CN114304713B - Electronic cigarette liquid containing hyaluronic acid composition and preparation method thereof - Google Patents
Electronic cigarette liquid containing hyaluronic acid composition and preparation method thereof Download PDFInfo
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Abstract
The invention provides an electronic cigarette liquid and a preparation method thereof. Wherein the first hyaluronic acid or its salt has a molecular weight of 10-50kDa, and the second hyaluronic acid or its salt has a molecular weight of 100-400kDa. According to the invention, the hyaluronic acid composition with the biological active ingredient is added into the electronic cigarette liquid, so that the electronic cigarette liquid has high water retention, discomfort symptoms such as dry mouth, dry throat, throat itching, pharyngitis and the like caused by an electronic cigarette are improved, and meanwhile, the hyaluronic acid with higher molecular weight and better moisture retention is added into the electronic cigarette liquid through reasonable proportioning of the hyaluronic acids with different molecular weights, so that the general problem that the high molecular weight hyaluronic acid liquid blocks a filter element for a long time is solved, and the atomization effect of the effective ingredients in the liquid is improved.
Description
Technical Field
The invention belongs to the technical field of novel tobacco, and particularly relates to electronic cigarette liquid containing a hyaluronic acid composition and a preparation method thereof.
Background
The electronic cigarette (e-cigarette) is powered by a lithium ion rechargeable battery, and the electronic cigarette atomized liquid is heated by a specific structure, so that the atomized liquid is heated and flashed to generate aerosol, and the aim of smoking is fulfilled. The electronic cigarette is similar to the traditional cigarette in appearance and taste, does not have cigarette ash, does not burn, does not generate harmful substances, and is popular with consumers. Electronic cigarettes have been widely used since the advent of 2004, with exponential growth in usage throughout the world. The electronic cigarette is publicized vigorously as an auxiliary means for quitting smoking; compared with the traditional cigarette, the cigarette is healthier, cheaper and more socially accepted, however, dry mouth, dry throat, throat itch and pharyngitis are common side effects of the electronic cigarette.
Hyaluronic Acid (HA), also known as hyaluronic acid, is a disaccharide glycosaminoglycan composed of D-glucuronic acid and N-acetylglucosamine, and is a major component constituting connective tissues such as human intercellular substance, ocular vitreous body, synovial fluid of joints, etc., and plays important physiological roles of water retention, extracellular space maintenance, osmotic pressure regulation, lubrication, and cell repair promotion in vivo. Hyaluronic acid molecules contain a large amount of carboxyl and hydroxyl, and hydrogen bonds in molecules and among molecules are formed in an aqueous solution, so that the hyaluronic acid has a strong water retention effect, can be combined with thousands of times of water per se, and can be understood that hyaluronic acid with higher molecular weight has higher water retention within a certain range.
Therefore, hyaluronic acid has long been expected to be used as an additive for electronic cigarette liquid to improve various uncomfortable symptoms caused by electronic cigarettes.
Disclosure of Invention
The hyaluronic acid serving as the electronic cigarette liquid additive has the common problems that an electronic cigarette filter element is very easy to block, the service life of an electronic cigarette is greatly shortened, the practicability is not good, the blockage condition of the electronic cigarette filter element is more serious due to the higher molecular weight of the hyaluronic acid, and the addition of the hyaluronic acid with higher molecular weight and more excellent water retention performance in the electronic cigarette liquid is limited.
A large number of experiments prove that the problem that hyaluronic acid blocks a filter element can be solved obviously by adding the composition containing hyaluronic acid with different molecular weights, and hyaluronic acid with a higher molecular weight can be added into the cigarette liquid of the electronic cigarette, so that the cigarette liquid has better water retention property, and the effect of improving uncomfortable symptoms caused by the electronic cigarette is enhanced.
Therefore, the invention aims to provide electronic cigarette liquid added with a hyaluronic acid composition and a preparation method thereof, and the invention adopts the technical scheme that:
1. an electronic cigarette liquid, characterized in that the electronic cigarette liquid contains a first hyaluronic acid or a salt thereof and a second hyaluronic acid or a salt thereof.
2. The e-cigarette liquid of claim 1, wherein the first hyaluronic acid or salt thereof has a molecular weight of 10-50kDa, preferably 30-50kDa.
3. The e-cigarette liquid of claim 1 or 2, wherein the second hyaluronic acid or salt thereof has a molecular weight of 100-400kDa, preferably 100-150kDa.
4. The electronic cigarette liquid according to any one of claims 1 to 3, wherein the first hyaluronic acid or a salt thereof is contained in an amount of 0.002 to 1.0 part by weight, preferably 0.005 to 0.1 part by weight, relative to 100 parts by weight of the liquid.
5. The electronic cigarette liquid according to any one of items 1 to 4, wherein the second hyaluronic acid or a salt thereof is contained in an amount of 0.001 to 0.1 part by weight, preferably 0.005 to 0.05 part by weight, relative to 100 parts by weight of the liquid.
6. The e-cigarette liquid of any of claims 1-5, wherein the first and second hyaluronic acid salts are sodium, potassium, magnesium, calcium, zinc, bismuth salts of hyaluronic acid.
