CN112956729A - Nicotine salt and preparation method thereof - Google Patents
Nicotine salt and preparation method thereof Download PDFInfo
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- CN112956729A CN112956729A CN202110262138.9A CN202110262138A CN112956729A CN 112956729 A CN112956729 A CN 112956729A CN 202110262138 A CN202110262138 A CN 202110262138A CN 112956729 A CN112956729 A CN 112956729A
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical 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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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/10—Devices using liquid inhalable precursors
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/405—Methods of mixing liquids with liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/43—Mixing liquids with liquids; Emulsifying using driven stirrers
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Abstract
The application relates to the field of electronic cigarette oil, in particular to nicotine salt and a preparation method thereof, wherein the nicotine salt is prepared from the following raw materials in parts by weight: 30-40 parts of nicotine, 20-25 parts of benzoic acid, 7-11 parts of auxiliary synergist and 24-43 parts of propylene glycol, wherein the total parts are 100 parts; the nicotine is artificially synthesized nicotine, and the EE value of the levorotatory nicotine relative to the dextrorotatory nicotine in the nicotine is more than 99 percent. The nicotine salt can be used for preparing the electronic cigarette tobacco tar, the inhibiting effect of the high-concentration nicotine salt on the fragrance of the perfume is reduced, the electronic cigarette tobacco tar has the advantages of strong throat exciting feeling, high comfortable feeling, natural and pleasant fragrance, no miscellaneous gas and peculiar smell, the more pleasant and natural fragrance and taste are released, and the symptoms of nausea and retching, cough, excessive phlegm and the like after smoking are relieved to a certain extent.
Description
Technical Field
The application relates to the field of electronic cigarette oil, in particular to nicotine salt and a preparation method thereof.
Background
Nicotine is commonly known as nicotine, belongs to pyridine derivative alkaloids, has certain alkalinity, and can react with acid to produce amine salt, so the nicotine salt is essentially amine salt, and compared with nicotine per se, the nicotine salt has much less stimulation to mucous membranes of oral cavity or throat; nicotine salts have gradually replaced traditional nicotine tobacco tar because they are perceived as similar to the physiological satisfaction of traditional cigarettes.
However, in order to achieve physiological satisfaction of nicotine salts and to match the taste bud requirements of nicotine tobacco products, it is desirable to have higher concentrations of nicotine salts in e-cigarettes (up to 40-50mg/mL is required for nicotine salts in e-cigarettes); however, the high-concentration nicotine salt is easy to reduce the comfort of the atomizing taste of the electronic cigarette oil, and the high-concentration nicotine salt is easy to interfere with the electronic cigarette oil, so that the purity of the aroma of the spice in the electronic cigarette oil is reduced, and the sensory suction effect of the spice in the electronic cigarette oil is influenced.
Disclosure of Invention
In order to reduce the inhibiting effect of high-concentration nicotine salt on perfume fragrance, the application provides nicotine salt and a preparation method thereof.
In a first aspect, the present application provides a nicotine salt, which adopts the following technical scheme:
a nicotine salt is prepared from the following raw materials in parts by weight: 30-40 parts of nicotine, 20-25 parts of benzoic acid, 7-11 parts of auxiliary synergist and 24-43 parts of propylene glycol, wherein the total parts are 100 parts; the nicotine is artificially synthesized nicotine, and the EE value of the levorotatory nicotine relative to the dextrorotatory nicotine in the nicotine is more than 99 percent.
The inventor finds that the nicotine salt tobacco tar has inhibiting effect on the fragrance of the spice after the concentration of the nicotine salt is increased, so that the smoking taste of the electronic tobacco tar is poor; after research, the nicotine extracted from the tobacco leaves harmful impurities such as anatabine, dieneonicotin, cotinine, meslamin, nicotine-N-oxide, nornicotine and/or anabasine and the like, which are not beneficial to human health, and the nicotine salt prepared from the artificial nicotine is prepared into the electronic cigarette tobacco tar, so that the smoking taste of the nicotine salt tobacco tar is kept at a better physiological satisfaction and the requirement for bud taste even if the concentration of the artificial nicotine salt is improved.
