.
3. The method of preparing an antioxidant nicotine salt of claim 2, wherein the step of preparing an antioxidant comprises:
mixing the tea seed green tangerine peel particles and n-hexane according to a material-liquid ratio of 1: 1.2-1.4, soaking for 3 times at 50 ℃ for 2 hours each time, filtering and combining to obtain a leaching solution;
heating the combined leaching liquor to 60 ℃ to obtain a concentrated solution;
slowly cooling the concentrated solution to-5 to-7 ℃, controlling the cooling time to be 6 hours, and filtering and removing the wax in the oil after the wax in the concentrated solution is separated out to obtain a purified solution;
and (3) removing the residual solvent from the purified liquid by a molecular distillation method to obtain the antioxidant.
4. The method for preparing an antioxidant nicotine salt as in claim 1, wherein the first predetermined condition is normal temperature, and the second predetermined condition is: the temperature is 60-150 ℃, the stirring speed is 200-500r/min, the reflux ratio is 2:1, and the reflux reaction is 0.5-2 h.
5. The method for preparing antioxidant nicotine salt of claim 1, wherein the organic acid is one or more of benzoic acid, glutamic acid, malic acid, and citric acid.
6. The method of claim 1, wherein the organic solvent is one or both of propylene glycol and glycerol.
7. The method of preparing an antioxidant nicotine salt of claim 1, wherein the weight ratio of nicotine, the antioxidant and the organic solvent is 1: 0.1-1: 0.1-1.
8. The method of claim 1, wherein the weight ratio of the first mixed solution to the organic acid is 1: 0.1-1.
9. The method of claim 1, wherein the weight ratio of the first mixed solution to the organic acid is 1: 0.3-1.
10. The use of the antioxidant nicotine salt of claim 1, wherein the antioxidant nicotine salt is used in electronic cigarette liquid, and the electronic cigarette liquid comprises the following raw materials in parts by weight: 2-5 parts of antioxidant nicotine salt, 30-50 parts of glycerol, 3-6 parts of cooling agent and 40-60 parts of solvent.
CN202210452249.0A 2022-04-27 2022-04-27 Preparation method and application of antioxidant nicotine salt Pending CN114601193A (en)

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Cited By (4)

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CN115119957A (en) * 2022-06-28 2022-09-30 深圳市艾普生物科技有限公司 Antioxidant electronic cigarette oil and preparation method thereof
CN115191635A (en) * 2022-08-24 2022-10-18 深圳市恒云生物科技有限公司 Nicotine salt and preparation method thereof
CN115281366A (en) * 2022-06-28 2022-11-04 深圳市艾普生物科技有限公司 Preparation method and application of antioxidant nicotine salt
CN116235982A (en) * 2023-02-28 2023-06-09 深圳正和生物科技有限公司 Electronic cigarette oil, preparation method thereof and electronic cigarette

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CN112841709A (en) * 2021-01-20 2021-05-28 深圳市艾普生物科技有限公司 Preparation method and application of nicotine salt
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Publication number Priority date Publication date Assignee Title
CN115119957A (en) * 2022-06-28 2022-09-30 深圳市艾普生物科技有限公司 Antioxidant electronic cigarette oil and preparation method thereof
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CN116235982A (en) * 2023-02-28 2023-06-09 深圳正和生物科技有限公司 Electronic cigarette oil, preparation method thereof and electronic cigarette

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