7. The electronic cigarette liquid according to any one of claims 1 to 6, wherein the first hyaluronic acid and the second hyaluronic acid are pharmaceutical grade hyaluronic acid, preferably the first hyaluronic acid and the second hyaluronic acid are pharmaceutical grade hyaluronic acid prepared by a microbial fermentation method.
8. The e-cigarette liquid of any of claims 1-7, wherein the e-cigarette liquid further comprises glycerin, propylene glycol, water, and/or nicotine.
9. The electronic cigarette liquid according to claim 8, wherein the glycerin is contained in an amount of 20 to 80 parts by weight relative to 100 parts by weight of the liquid; the content of the propylene glycol is 5-60 parts by weight; the content of the water is 0.05 to 3 weight portions.
10. The electronic cigarette liquid of claim 8 or 9, wherein the nicotine is selected from one or more of nicotine base, nicotine salt, and nicotine substitute.
11. A preparation method of electronic cigarette liquid is characterized by comprising the following steps:
mixing glycerol, propylene glycol and/or nicotine, and dissolving to obtain component A;
uniformly mixing and dissolving the first hyaluronic acid or the salt thereof, the second hyaluronic acid or the salt thereof and water to obtain a component B;
and adding the component B into the component A, and uniformly mixing to obtain the electronic cigarette liquid.
12. The e-liquid of claim 11, wherein the first hyaluronic acid or salt thereof has a molecular weight of 10-50kDa, preferably 30-50kDa.
13. The e-cigarette smoke solution of claim 11 or 12, wherein the second hyaluronic acid or salt thereof has a molecular weight of 100-400kDa, preferably 100-150kDa.
14. The electronic cigarette liquid according to any one of claims 11 to 13, wherein the first hyaluronic acid or the salt thereof is contained in an amount of 0.002 to 1.0 part by weight, preferably 0.005 to 0.1 part by weight, based on 100 parts by weight of the liquid.
15. The electronic cigarette liquid according to any one of claims 11 to 14, wherein the second hyaluronic acid or a salt thereof is contained in an amount of 0.001 to 0.1 part by weight, preferably 0.005 to 0.05 part by weight, relative to 100 parts by weight of the liquid.
16. The e-cigarette liquid of any of claims 11-15, wherein the first and second hyaluronic acid salts are sodium, potassium, magnesium, calcium, zinc, bismuth salts of hyaluronic acid.
17. The electronic cigarette liquid of any one of claims 11-16, wherein the first hyaluronic acid or salt thereof and the second hyaluronic acid are pharmaceutical-grade hyaluronic acid or salt thereof, preferably wherein the first hyaluronic acid or salt thereof and the second hyaluronic acid or salt thereof are pharmaceutical-grade hyaluronic acid or salt thereof prepared by a microbial fermentation process.
18. The method according to item 11-17, wherein the dissolution is assisted by using a stirrer, preferably at a stirrer speed of 200-500rpm.
ADVANTAGEOUS EFFECTS OF INVENTION
1. According to the invention, the bioactive component hyaluronic acid composition is added into the electronic cigarette liquid, so that the electronic cigarette liquid has high water retention property, and can improve uncomfortable symptoms such as dry mouth, dry throat, throat itching, pharyngitis and the like caused by the electronic cigarette.
2. According to the invention, through reasonable proportioning of hyaluronic acids with different molecular weights, hyaluronic acid with higher molecular weight and better moisture retention performance is added into the cigarette liquid of the electronic cigarette, so that the general problem that the cigarette liquid of high molecular weight hyaluronic acid blocks a filter element for a long time is solved, and the atomization effect of effective components in the cigarette liquid is improved.
3. The hyaluronic acid with each molecular weight selected by the invention is prepared by microbial fermentation, is a pharmaceutical grade raw material, and greatly ensures the safety of the product.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention and are not intended to be limiting.
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. Although methods and materials similar or equivalent to those described herein can be used in experimental or practical applications, the materials and methods are described below. In case of conflict, the present specification, including definitions, will control, and the materials, methods, and examples are illustrative only and not intended to be limiting. The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
In one aspect, the invention provides an electronic cigarette liquid comprising hyaluronic acid or a salt thereof, wherein the liquid further comprises two hyaluronic acids or salts thereof with different molecular weights, a first hyaluronic acid or a salt thereof and a second hyaluronic acid or a salt thereof.
The types of the electronic cigarette liquid include, but are not limited to, cigar electronic cigarette liquid, pipe electronic cigarette liquid, flat-mouth electronic cigarette liquid, mini electronic cigarette liquid, woman electronic cigarette liquid, cartmizer electronic cigarette liquid (top-quality electronic cigarette liquid), soft-mouthpiece electronic cigarette liquid, disposable cigar electronic cigarette liquid, EGO electronic cigarette liquid, VGO electronic cigarette liquid, mechanical electronic cigarette liquid, high-power electronic cigarette liquid, and the like. The electronic cigarette liquid provided by the invention can be electronic cigarette liquid used by various types of electronic cigarettes.
In the present invention, the term "hyaluronic acid" as a biodegradable polymer having a connection structure in which disaccharide units of N-acetylglucosamine and glucuronic acid are repeated includes not only hyaluronic acid but also all hyaluronate salts including, but not limited to, sodium hyaluronate, potassium hyaluronate, magnesium hyaluronate, calcium hyaluronate, ammonium hyaluronate, calcium hyaluronate, bismuth hyaluronate, zinc hyaluronate, cobalt hyaluronate, and the like, and mixtures thereof.