After further research, the EE value of the L-nicotine relative to the D-nicotine in the artificially synthesized nicotine is more than 99%, harmful impurities such as anatabine, dienone, cotinine, mesmine, nicotine-N-oxide, nornicotine and/or anabasine and the like are further greatly reduced, and even the corresponding harmful impurities are not detected; meanwhile, after the nicotine salt prepared from the artificial synthetic nicotine with the EE value of more than 99 percent of the levorotatory nicotine and the dextrorotatory nicotine is prepared into the electronic tobacco tar, even if the concentration of the artificial synthetic nicotine salt is improved, the physical satisfaction intensity and the taste bud requirement are extremely excellent, the suppression effect of the high-concentration nicotine salt on the fragrance of the spice can be greatly improved while the nicotine tobacco tar is matched, the natural degree of the fragrance of the spice is reduced, and the smoking taste of the nicotine salt tobacco tar is improved.
Preferably, the auxiliary synergist is selected from two or more of propionic acid, levulinic acid, lactic acid, citric acid, tartaric acid, acetic acid, oxalic acid, succinic acid, gluconic acid, formic acid, propionic acid, malonic acid, lactic acid, butyric acid, isobutyric acid, fumaric acid, valeric acid, isovaleric acid, adipic acid, sorbic acid, phytic acid, heptanoic acid, benzoic acid, salicylic acid, gallic acid, phenylacetic acid, pelargonic acid, cinnamic acid, capric acid, edetic acid, lauric acid, myristic acid, palmitic acid and the like.
Preferably, the auxiliary synergist is selected from any three of propionic acid, levulinic acid, lactic acid, citric acid and tartaric acid.
By adopting the technical scheme, the auxiliary synergist can improve the smoking taste of the nicotine salt tobacco tar, and can effectively improve the physiological satisfaction and the taste bud requirements of the nicotine salt tobacco tar in the aspects of throat stimulation, fragrance, comfort and the like by combining other components.
Preferably, the auxiliary synergist is selected from propionic acid, levulinic acid and lactic acid.
Preferably, the mass ratio of the propionic acid to the levulinic acid to the lactic acid is (1-2): (6-8): (0.1-0.2).
By adopting the technical scheme, the propionic acid, the levulinic acid and the lactic acid have special synergistic action, the smoke aroma generated by the prepared electronic cigarette tobacco tar after atomization is plump and exquisite, and the special synergistic action among the propionic acid, the levulinic acid and the lactic acid has a good enhancement effect on the smoking taste of the electronic cigarette tobacco tar.
Preferably, the mass ratio of the nicotine to the benzoic acid is (1-2): 1.
by adopting the technical scheme, the addition amount of benzoic acid is insufficient, nicotine is difficult to react with acid sufficiently to generate nicotine salt, so that smoke generated by atomization of corresponding electronic cigarette oil is good in throat irritation feeling, but poor in comfortableness of oral cavity and nasal cavity.
Preferably, the toothpaste also comprises 2-5 parts by weight of erythritol and 1-3 parts by weight of trehalose.
By adopting the technical scheme, the erythritol and the trehalose have a special synergistic effect, and the synergistic effect of the erythritol and the trehalose can effectively improve the heavy feeling and the smooth feeling of smoke generated by atomizing the electronic cigarette tobacco tar, reduce the bitter feeling, effectively mask the peculiar smell and improve the taste and the flavor of the electronic cigarette tobacco tar; meanwhile, the flavor of the trehalose can improve the sweet and greasy taste of the propylene glycol in the smoke generated after atomization, the natural degree of the essence can be well maintained and exerted, the enhancement and improvement effects are realized, the reduction and covering effects on the unpleasant tastes such as bitter taste and astringent taste and certain pungent tastes are realized, and the taste is better; trehalose still has certain effect to the stability of electron tobacco tar, and the invariable inactivation of each raw materials of effectual protection is favorable to reducing the oxidation rate of each raw materials to make the stable performance synergism of each raw materials promote the suction taste of electron tobacco tar, make the flue gas that the electron tobacco tar produced through the atomizing milder more delicious, smooth thick, reduce effective component's loss, thereby guarantee the stability of product quality itself.
