Preparation method of atomized liquid and atomized liquid

Abstract

The invention provides a preparation method of atomized liquid containing a caffeine extract. The preparation method comprises the following steps: grinding coffee, adding water, mixing, and extracting to obtain a first extract; concentrating the first extract, adjusting the pH value to be more than or equal to 10 and less than or equal to 11 by using sodium hydroxide, and extracting by using ethyl acetate to obtain a second extract; evaporating and recovering ethyl acetate to obtain a third extract containing caffeine; taking a certain amount of third extract containing caffeine, and adding a solvent to obtain atomized liquid; the atomized liquid prepared by the preparation method of the atomized liquid containing caffeine provided by the invention is relatively high in caffeine content, and carbon deposition is not easy to cause.

Description

Technical Field

[0001] The embodiments of the present application relate to the field of atomization liquids, and in particular, to a preparation method of an atomization liquid. Background Art

[0002] Caffeine, with the chemical formula C 8 H 10 N 4 O 2 , is a xanthine alkaloid compound. By competing with adenosine receptors for binding, it inhibits the action of adenosine, thereby increasing neuronal activity, temporarily driving away drowsiness, and improving alertness and attention. In addition, caffeine can also promote the release of neurotransmitters such as dopamine, norepinephrine, and epinephrine, further enhancing the excitability of the nervous system. Caffeine exists in many foods and beverages, mainly in coffee, tea, cocoa, and some beverages.

[0003] Atomization inhalation therapy is a method of forming tiny droplets or particles from the required liquid medicine through an atomization device and inhaling them through a special mask or mouthpiece, so that the pharmaceutical preparation is directly delivered to the respiratory tract and alveoli. Therefore, taking caffeine by atomization can more quickly and effectively achieve the effects of caffeine than by drinking.

[0004] Currently, even if a small amount of plant extract is added to the atomization liquids seen on the market, the heating element is prone to carbon deposition during the heating and atomization process, resulting in a burnt taste in the mouthfeel and abnormal atomization. Summary of the Invention

[0005] To solve the problem that the atomization liquid containing plant extract is prone to carbon deposition during the heating and atomization process, an embodiment of the present application provides a preparation method of an atomization liquid containing caffeine extract, including:

[0006] Crush coffee, mix it with water and extract to obtain a first extract;

[0007] Concentrate the first extract, adjust it to 10 ≤ pH ≤ 11 using sodium hydroxide, and extract with ethyl acetate to obtain a second extract;

[0008] Evaporate and recover ethyl acetate to obtain a third extract containing caffeine;

[0009] Take a certain amount of the third extract containing caffeine, add a solvent to obtain an atomization liquid.

[0010] In the preparation method of the atomization liquid containing caffeine extract provided by an embodiment of the present application, in the step of obtaining the first extract, the liquid-solid ratio of water to coffee is 4:1 - 20:1.

[0011] In the preparation method of the atomizing liquid containing caffeine extract provided by an embodiment of the present application, in the step of obtaining the second extract, it further includes concentrating the first extract to the same mass as that of coffee.

[0012] In the preparation method of the atomizing liquid containing caffeine extract provided by an embodiment of the present application, the volume ratio of the first extract to ethyl acetate in the ethyl acetate extraction process is 0.5 - 2, and the number of extraction times is 3 - 10 times.

[0013] In the preparation method of the atomizing liquid containing caffeine extract provided by an embodiment of the present application, the mass content of caffeine in the third extract is 95.0% - 99.7%.

[0014] In the preparation method of the atomizing liquid containing caffeine extract provided by an embodiment of the present application, the solvent is a combination of one or more of propylene glycol, glycerol, and ethanol.

[0015] In the preparation method of the atomizing liquid containing caffeine extract provided by an embodiment of the present application, the atomization efficiency of caffeine in the atomizing liquid is 93.74% - 99.08%.

[0016] An embodiment of the present application further provides an atomizing liquid, which includes a caffeine extract, benzoic acid, and a solvent, wherein the mass content of caffeine in the added caffeine extract is 95.0% - 99.7%.

[0017] In the atomizing liquid provided by an embodiment of the present application, the mass content of caffeine in the atomizing liquid is 0.111 - 11.061%.

[0018] In the atomizing liquid provided by an embodiment of the present application, the mass ratio of benzoic acid to the caffeine extract is 1:1 - 3:1.

[0019] In the atomizing liquid provided by an embodiment of the present application, the atomization efficiency of caffeine in the atomizing liquid is 93.74% - 99.08%. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] One or more embodiments are exemplarily illustrated by the pictures in the corresponding drawings. These exemplary illustrations do not constitute limitations on the embodiments. Elements with the same reference numerals in the drawings are represented as similar elements. Unless otherwise stated, the drawings in the figures do not constitute a proportional limitation.