In certain embodiments of the invention, the first hyaluronic acid or salt thereof may be hyaluronic acid or any hyaluronate salt as described above, the molecular weight of the first hyaluronic acid or salt thereof being 10-50kDa, e.g. the molecular weight may be 10kDa, 12kDa, 14kDa, 16kDa, 18kDa, 20kDa, 21kDa, 23kDa, 25kDa, 27kDa, 29kDa, 30kDa, 32kDa, 35kDa, 38kDa, 40kDa, 42kDa, 44kDa, 46kDa, 48kDa, 50kDa.
In certain preferred embodiments, the first hyaluronic acid or salt thereof has a molecular weight of 30-50kDa.
In certain embodiments of the invention, the second hyaluronic acid or salt thereof may be hyaluronic acid or any hyaluronate salt as described above, the molecular weight of the second hyaluronic acid or salt thereof being 100-400kDa, e.g. the molecular weight may be 100kDa, 106kDa, 110kDa, 130kDa, 150kDa, 160kDa, 180kDa, 200kDa, 220kDa, 250kDa, 270kDa, 290kDa, 300kDa, 320kDa, 340kDa, 360kDa, 380kDa, 400kDa.
In certain preferred embodiments, the second hyaluronic acid or salt thereof has a molecular weight of 100-150kDa.
In certain specific embodiments of the electronic cigarette liquid provided by the present invention, the first hyaluronic acid or a salt thereof is contained in an amount of 0.002 to 1.0 part by weight, for example, 0.002 part by weight, 0.005 part by weight, 0.008 part by weight, 0.01 part by weight, 0.015 part by weight, 0.02 part by weight, 0.026 part by weight, 0.03 part by weight, 0.04 part by weight, 0.05 part by weight, 0.07 part by weight, 0.09 part by weight, 0.1 part by weight, 0.15 part by weight, 0.2 part by weight, 0.25 part by weight, 0.3 part by weight, 0.4 part by weight, 0.5 part by weight, 0.6 part by weight, 0.7 part by weight, 0.8 part by weight, 0.85 part by weight, 0.88 part by weight, 0.9 part by weight, 0.92 part by weight, 0.94 part by weight, 0.96 part by weight, 0.99 part by weight, 1.99 part by weight, relative to 100 parts by weight of the cigarette liquid.
In certain preferred embodiments, the first hyaluronic acid or salt thereof is present in an amount of 0.005-0.1 parts by weight.
In certain specific embodiments of the electronic cigarette smoke solution provided by the present invention, the second hyaluronic acid or a salt thereof is contained in an amount of 0.001 to 0.1 parts by weight, for example, 0.002 parts by weight, 0.005 parts by weight, 0.008 parts by weight, 0.01 parts by weight, 0.015 parts by weight, 0.02 parts by weight, 0.026 parts by weight, 0.03 parts by weight, 0.035 parts by weight, 0.04 parts by weight, 0.045 parts by weight, 0.05 parts by weight, 0.055 parts by weight, 0.06 parts by weight, 0.065 parts by weight, 0.07 parts by weight, 0.075 parts by weight, 0.08 parts by weight, 0.085 parts by weight, 0.09 parts by weight, 0.095 parts by weight, 0.1 parts by weight, relative to 100 parts by weight of the smoke solution.
In certain preferred embodiments, the second hyaluronic acid or salt thereof is present in an amount of 0.005-0.05 parts by weight.
The first and second hyaluronic acid salts can be any salt of hyaluronic acid, including, but not limited to, sodium hyaluronate, potassium hyaluronate, magnesium hyaluronate, calcium hyaluronate, ammonium hyaluronate, calcium hyaluronate, bismuth hyaluronate, zinc hyaluronate, or cobalt hyaluronate, and the like, in certain embodiments, the first and second hyaluronic acid salts are the same hyaluronic acid salt, and in certain embodiments, the first and second hyaluronic acid salts are different hyaluronic acid salts.
In certain preferred embodiments, the first and second hyaluronic acid salts are selected from the group consisting of hyaluronic acid sodium salt, hyaluronic acid potassium salt, hyaluronic acid magnesium salt, hyaluronic acid calcium salt, hyaluronic acid zinc salt, hyaluronic acid bismuth salt.
The electronic cigarette liquid of the present invention further contains glycerin, propylene glycol, water and/or nicotine.
In certain embodiments, the glycerol is present in an amount of 20 to 80 parts by weight, for example in an amount of 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, relative to 100 parts by weight of the tobacco smoke.
In certain embodiments, the propylene glycol is present in an amount of 5 to 60 parts by weight, for example in an amount of 5, 8, 9, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, relative to 100 parts by weight of the tobacco smoke.
In certain embodiments, the water is present in an amount of 0.05 to 3 parts by weight, for example 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.5, 2.0, 2.5, 3.0, relative to 100 parts by weight of the tobacco smoke.
The water may be deionized water, distilled water, ultrapure water, or the like.