In a second aspect, the present application provides a method for preparing a nicotine salt, which adopts the following technical scheme:
a method of preparing a nicotine salt comprising the steps of:
the nicotine salt is prepared from the following raw materials in parts by weight: 30-40 parts of nicotine, 20-25 parts of benzoic acid, 7-11 parts of auxiliary synergist and 24-43 parts of propylene glycol, wherein the total parts are 100 parts; the nicotine is artificially synthesized nicotine, and the EE value of the levorotatory nicotine relative to the dextrorotatory nicotine in the nicotine is more than 99 percent;
s1, mixing the benzoic acid with propylene glycol, heating and stirring until the benzoic acid is fully dissolved;
s2, cooling the mixed solution of benzoic acid and propylene glycol to normal temperature, mixing the mixed solution with the auxiliary synergist, erythritol and trehalose, stirring, adding nicotine while stirring for 10-15min, wherein the stirring temperature is 30-60 ℃;
and S3, cooling the mixture obtained in the step S2 to room temperature to obtain the nicotine salt.
In summary, the present application has the following beneficial effects:
1. because the artificial synthetic nicotine with the EE value of more than 99 percent of the levorotatory nicotine relative to the dextrorotatory nicotine is adopted, the nervous activity and the impurity of the levorotatory nicotine are greatly reduced, the inhibiting effect of high-concentration nicotine salt on the fragrance of the spice is reduced, and the effects of multiple indexes of strong throat stimulation, high comfort, natural and pleasant fragrance and no offensive odor and peculiar smell are obtained, the nicotine salt prepared from the artificial synthetic nicotine has obvious advantages in taste and comfort compared with the naturally extracted nicotine in the application of the nicotine salt to the electronic cigarette oil, and the throat stimulation is gradually improved along with the increase of the concentration of the levorotatory nicotine, so the nicotine extracted from plants is optimal in the intensity of physiological satisfaction;
2. propionic acid, levulinic acid and lactic acid are preferably adopted as auxiliary synergists in the application, and due to the specific grading of the propionic acid, the levulinic acid and the lactic acid, the effect that smoke generated by atomizing the electronic cigarette oil has the characteristics of thick throat hitting feeling, low nasal cavity peculiar smell and reduced oral cavity pungent feeling is obtained, the inhibition effect of high-concentration nicotine salt on fragrance is remarkably reduced, more pleasant and natural fragrance and taste are released, and the symptoms of nausea, retching, cough, excessive phlegm and the like after smoking are relieved to a certain extent;
3. in the application, the erythritol and the trehalose are preferably used as part of raw materials for preparing the nicotine salt, and the erythritol and the trehalose have a special synergistic effect, so that the thick and smooth feeling of smoke generated by atomizing the electronic cigarette tobacco tar is improved, the bitter feeling is reduced, the peculiar smell is effectively masked, and the taste and the flavor of the electronic cigarette tobacco tar are improved; meanwhile, the trehalose has a good synergistic effect on the benzoic acid and the auxiliary synergist, so that the stability of the benzoic acid and the auxiliary synergist can be improved, nicotine can be more fully converted into nicotine salt, the effect of the auxiliary synergist on improving the overall taste of the electronic cigarette oil is enhanced, smoke generated by atomizing the electronic cigarette oil is milder and more delicious, smooth and thicker, the loss of effective components is reduced, and the stability of the quality of the product is ensured;
4. trehalose is preferably adopted as one of raw materials for preparing the nicotine salt, and the fragrance of the trehalose can improve the sweet and greasy taste of propylene glycol in smoke generated after atomization, simultaneously the naturalness of essence can be well maintained and exerted, and the trehalose has the effects of strengthening and improving, has the effects of reducing and covering the unpleasant tastes such as bitter taste and astringent taste and certain pungent tastes, and has better mouthfeel; simultaneously, trehalose can form unique protection film on each raw materials surface, and the indeformable inactivation of each raw materials of effectual protection to make the stable performance synergism of each raw materials promote the suction taste of electron tobacco tar, thereby prolonged the life of electron tobacco tar.