[0021] Figure 1 Schematic diagram of the carbon deposition situation of Comparative Example 1;

[0022] Figure 2 Schematic diagram of the carbon deposition situation of Comparative Example 2;

[0023] Figure 3 Schematic diagram of carbon deposition in Example 1;

[0024] Figure 4 Chromatogram of the atomizing liquid containing caffeine extract prepared in Example 1 of the present application before atomization;

[0025] Figure 5 Chromatogram of the atomizing liquid containing caffeine extract prepared in Example 1 of the present application after atomization. Detailed implementation manners

[0026] For the convenience of understanding the present application, the present application will be described in more detail below with reference to the accompanying drawings and specific implementation manners.

[0027] Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present application without creative efforts belong to the scope protected by the present application.

[0028] Referring to "embodiments" herein means that the specific features, structures or characteristics described in connection with the embodiments can be included in at least one embodiment of the present application. The phrase appears in various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment mutually exclusive with other embodiments. Those skilled in the art explicitly and implicitly understand that the embodiments described herein can be combined with other embodiments.

[0029] An embodiment of the present application provides a method for preparing an atomizing liquid containing caffeine extract, the method comprising:

[0030] Crush coffee, mix with water and extract to obtain a first extract;

[0031] Concentrate the first extract, adjust to 10 ≤ pH ≤ 11 with sodium hydroxide, extract with ethyl acetate to obtain a second extract; evaporate and recover ethyl acetate to obtain a third extract;

[0032] Take a certain amount of the third extract containing caffeine, add a solvent to obtain an atomizing liquid.

[0033] The atomizing liquid prepared by the method for preparing an atomizing liquid containing caffeine provided by the present application has a high caffeine content and is not likely to cause carbon deposition.

[0034] In some embodiments of the present application, the caffeine extract is derived from coffee, tea, guarana, cacao beans, etc.

[0035] In one embodiment of the present application, the liquid-solid ratio of water to coffee is 4:1 - 10:1, and heating under reflux extraction is adopted. After boiling gently for 0.5 - 2 h, a first extract is obtained. The liquid-solid ratio of water to coffee refers to the mass ratio of water to coffee.

[0036] In one embodiment of the present application, it further includes concentrating the first extract to the same mass as that of the coffee.

[0037] In one embodiment of the present application, during the extraction process with ethyl acetate, the volume ratio of the first extract to ethyl acetate is 0.5 - 2, and the number of extraction times is 3 - 10 times.

[0038] In one embodiment of the present application, it further includes evaporating and recovering ethyl acetate.

[0039] In one embodiment of the present application, the mass content of caffeine in the third extract is 95.0% - 99.7%.

[0040] In one embodiment of the present application, the solvent is a combination of one or more of propylene glycol, glycerol, ethanol, and water. Propylene glycol can be 1,2 - propylene glycol or 1,3 - propylene glycol. Propylene glycol and vegetable glycerol are common components of e - liquid. As carriers of the components, they can also improve the taste.

[0041] In one embodiment of the present application, propylene glycol can be 1,2 - propylene glycol or 1,3 - propylene glycol, with a mass percentage of 20 - 80%, vegetable glycerol with a mass percentage of 30 - 70%, and water with a mass percentage of 10 - 100%.

[0042] E - liquids containing caffeine extracts are prepared by different preparation methods, and the carbon deposition conditions of the e - liquids prepared by different methods are compared.

[0043] Comparative Example 1

[0044] The coffee is moderately crushed and reserved. Using water as the solvent, the solid - liquid ratio of coffee to water is 10:1 for heating under reflux extraction, keeping it boiling gently for 1 h. After filtration, a caffeine extract is obtained. The obtained caffeine extract is tested by HPLC, and the content of caffeine in the caffeine extract is 1.44%.

[0045] Take 7% of the caffeine extract and 50% of vegetable glycerol, and make up the balance with 1,2 - propylene glycol to obtain an e - liquid. The content of caffeine in the e - liquid is 0.101%.

[0046] Take the e - liquid for aspiration test. After all the e - liquid carried in the atomizer is atomized, disassemble the atomizer to take out the heating element, and observe the carbon deposition situation as Figure 1 shown.

[0047] Comparative Example 2

[0048] Moderately crush the coffee and set it aside for later use. Using water as the solvent, perform heating under reflux extraction at a solid-liquid ratio of 10:1, maintain gentle boiling for 1 h, and obtain the extraction solution after filtration.

[0049] Concentrate the extraction solution, add ethanol until the ethanol content reaches 75%, perform ethanol precipitation, filter after standing for 24 h, recover ethanol using a rotary evaporator, and concentrate to obtain a product where 1 g of the extract is equivalent to 9.98 g of coffee, which is set aside as the caffeine extract. The obtained caffeine extract is tested by HPLC, and the caffeine content in the prepared caffeine extract is 6.5%.