Forms of said nicotine include, but are not limited to: nicotine in free base form; protonated or partially protonated nicotine; nicotine salts, and in particular acid addition salts formed by addition of inorganic or organic acids, such as nicotine bitartrate or nicotine hydrochloride; solvates, hydrates, clathrates, complexes, and the like. Since nicotine in its pure free base form is a liquid at room temperature, these forms include nicotine in liquid form or nicotine in particulate (which may be micronized, crystalline and/or amorphous) form (e.g., nicotine salt), as well as any mixture of the foregoing forms.
Such nicotine substitutes include, but are not limited to, caffeine, kava, passion flower, calamus, and the like.
The electronic cigarette liquid of the invention can further contain essence and taste improvement additives.
The flavoring may be any flavoring used in tobacco liquids, including but not limited to tobacco flavoring, mint flavoring, fruit flavoring, chocolate flavoring, and the like.
The mouthfeel improving additives include, but are not limited to, acidulants, sweeteners, peppers, bitterants, throat-soothing agents, deionized water, and the like.
In another aspect, the present invention further provides a preparation method of an electronic cigarette liquid, including:
mixing glycerol, propylene glycol and/or nicotine, and dissolving to obtain component A;
mixing and dissolving the first hyaluronic acid or salt thereof, the second hyaluronic acid or salt thereof and water uniformly to obtain a component B;
and adding the component B into the component A, and uniformly mixing to obtain the electronic cigarette liquid.
In a specific embodiment, glycerin and propylene glycol are mixed and dissolved uniformly to obtain a component A; mixing and dissolving the first hyaluronic acid or salt thereof, the second hyaluronic acid or salt thereof and water uniformly to obtain a component B; and adding the component B into the component A, and uniformly mixing to obtain the electronic cigarette liquid.
In a specific embodiment, glycerin, propylene glycol and nicotine are mixed and dissolved uniformly to obtain a component A; mixing and dissolving the first hyaluronic acid or salt thereof, the second hyaluronic acid or salt thereof and water uniformly to obtain a component B; and adding the component B into the component A, and uniformly mixing to obtain the electronic cigarette liquid.
In certain preferred embodiments, the a-component, B-component, and the e-liquid are performed in a clean reaction kettle.
The mixing and dissolving may be any means that allows complete and uniform dissolution of the substances, including but not limited to manual stirring, ultrasonic stirring, stirrer stirring, heating, and the like.
In certain embodiments, the present invention utilizes an agitator to effect dissolution with agitation.
The stirrer may stir at a speed of 200 to 500rpm, which may be, for example, 200rpm, 220rpm, 250rpm, 280rpm, 300rpm, 320rpm, 350rpm, 370rpm, 390rpm, 400rpm, 450rpm, 460rpm, 480rpm, 500rpm, and in certain embodiments, 350rpm.
In the preparation method as described above, the component B is heated during the stirring dissolution.
In certain embodiments, the temperature is 40-65 deg.C, for example, 40 deg.C, 42 deg.C, 45 deg.C, 47 deg.C, 48 deg.C, 49 deg.C, 50 deg.C, 52 deg.C, 54 deg.C, 56 deg.C, 58 deg.C, 60 deg.C, 62 deg.C, 63 deg.C, 65 deg.C, and in certain preferred embodiments, the heating temperature is 60 deg.C.
In the preparation method, the component B is added into the component A, and the stirring time is 35-70min, such as 35min, 38min, 40min, 45min, 48min, 50min, 52min, 54min, 56min, 58min, 60min, 62min, 64min, 68min, 70min. In certain preferred embodiments, the stirring time is 40min.
In certain embodiments of the invention, the first hyaluronic acid or salt thereof may be hyaluronic acid or any hyaluronate salt as described above, the molecular weight of the first hyaluronic acid or salt thereof being 10-50kDa, e.g. the molecular weight may be 10kDa, 12kDa, 14kDa, 16kDa, 18kDa, 20kDa, 21kDa, 23kDa, 25kDa, 27kDa, 29kDa, 30kDa, 32kDa, 35kDa, 38kDa, 40kDa, 42kDa, 44kDa, 46kDa, 48kDa, 50kDa.
In certain preferred embodiments, the first hyaluronic acid or salt thereof has a molecular weight of 30-50kDa.
In certain embodiments of the invention, the second hyaluronic acid or salt thereof may be hyaluronic acid or any hyaluronate salt as described above, the molecular weight of the second hyaluronic acid or salt thereof being 100-400kDa, e.g. the molecular weight may be 100kDa, 106kDa, 110kDa, 130kDa, 150kDa, 160kDa, 180kDa, 200kDa, 220kDa, 250kDa, 270kDa, 290kDa, 300kDa, 320kDa, 340kDa, 360kDa, 380kDa, 400kDa.
In certain preferred embodiments, the second hyaluronic acid or salt thereof has a molecular weight of 100-150kDa.
In certain specific embodiments of the electronic cigarette liquid provided by the present invention, the first hyaluronic acid or a salt thereof is contained in an amount of 0.002 to 1.0 part by weight, for example, 0.002 part by weight, 0.005 part by weight, 0.008 part by weight, 0.01 part by weight, 0.015 part by weight, 0.02 part by weight, 0.026 part by weight, 0.03 part by weight, 0.04 part by weight, 0.05 part by weight, 0.07 part by weight, 0.09 part by weight, 0.1 part by weight, 0.15 part by weight, 0.2 part by weight, 0.25 part by weight, 0.3 part by weight, 0.4 part by weight, 0.5 part by weight, 0.6 part by weight, 0.7 part by weight, 0.8 part by weight, 0.85 part by weight, 0.88 part by weight, 0.9 part by weight, 0.92 part by weight, 0.94 part by weight, 0.96 part by weight, 0.99 part by weight, 1.99 part by weight, relative to 100 parts by weight of the cigarette liquid.