Drawings
FIG. 1 is a gas chromatogram of a nicotine sample for purity analysis in example 1.
FIG. 2 is a high performance liquid chromatogram of a chiral analysis performed on a nicotine sample in example 1.
Fig. 3 is a gas chromatogram of a nicotine sample for purity analysis in comparative example 1.
FIG. 4 is a high performance liquid chromatogram of a chiral analysis performed on a nicotine sample of comparative example 1.
Fig. 5 is a gas chromatogram of a nicotine sample for purity analysis in comparative example 2.
FIG. 6 is a high performance liquid chromatogram of a chiral analysis performed on a nicotine sample of comparative example 2.
FIG. 7 is a high performance liquid chromatogram of a chiral analysis performed on a nicotine sample of comparative example 3.
Detailed Description
Example 1
A nicotine salt is prepared from the following raw materials in parts by weight: 30 parts of nicotine, 25 parts of benzoic acid, an auxiliary synergist, 3 parts of erythritol, 2 parts of trehalose and 29.8 parts of propylene glycol, wherein the total is 100 parts; the auxiliary synergist is prepared from the following raw materials in parts by weight: 2 parts of propionic acid, 5 parts of levulinic acid, 0.2 part of lactic acid, 2 parts of citric acid and 1 part of tartaric acid. Wherein the nicotine is artificially synthesized nicotine purchased from Henoco creatures, and the nicotine content is more than or equal to 99.5%.
The process for preparing the nicotine salt of this example comprises the following steps:
s1, mixing the benzoic acid and the propylene glycol which are weighed according to the proportion, and heating and stirring the mixture by using a magnetic heating stirrer until the benzoic acid is fully dissolved;
s2, cooling the mixed solution obtained in the step S1 to normal temperature, mixing the cooled mixed solution with the auxiliary synergist, fully stirring the mixed solution for 10min, slowly adding nicotine while stirring the mixed solution, and controlling the temperature to be 35 ℃;
and S3, cooling the mixed solution obtained in the step S2 to room temperature to obtain the nicotine salt.
As shown in fig. 1, the purity of the synthesized nicotine sample was analyzed by gas chromatography, and the gas chromatography signal of nicotine is tabulated in table 1, and the purity of nicotine was as high as 99.58% with a retention time of 14.921 min.
Table 1 gas chromatography signal tabulation of nicotine samples in example 1
The above synthesized nicotine sample was subjected to impurity analysis by gas chromatography-mass spectrometer to find anatabine (C) in nicotine10H12N2) Neonicotinoid (C)10H14N2) The impurities such as dieneonicotinyl, cotinine and mesamin were very low or even no corresponding impurities were detected, as shown in table 2.
Table 2 gas chromatography-mass spectrometry analysis of impurities for nicotine samples in example 1
As shown in FIG. 2, chiral analysis was performed on the synthesized nicotine sample by HPLC using EtOH HEXANE Et2NH, the sample concentration is 1mg/mL, the sample volume is 5 muL, the sample introduction channel is W2996, the liquid chromatogram signal list of nicotine is shown in Table 3, and the EE value of levorotatory nicotine relative to dextrorotatory nicotine is as high as 99.28%.
Table 3 chiral analysis of liquid chromatography analysis of nicotine samples in example 1
Comparative example 1
The difference between the comparative example 1 and the example 1 is that the nicotine is artificially synthesized nicotine purchased from Henoco creatures, the EE value of the levorotatory nicotine relative to the dextrorotatory nicotine is lower than that of the levorotatory nicotine relative to the dextrorotatory nicotine in the example 1, and the nicotine content is more than or equal to 99.5 percent.
As shown in fig. 3, the purity of the synthesized nicotine sample was analyzed by gas chromatography, and the gas chromatography signal of nicotine is tabulated in table 4, which can obtain the purity of nicotine as high as 98.79% and the retention time of 14.907 min.
Table 4 gas chromatography signal tabulation of nicotine samples in comparative example 1
Is aligned by a gas chromatography-mass spectrometerThe synthesized nicotine sample is analyzed for impurities, and the anatabine (C) in the nicotine is found10H12N2) Neonicotinoid (C)10H14N2) Diene nicotine was not detected, but contained small amounts of cotinine and mesalamine, as shown in table 5.
TABLE 5 GC-MS analysis of impurities analysis of nicotine samples from comparative example 1
As shown in FIG. 4, chiral analysis was performed on the nicotine sample synthesized as described above by HPLC using EtOH HEXANE Et2NH, the injection concentration is 1mg/mL, the injection volume is 5 muL, the injection channel is W2996, the liquid chromatogram signal list of nicotine is shown in Table 6, and the EE value of levorotatory nicotine relative to dextrorotatory nicotine is 79.28%.
TABLE 6 chiral analysis of liquid chromatography analysis of nicotine samples in comparative example 1
Comparative example 2
The difference between the comparative example 2 and the example 1 is that the nicotine is obtained from Nicotiana and extracted from tobacco, and has a higher relative levorotatory-to-dextrorotatory-nicotine EE value than that of the example 1 and the comparative example 1, and the nicotine content is more than or equal to 99.5%.
As shown in fig. 5, the purity of the synthesized nicotine sample was analyzed by gas chromatography, and the gas chromatography signal of nicotine is tabulated in table 7, and the purity of nicotine was 99.69% and the retention time was 14.898 min.
Table 7 gas chromatography signal tabulation of nicotine samples from comparative example 2
The impurity analysis of the synthesized nicotine sample by a gas chromatography-mass spectrometer shows that the nicotine contains anatabine (C)10H12N2) Neonicotinoid (C)10H14N2) Diene nicotine, cotinine, and mesalamine, and the like, with higher impurity content, as shown in table 8.
TABLE 8 GC-MS analysis of impurities analysis of nicotine samples in comparative example 2
As can be seen from tables 2, 5 and 8, the content of metabolic derivatives of nicotine such as anatabine, anabasine, diennicotine, etc. in the synthetic nicotine (i.e., example 1 and comparative example 1) is significantly lower than that of the plant-extracted nicotine (i.e., comparative example 2), which is advantageous in that example 1 and comparative example 1 ensure that the odor of nicotine salt is hardly affected by the unpleasant taste of the substance such as metabolic derivatives of nicotine.
As shown in FIG. 6, chiral analysis was performed on the nicotine sample synthesized as described above by HPLC using EtOH HEXANE Et2NH, the injection concentration is 1mg/mL, the injection volume is 5 muL, the injection channel is W2996, the liquid chromatogram signal list of nicotine is shown in Table 9, and the EE value of levorotatory nicotine relative to dextrorotatory nicotine is 99.72%.
TABLE 9 chiral analysis of liquid chromatography analysis of nicotine samples in comparative example 2
Combining example 1 with tables 3, 6 and 9, it can be seen that the EE value of l-nicotine versus d-nicotine in example 1 can reach over 99%, so that the l-nicotine content in example 1 can be compared favorably with the high l-nicotine content in plant-extracted nicotine (i.e., comparative example 2).
The purity contrast (gc-ar) of the nicotine samples in example 1 and comparative examples 1-2 is summarized in the following table:
it can be seen from the table that the synthetic nicotine (i.e. example 1) is completely comparable to the plant-extracted nicotine (i.e. comparative example 2) in terms of purity and L-nicotine content, and the contents of impurities such as anatabine, neonicotinoid, cotinine, macramine and diennicotinoid in the synthetic nicotine are far lower than the levels of the corresponding impurities in the plant-extracted nicotine. Therefore, the nicotine of example 1 was used as a raw material for preparing the nicotine salt in each of examples 3 to 10 and comparative example 4 described below.
Comparative example 3
The difference between the comparative example 3 and the example 1 is that the nicotine is artificial synthesized racemic nicotine purchased from Heno organism, and the type of the racemic nicotine is that the nicotine content is more than or equal to 99.5 percent.