In certain preferred embodiments, the first hyaluronic acid or salt thereof is present in an amount of 0.005-0.1 parts by weight.
In certain specific embodiments of the electronic cigarette smoke solution provided by the present invention, the second hyaluronic acid or a salt thereof is contained in an amount of 0.001 to 0.1 parts by weight, for example, 0.002 parts by weight, 0.005 parts by weight, 0.008 parts by weight, 0.01 parts by weight, 0.015 parts by weight, 0.02 parts by weight, 0.026 parts by weight, 0.03 parts by weight, 0.035 parts by weight, 0.04 parts by weight, 0.045 parts by weight, 0.05 parts by weight, 0.055 parts by weight, 0.06 parts by weight, 0.065 parts by weight, 0.07 parts by weight, 0.075 parts by weight, 0.08 parts by weight, 0.085 parts by weight, 0.09 parts by weight, 0.095 parts by weight, 0.1 parts by weight, relative to 100 parts by weight of the smoke solution.
In certain preferred embodiments, the second hyaluronic acid or salt thereof is present in an amount of 0.005-0.05 parts by weight.
The first and second hyaluronic acid salts can be any one of salts of hyaluronic acid, including but not limited to sodium hyaluronate, potassium hyaluronate, magnesium hyaluronate, calcium hyaluronate, ammonium hyaluronate, calcium hyaluronate, bismuth hyaluronate, zinc hyaluronate, cobalt hyaluronate, and the like, in certain embodiments, the first and second hyaluronic acid salts are the same hyaluronic acid salt, and in certain embodiments, the first and second hyaluronic acid salts are different kinds of hyaluronic acid salts.
In certain preferred embodiments, the first and second hyaluronic acid salts are selected from the group consisting of hyaluronic acid sodium salt, hyaluronic acid potassium salt, hyaluronic acid magnesium salt, hyaluronic acid calcium salt, hyaluronic acid zinc salt, hyaluronic acid bismuth salt.
The first hyaluronic acid or salt thereof and the second hyaluronic acid or salt thereof may be any grade of hyaluronic acid including, but not limited to, food grade, pharmaceutical grade, cosmetic grade, injection grade, and the like, and in certain preferred embodiments, the first hyaluronic acid or salt thereof and the second hyaluronic acid or salt thereof are pharmaceutical grade hyaluronic acid, and further preferred, the first hyaluronic acid or salt thereof and the second hyaluronic acid or salt thereof are pharmaceutical grade hyaluronic acid prepared by microbial fermentation.
The bacterial species used in the microbial fermentation method include, but are not limited to, streptococcus zooepidemicus, streptococcus equi, streptococcus equisimilis, and the like.
Advantageous effects
1. According to the electronic cigarette liquid provided by the invention, the hyaluronic acid with different molecular weights is compounded, the proportion of the hyaluronic acid with different molecular weights is optimized, and the hyaluronic acid with higher molecular weight is introduced into the electronic cigarette liquid, so that the electronic cigarette liquid has high water retention property, the content of the hyaluronic acid in the smoke is not obviously reduced in the using process, the atomization effect of the hyaluronic acid in the electronic cigarette liquid is improved, and common uncomfortable symptoms such as dry mouth, dry throat, throat itching, pharyngitis and the like caused by electronic cigarettes can be improved.
2. Compared with the electronic cigarette liquid only added with one type of hyaluronic acid, the electronic cigarette liquid containing hyaluronic acid with different molecular weights has an obvious effect of improving the blocking degree of the electronic cigarette filter element, and compared with the electronic cigarette liquid only added with one type of hyaluronic acid, the blocking degree of the electronic cigarette liquid to the filter element reaches about 50, the blocking degree of the electronic cigarette liquid to the filter element is only about 2-6 and at most no more than 16, the filter element is hardly blocked, the common problem that the filter element is blocked by the cigarette liquid containing hyaluronic acid is solved, and the hyaluronic acid with higher molecular weight is introduced into the electronic cigarette liquid, so that the electronic cigarette liquid has high water retention.
Examples
The present invention will be described in detail with reference to examples. It should be understood, however, that the present invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. The numerical ranges recited in the present invention each include data for both endpoints of the numerical range, and also include each of the specific values in the numerical range, and the numerical values can be combined with the endpoints at will to form a new subrange.
The contents of the first hyaluronic acid and the second hyaluronic acid in each of the examples, the comparative examples, and the blank examples are shown in table 1.
TABLE 1 molecular weight and content of hyaluronic acid of each example and comparative example
Example 1
60.9 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
And sequentially adding 0.05 percent of first hyaluronic acid with the molecular weight of 44kDa and 0.01 percent of second hyaluronic acid with the molecular weight of 106kDa into 1.04 percent of deionized water in another clean reaction kettle according to weight percentage, heating to 60 ℃, heating while stirring at the rotating speed of 350rpm, and completely stirring and dissolving to obtain the component B.