As shown in FIG. 7, chiral analysis was performed on the nicotine sample synthesized as described above by HPLC using EtOH HEXANE Et2NH, the sample concentration is 1mg/mL, the sample volume is 5 muL, the sample injection channel is W2996, the liquid chromatogram signal list of nicotine is shown in Table 10, and the EE value of levorotatory nicotine relative to dextrorotatory nicotine is-0.02%.
TABLE 10 chiral analysis of liquid chromatography analysis of nicotine samples in comparative example 3
Examples 2 to 9
Examples 2-9 differ from example 1 in the composition or amount of the starting materials used in the nicotine salt preparation process, see in particular tables 11 and 12.
Comparative example 4
The difference between the comparative example 4 and the example 1 is that the addition amount of each component in the raw material of the nicotine salt is different; specifically, the nicotine salt is prepared from the following raw materials in parts by weight: 42 parts of nicotine, 15 parts of benzoic acid, an auxiliary synergist, 2 parts of erythritol, 2 parts of trehalose and 30.8 parts of propylene glycol, wherein the total parts are 100 parts; the auxiliary synergist is prepared by mixing the following raw materials in parts by weight: 2 parts of propionic acid, 6 parts of levulinic acid and 0.2 part of lactic acid.
TABLE 11 EXAMPLES 1-4 compositions and amounts of the respective feed Components
Table 12 compositions and amounts of respective raw material components of examples 5 to 9 and comparative example 4
Test method
First, professional technicians perform sensory smoking evaluation on nicotine salt
1. Design of experiments
The nicotine salts prepared in examples 1-9 and comparative examples 1-4 were formulated to an electronic cigarette liquid according to the same liquid flavor formulation, injected into the same electronic cigarette cartridge equipment, and blindly tested by multiple professional evaluation technicians. Electronic cigarette evaluation equipment: AIRSCREAM tobacco stems and empty cartridges.
Specifically, the electronic cigarette tobacco tar is prepared by mixing the following raw materials in parts by weight: 2 parts of nicotine salt, 1.5 parts of grape essence, 1.5 parts of propylene glycol and 10 parts of glycerol in total in the balance; the nicotine salt concentration in the tobacco tar is about 50 mg/mL. The electronic cigarette liquid prepared from the nicotine salt prepared in example 2 and example 9 was kept for six months as comparative test 1 (using the nicotine salt prepared in example 2) and comparative test 2 (using the nicotine salt prepared in example 9).
The essence of the electronic cigarette tobacco tar is illustrated by adding 1.5 parts of grape essence, and the adding type and the adding amount of the essence are not limited; the electronic cigarette tobacco tar is exemplified by adding 1.5 parts of propylene glycol and 5 parts of glycerol, and the adding type and the adding amount of the nicotine salt solvent are not limited; the electronic cigarette liquid is exemplified by adding 2 parts of nicotine salt, and the adding amount of the nicotine salt is not limited.
The sensory aspiration evaluation method comprises the following steps: setting five evaluation indexes including throat feeling, irritation, aroma and miscellaneous gas, and giving different scores according to different influence degrees of the evaluation indexes on the sensory quality of the electronic cigarette tobacco.
Throat hitting feeling: the electronic cigarette smoke is inhaled by smoke generated by atomization and then stimulates the throat and the lung;
irritation: the smoke generated by atomizing the smoke oil inhaled into the electronic cigarette can generate uncomfortable feeling on sense organs including oral cavity, throat and nasal cavity;
fragrance: the electronic cigarette tobacco tar can have the fragrance in the smoking process;
miscellaneous gas: the electronic cigarette tobacco tar produces the bad smell of the non-tobacco tar during smoking.
The sensory quality evaluation indexes and the evaluation value meaning tables of the electronic cigarette tobacco tar are shown in table 14.
TABLE 13 sensory quality evaluation index and evaluation value of electronic cigarette tobacco tar
2. Evaluation method
15 evaluators were set, each person used an electronic cigarette tobacco sensory quality evaluation table, smoking the electronic cigarette tobacco tar prepared in examples 1 to 9, comparative examples 1 to 4, and comparative tests 1 to 2 by a dark evaluation method and an overall cyclic evaluation method, and comprehensive evaluation was performed on the sensory quality of the electronic cigarette tobacco tar by a percentage evaluation method according to the meaning of the evaluation index scores of the five sensory smoking evaluation indexes in table 13, and each evaluation index was scored by twenty degrees.
According to the evaluation indexes and the score values in table 13, the evaluators should perform sensory quality evaluation on each evaluation index, and record the evaluation results, with the minimum score unit of the score value being 0.5.
3. Statistics of results
The lowest score and the highest score are removed from the sensory quality evaluation results of all evaluators, the arithmetic mean of the scores of the remaining effective single evaluation indexes is calculated, finally, the sensory quality evaluation comprehensive score of the electronic cigarette tobacco tar is the sum of the arithmetic mean of the scores of the single evaluation indexes, so as to obtain the total score, and the comparative evaluation results of the electronic cigarette tobacco tar prepared in the examples 1-9, the comparative examples 1-4 and the comparative experiments 1-2 are shown in the table 14.
TABLE 14 comparative evaluation results of E-cigarette tobacco tar obtained in examples 1 to 9, comparative examples 1 to 4, and comparative tests 1 to 2
Combining example 1 and comparative examples 1-3 and table 14, it can be seen that example 1 and comparative example 2 with high levels of levorotatory nicotine are the strongest in the physiological satisfaction of the throat-stimulating sensation, followed by comparative example 1 with slightly less levorotatory nicotine and the weakest of the throat-stimulating sensation is comparative example 3 lacking levorotatory nicotine.
In terms of the comfort of the oral cavity and the nasal cavity, the comfort of the comparative example 3 is the best, the irritation of the oral cavity and the nasal cavity is the weakest, and the comfort of the oral cavity and the nasal cavity is the second time of the comfort of the example 1 and the comfort of the comparative example 1; comparative example 2 has a more obvious pungency on the lingual surface of the oral cavity and is strongest in the irritation of the oral cavity and the nasal cavity, the smoke generated by the atomization of the electronic cigarette oil has a little offensive odor, the fragrance naturalness is insufficient, the comfort score of comparative example 3 is the highest on the comprehensive application score, the comfort score of comparative example 2 is the lowest, and the comfort score of comparative example 1 and the comfort score of example 1 are centered.
In the aspect of aroma and miscellaneous gas performance, compared with the smoke generated by atomizing the inhaled electronic cigarette tobacco tar in the comparative example 1, the comparative example 3 and the example 1, the smoke generated by the atomization of the inhaled electronic cigarette tobacco tar has obvious baking aroma and scorching aroma in the first aroma section of the nose aroma, the natural feeling of grape aroma is poor, and the comparative example 1, the comparative example 3 and the example 1 are basically equal.
Compared with nicotine salt prepared by blending nicotine extracted from tobacco, smoke generated by atomizing electronic cigarette oil prepared from the synthetic nicotine has the characteristics of thick throat hitting feeling, low nasal cavity peculiar smell and reduced oral cavity pungent feeling, the suppression effect of high-concentration nicotine salt on aroma can be obviously reduced, more pleasant and natural aroma and taste are released, and symptoms of nausea, retching, cough, excessive phlegm and the like after smoking are relieved to a certain extent.
As can be seen by combining examples 1-7 and table 14, the propionic acid, the levulinic acid and the lactic acid have special synergistic effect, and the smoke fragrance generated by atomizing the electronic cigarette tobacco tar prepared in the inhalation examples 2-4 is fullest and exquisite; when the smoking mouthfeel of the prepared electronic cigarette oil is influenced by increasing or reducing the adding amount of a certain component, the special synergistic effect of the propionic acid, the levulinic acid and the lactic acid has a good enhancement effect on the smoking mouthfeel of the electronic cigarette oil.