And adding the component B into the component A, and stirring at room temperature at the rotation speed of 350rpm for 40min to obtain the electronic cigarette liquid.
Example 2
Adding 60% of glycerol, 35% of propylene glycol and 3% of nicotine into a clean reaction kettle in sequence according to the weight percentage, stirring at room temperature by using a stirrer (coating MICCRA os-25) at the rotating speed of 350rpm, and completely stirring and dissolving to obtain the component A.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 44kDa and 0.05 percent of hyaluronic acid with the molecular weight of 106kDa into 1.9 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 3
In a clean reaction kettle, 59.6 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added according to weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 44kDa and 0.1 percent of hyaluronic acid with the molecular weight of 106kDa into 2.25 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 4
60.9 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by using a stirrer (coating MICCRAS-25) at the rotating speed of 350rpm to obtain the component A after being completely stirred and dissolved.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 44kDa and 0.01 percent of hyaluronic acid with the molecular weight of 150kDa into 1.04 percent of deionized water according to weight percentage in another clean reaction kettle, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 5
60.9 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by using a stirrer (coating MICCRAS-25) at the rotating speed of 350rpm to obtain the component A after being completely stirred and dissolved.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 30kDa and 0.01 percent of hyaluronic acid with the molecular weight of 106kDa into 1.04 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 6
60.9 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 10kDa and 0.01 percent of hyaluronic acid with the molecular weight of 106kDa into 1.04 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 7
60.9 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 44kDa and 0.01 percent of hyaluronic acid with the molecular weight of 400kDa into 1.04 percent of deionized water according to weight percentage in another clean reaction kettle, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 8
61.2 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred by a stirrer (coating MICCRAS-25) at room temperature, the rotating speed is 350rpm, and the A component is obtained after complete stirring and dissolution.
And (3) sequentially adding 0.002 percent of hyaluronic acid with the molecular weight of 44kDa and 0.01 percent of hyaluronic acid with the molecular weight of 106kDa into 0.788 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 9
59.09 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred by a stirrer (coating MICCRAS-25) at room temperature and the rotating speed of 350rpm to obtain the component A after being completely stirred and dissolved.
And (3) sequentially adding 1 percent of hyaluronic acid with the molecular weight of 44kDa and 0.01 percent of hyaluronic acid with the molecular weight of 106kDa into 1.9 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 10
60.95 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by using a stirrer (coating MICCRAS-25) at the rotating speed of 350rpm to obtain the component A after being completely stirred and dissolved.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 44kDa and 0.005 percent of hyaluronic acid with the molecular weight of 106kDa into 0.995 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 11
In a clean reaction kettle, 59.99 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added according to weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
And (3) sequentially adding 0.1 percent of hyaluronic acid with the molecular weight of 44kDa and 0.01 percent of hyaluronic acid with the molecular weight of 106kDa into 1.9 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Example 12
61.19 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred by a stirrer (coating MICCRA os-25) at room temperature and the rotating speed of 350rpm, so as to obtain the component A after complete stirring and dissolution.
And (3) sequentially adding 0.005% of hyaluronic acid with the molecular weight of 44kDa and 0.01% of hyaluronic acid with the molecular weight of 106kDa into 0.795% of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Blank example
And sequentially adding 60.96% of glycerol, 35% of propylene glycol, 3% of nicotine and 1.04% of deionized water in a clean reaction kettle according to the weight percentage, stirring at the rotating speed of 350rpm, and completely stirring and dissolving at room temperature to obtain the blank electronic cigarette liquid.
Comparative example 1
61.01 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
In another clean reaction kettle, adding 0.01 percent of hyaluronic acid with the molecular weight of 106kDa into 0.98 percent of deionized water according to the weight percentage, heating and stirring at 60 ℃, and completely dissolving at the rotating speed of 350rpm to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Comparative example 2
60.9 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 44kDa and 0.01 percent of hyaluronic acid with the molecular weight of 500kDa into 1.04 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Comparative example 3
60.9 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by using a stirrer (coating MICCRAS-25) at the rotating speed of 350rpm to obtain the component A after being completely stirred and dissolved. .
And (3) sequentially adding 0.05 percent of hyaluronic acid with the molecular weight of 70kDa and 0.01 percent of hyaluronic acid with the molecular weight of 106kDa into 1.04 percent of deionized water in another clean reaction kettle according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Comparative example 4
61.03 percent of glycerol, 35 percent of propylene glycol and 3 percent of nicotine are sequentially added into a clean reaction kettle according to the weight percentage, and stirred at room temperature by a stirrer (coating MICCRAS os-25) at the rotating speed of 350rpm to be completely dissolved to obtain the component A.
In another clean reaction kettle, adding 0.005% of hyaluronic acid with the molecular weight of 106kDa into 0.965% of deionized water according to weight percentage, heating and stirring at 60 ℃, wherein the rotating speed is 350rpm, and completely dissolving to obtain the component B.
And adding the component B into the component A, starting stirring at the rotation speed of 350rpm for 40min at room temperature to obtain the electronic cigarette liquid.
Test example 1
The test method comprises the following steps: headspace gas chromatography-mass spectrometry (HS/GC-MS)
4mL of the electronic cigarette liquid prepared in examples 1-12 and comparative examples 1-4 were added to a headspace bottle, and the bottle cap was closed. The headspace vials were placed in a GC-MS liquid injector system autosampler (CTC analytical AG; GC-PAL) sample pan with the extraction conditions set to: keeping the temperature at 80 ℃ for 3min, adsorbing at 80 ℃ for 30min, and rotating the extraction disc at the speed of 250r/min; desorbing the extracted substance at 250 deg.C for 5min.
The GC/MS analysis conditions were:
a chromatographic column: HP-5MS capillary column (30 m.times.0.25 mm.times.0.25 μm); carrier gas: he (purity 99.999%); constant voltage mode: 70kPa; temperature rising procedure: 30 ℃ (1 min), then heating to 260 ℃ (2 min) at 2 ℃/min; and (3) sample introduction mode: no shunt sampling; sample inlet temperature: 250 ℃; transmission line temperature: 280 ℃; an ionization mode: EI; ionization energy: 70eV; the ion source temperature is 220 ℃; quadrupole rod temperature: 160 ℃; scanning mass range: 35-450 amu; solvent retardation: and 2min.
And (3) retrieving the detection data through a Nist and Wiley standard spectrum library, analyzing and comparing the detection data with the standard spectrum time, determining the components in the smoke, and calculating the relative percentage content of the sodium hyaluronate in the smoke by using a peak area normalization method to obtain the content of the sodium hyaluronate in the smoke.
The content of the total amount of hyaluronic acid in the smoke solution and the content of hyaluronic acid in the smoke in each of the examples and comparative examples are shown in table 2.
Table 2 content of hyaluronic acid in tobacco smoke and smoke of each example and comparative example
| Content in tobacco juice (%) | Content in Smoke (%) | Efficiency of atomization (%) | |
| Example 1 | 0.060 | 0.056 | 93.3 |
| Example 2 | 0.100 | 0.092 | 92.0 |
| Example 3 | 0.150 | 0.130 | 86.7 |
| Example 4 | 0.060 | 0.054 | 90.0 |
| Example 5 | 0.060 | 0.055 | 91.7 |
| Example 6 | 0.060 | 0.048 | 80.0 |
| Example 7 | 0.060 | 0.046 | 76.7 |
| Example 8 | 0.012 | 0.009 | 75.0 |
| Example 9 | 1.010 | 0.880 | 87.1 |
| Example 10 | 0.055 | 0.052 | 94.5 |
| Example 11 | 0.110 | 0.102 | 92.7 |
| Example 12 | 0.015 | 0.013 | 86.7 |
| Comparative example 1 | 0.010 | 0.004 | 40.0 |
| Comparative example 2 | 0.060 | 0.023 | 38.3 |
| Comparative example 3 | 0.060 | 0.025 | 41.7 |
| Comparative example 4 | 0.005 | 0.003 | 60.0 |
As can be seen from the table, in each embodiment of the invention, compared with the content of hyaluronic acid in the cigarette liquid, the content of hyaluronic acid in the corresponding smoke is not obviously reduced, the atomization efficiency of the electronic cigarette liquid is higher, the atomization efficiency is over 70%, and can reach as high as 94.5%, which indicates that the cigarette liquid provided by the embodiment of the invention can increase the atomization efficiency of hyaluronic acid, especially hyaluronic acid with higher molecular weight, so that the cigarette liquid and the smoke both contain more hyaluronic acid, thereby having higher water retention, and improving uncomfortable symptoms such as dry mouth, dry throat, throat itching, pharyngitis and the like caused by the electronic cigarette.
The comparative example 1 only contains the second hyaluronic acid, the content of the hyaluronic acid in the smoke is low, and the water retention of the hyaluronic acid on the smoke liquid and the smoke can not be exerted; when the smoke solution contains the first hyaluronic acid and the second hyaluronic acid at the same time, when the molecular weight of the first hyaluronic acid is too large, as shown in comparative example 2, or the molecular weight of the second hyaluronic acid is too large, as shown in comparative example 3, after the smoke solution is gasified, the content of the hyaluronic acid is also greatly reduced relative to the content of the smoke solution, compared with example 1 of the invention, the content of hyaluronic acid in the electronic smoke solution is 0.06%, but the content difference of hyaluronic acid in the smoke is large, the content of hyaluronic acid in the smoke of comparative example 2 is 0.023%, the content of hyaluronic acid in the smoke of comparative example 3 is only 0.025%, and compared with 0.056% in example 1 of the invention, the atomization efficiency is only about 40%, which is far from that of the example of the invention. In the embodiment of the invention, two kinds of hyaluronic acid with different molecular weights are selected, so that the atomization efficiency of the hyaluronic acid in the smoke liquid is higher, the content of the hyaluronic acid in the smoke is increased, and the effect of the hyaluronic acid is favorably exerted.