As can be seen from the combination of examples 2 to 4 and comparative example 4 and table 14, in comparative example 4, after the addition of benzoic acid is reduced, nicotine hardly reacts with acid to form nicotine salt, so that the smoke generated by atomizing the electronic cigarette smoke inhaled in comparative example 4 has better throat irritation, but has poorer comfort in the oral cavity and the nasal cavity.
It can be seen from a combination of examples 2-4 and examples 8-9, and from Table 14 that the overall characteristic requirements of examples 2-4 are most desirable. The synergistic effect of the erythritol and the trehalose can effectively improve the heavy feeling and the smooth feeling of smoke generated by atomizing the electronic cigarette tobacco tar, reduce the bitter feeling, effectively mask the peculiar smell and improve the taste and the flavor of the electronic cigarette tobacco tar. Meanwhile, the flavor of the trehalose can improve the sweet and greasy taste of the propylene glycol in the smoke generated after atomization, the naturalness of the essence can be well maintained and exerted, the enhancement and improvement effects are realized, the reduction and covering effects on unpleasant tastes such as bitter taste and astringent taste and certain pungent tastes are realized, and the taste is better.
Combining the example 2 and the comparative tests 1-2, it can be seen that the smoking evaluation is performed after the electronic cigarette oil prepared by the comparative tests 1-2 is reserved for six months, and the reserved smoking taste of the comparative test 2 is changed greatly. This is because trehalose has certain effect to the stability of electron tobacco tar, trehalose can form unique protection film on each raw materials surface, the unchangeable deactivation of each raw materials of effectual protection, be favorable to reducing the oxidation rate of each raw materials, thereby make the stable performance synergism of each raw materials promote the suction taste of electron tobacco tar, the promotion effect of supplementary synergist to the whole taste of electron tobacco tar is strengthened, make the flue gas that the electron tobacco tar produced through the atomizing milder more delicious, smooth and thick, reduce the loss of active ingredient, thereby guarantee the stability of product quality itself.
The artificial synthesized nicotine salt has obvious advantages in taste and comfort compared with the naturally extracted nicotine in the aspect of application to electronic cigarette oil, and the excited throat feeling is gradually improved along with the increase of the concentration of the levorotatory body, so that the nicotine extracted from plants is optimal in the aspect of physiological satisfaction strength, which indirectly proves that the levorotatory nicotine has nerve activity, and the artificial synthesized nicotine also has gradually improved physiological stimulation along with the increase of the concentration of the levorotatory body.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (7)
1. A nicotine salt characterized by: the feed is prepared from the following raw materials in parts by weight: 30-40 parts of nicotine, 20-25 parts of benzoic acid, 7-11 parts of auxiliary synergist and 24-43 parts of propylene glycol, wherein the total parts are 100 parts; the nicotine is artificially synthesized nicotine, and the EE value of the levorotatory nicotine relative to the dextrorotatory nicotine in the nicotine is more than 99 percent.
2. A nicotine salt according to claim 1, characterized in that: the auxiliary synergist is selected from two or more of propionic acid, levulinic acid, lactic acid, citric acid and tartaric acid.
3. A nicotine salt according to claim 2, characterized in that: the auxiliary synergist is selected from propionic acid, levulinic acid and lactic acid.
4. A nicotine salt according to claim 2, characterized in that: the mass ratio of the propionic acid to the levulinic acid to the lactic acid is (1-2): (6-8): (0.1-0.2).
5. A nicotine salt according to claim 1, characterized in that: the mass ratio of the nicotine to the benzoic acid is (1-2): 1.
6. a nicotine salt according to claim 1, characterized in that: also comprises 2-5 parts of erythritol and 1-3 parts of trehalose.
7. A method of preparing a nicotine salt according to any of claims 1-6, comprising the steps of:
s1, mixing the benzoic acid with propylene glycol, heating and stirring until the benzoic acid is fully dissolved;
s2, cooling the mixed solution of benzoic acid and propylene glycol to normal temperature, mixing the mixed solution with the auxiliary synergist, erythritol and trehalose, stirring, adding nicotine while stirring for 10-15min, wherein the stirring temperature is 30-60 ℃;
and S3, cooling the mixture obtained in the step S2 to room temperature to obtain the nicotine salt.
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