Test example 2
The test method comprises the following steps:
2mL of the electronic cigarette smoke solution prepared in the examples 1 to 12 and the comparative examples 1 to 4 and the blank example are respectively added into the electronic cigarette, the samples of the electronic cigarette are sucked by a linear type smoking machine according to an ISO suction mode, the electronic cigarette is continuously sucked for 400 times, the blank example is not sucked, then the electronic cigarette of the sucked examples and comparative examples and the electronic cigarette of the non-sucked blank example are placed at a smoking interface of an electronic cigarette resistance testing machine (DELTA instrument), the sample is sucked under the condition of the gas flow rate of 17.5mL/s, and the screen of the electronic cigarette resistance testing machine displays the resistance to smoking. The clogging degree of the filter element of the electronic cigarette is calculated by the following formula. The e-liquid of each example and comparative example blocked the e-cigarette filter element to the extent shown in table 3.
Table 3 clogging degree of filter element of electronic cigarette by electronic cigarette liquid of each example and comparative example
The result shows that the blockage degree of the electronic cigarette filter element is below 16% in the using process of the electronic cigarette liquid provided by the invention, which indicates that the electronic cigarette liquid provided by the invention can be atomized into the total particulate matters of the smoke and further absorbed by a human body. Among them, the examples 1, 2, 4, 5, 9, 10, 11 and 12 are particularly excellent in effect, have high atomization efficiency, and efficiently improve the condition that the filter element is blocked by hyaluronic acid.
The electronic cigarette liquid only added with the second hyaluronic acid with the larger molecular weight is shown in comparative example 1, the blocking degree of the electronic cigarette liquid on the filter element of the electronic cigarette reaches about 51.7%, the use of the electronic cigarette liquid is seriously influenced, and the loss of the electronic cigarette filter element is too large; when the cigarette liquid contains the first hyaluronic acid and the second hyaluronic acid at the same time, when the molecular weight of the first hyaluronic acid is too large, as shown in comparative example 3, or the molecular weight of the second hyaluronic acid is too large, as shown in comparative example 2, the blockage degree of the electronic cigarette filter element is over 49%, so that the molecular weight ranges of the hyaluronic acids with two molecular weights contained in the cigarette liquid of the electronic cigarette provided by the invention are more reasonable, and the cigarette liquid has a remarkable effect of improving the blockage condition of the electronic cigarette filter element.
Claims (12)
1. An electronic cigarette liquid, which is characterized by comprising a first hyaluronic acid or a salt thereof and a second hyaluronic acid or a salt thereof;
the first hyaluronic acid or salt thereof has a molecular weight of 10-50kDa;
the second hyaluronic acid or salt thereof has a molecular weight of 100-400kDa;
the content of the first hyaluronic acid or the salt thereof is 0.002-1.0 part by weight relative to 100 parts by weight of the tobacco juice; the content of the second hyaluronic acid or the salt thereof is 0.001-0.1 weight part.
2. The e-cigarette liquid of claim 1, wherein the first hyaluronic acid or salt thereof has a molecular weight of 30-50kDa;
the second hyaluronic acid or salt thereof has a molecular weight of 100-150kDa.
3. The electronic cigarette liquid of claim 1 or 2, wherein the first hyaluronic acid or a salt thereof is contained in an amount of 0.005-0.1 parts by weight relative to 100 parts by weight of the liquid;
the content of the second hyaluronic acid or the salt thereof is 0.005-0.05 weight part.
4. The e-cigarette smoke solution of claim 1 or 2, wherein the first and second hyaluronic acid salts are sodium, potassium, magnesium, calcium, zinc, or bismuth salts of hyaluronic acid.
5. The e-cigarette liquid of claim 1 or 2, wherein the e-cigarette liquid further comprises glycerin, propylene glycol, water, and/or nicotine.
6. The electronic cigarette liquid of claim 5, wherein the glycerin is present in an amount of 20 to 80 parts by weight per 100 parts by weight of the liquid; the content of the propylene glycol is 5-60 parts by weight; the content of the water is 0.05 to 3 weight portions.
7. A preparation method of electronic cigarette liquid is characterized by comprising the following steps:
mixing glycerol, propylene glycol and/or nicotine, and dissolving to obtain component A;
mixing and dissolving the first hyaluronic acid or salt thereof, the second hyaluronic acid or salt thereof and water uniformly to obtain a component B;
adding the component B into the component A, and uniformly mixing to obtain the electronic cigarette liquid;
the first hyaluronic acid or salt thereof has a molecular weight of 10-50kDa;
the second hyaluronic acid or salt thereof has a molecular weight of 100-400kDa;
the content of the first hyaluronic acid or the salt thereof is 0.002-1.0 part by weight relative to 100 parts by weight of the tobacco juice; the content of the second hyaluronic acid or the salt thereof is 0.001-0.1 weight part.
8. The method of claim 7, wherein the first hyaluronic acid or salt thereof has a molecular weight of 30-50kDa;
the second hyaluronic acid or salt thereof has a molecular weight of 100-150kDa.
9. The method according to claim 7 or 8, wherein the first hyaluronic acid or the salt thereof is contained in an amount of 0.005 to 0.1 parts by weight;
the content of the second hyaluronic acid or the salt thereof is 0.005-0.05 weight part.
10. The method according to claim 7 or 8, wherein the first and second hyaluronic acid salts are sodium, potassium, magnesium, calcium, zinc or bismuth salts of hyaluronic acid.
11. The method according to claim 7 or 8, wherein the dissolving process is assisted with an agitator.
12. The method of claim 11, wherein the agitator speed is 200 to 500rpm.
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