[0050] Take 1.5% of the caffeine extract and 50% of vegetable glycerin, and make up the balance with 1,2 - propanediol to obtain the atomizing solution. The caffeine content in the atomizing solution is 0.098%.

[0051] Take the atomizing solution for aspiration test. After all the atomizing solution carried in the atomizer is atomized, disassemble the machine to take out the heating element and observe the carbon deposition situation as Figure 2 shown.

[0052] Example 1

[0053] Moderately crush the coffee and set it aside for later use. Using water as the solvent, perform heating under reflux extraction at a solid-liquid ratio of 10:1, maintain gentle boiling for 1 h, and obtain the first extract after filtration.

[0054] Concentrate the coffee extraction solution to the same mass as the coffee, adjust the pH of the extraction solution to 10 with sodium hydroxide, and perform extraction with an equal volume of ethyl acetate four times continuously. Collect the ethyl acetate layer to obtain the second extract. Recover ethyl acetate using a rotary evaporator to obtain the third extract. The obtained third extract is tested by HPLC, and the caffeine content reaches 98%.

[0055] Take 1% of the third extract and 50% of vegetable glycerin, and make up the balance with 1,2 - propanediol to obtain the atomizing solution. The caffeine content in the atomizing solution is 0.098%.

[0056] Take the atomizing solution for aspiration test. After all the atomizing solution carried in the atomizer is atomized, disassemble the machine to take out the heating element and observe the carbon deposition situation as Figure 3 shown.

[0057] From Comparative Example 1, Comparative Example 2 and Example 1, it can be seen that by using the preparation method of the atomizing solution containing caffeine of the present application, the prepared atomizing solution has a relatively high caffeine content and is not prone to carbon deposition.

[0058] The HPLC test refers to GB 5009.139 - 2014 "National Food Safety Standard Determination of Caffeine in Beverages", establishes a caffeine test method, uses a high performance liquid chromatograph (HPLC) with a diode array detector for analysis, and the HPLC analysis conditions are shown in Table 1.

[0059] Table 1 Chromatographic Conditions for Caffeine Content Determination

[0060]

[0061] In some embodiments of the present application, caffeine extracts are prepared under different experimental conditions. Among them, the caffeine content is shown in Table 2.

[0062] Table 2 Caffeine Content in Caffeine Extracts Prepared in Different Embodiments of the Present Application

[0063]

[0064] Take the atomized liquid containing caffeine extract prepared in Example 1 of the present application. The chromatograms before and after atomization are obtained by HPLC as shown in Figure 4 and Figure 5 shown. Figure 4 and Figure 5 There is no obvious change in the peak shape of the peak spectrum in the chromatograms of

[0065] It can be obtained that after the caffeine extract in the atomized liquid is heated and atomized, the components are relatively stable.

[0066] In one embodiment of the present application, the mass content of caffeine in the atomized liquid is 0.111 - 11.061%. In the atomized liquid of the present application, the caffeine content is relatively high. Under the atomization effect, caffeine can directly reach the respiratory tract and alveoli, enhancing the excitability of the nervous system.

[0067] In one embodiment of the present application, the atomized liquid also contains benzoic acid, and the mass ratio of benzoic acid to caffeine extract is 1:1 - 3:1. When the mass ratio of benzoic acid to caffeine extract is in the range of 1:1 - 3:1, with the increase of the mass ratio of added benzoic acid, the solubility of caffeine in the atomized liquid can be promoted.

[0068] In one embodiment of the present application, the atomized liquid uses glycerol and ethanol as solvents, and the mass ratio of glycerol to ethanol is 1:1. The solubility of caffeine in atomized liquids with different mass ratios of benzoic acid to caffeine extract is investigated, as shown in Table 3, which shows the solubility of caffeine in the atomized liquids in Comparative Example 3 and Examples 4 - 5.

[0069] Table 3 Solubility of Caffeine in Atomized Liquids with Different Mass Ratios of Benzoic Acid to Caffeine Extract

[0070]

[0071] As shown in Table 3, the mass ratio of benzoic acid / caffeine extract in Comparative Example 3 is 0:1, and the solubility of caffeine is 17.500 mg / mL. The mass ratio of benzoic acid / caffeine extract in Example 4 is 1:1, and the solubility of caffeine is 25.815 mg / mL. It can be seen that the addition of benzoic acid can promote the dissolution of caffeine in the atomized liquid. From Example 4 to Example 6, the mass ratio of benzoic acid / caffeine extract increases from 1:1 to 3:1, and the solubility of caffeine increases from 25.815 mg / mL to 110.613 mg / mL. It can be seen that in the range of the mass ratio of benzoic acid / caffeine extract from 1:1 to 3:1, the solubility of caffeine increases.

[0072] In some embodiments of the present application, the caffeine extract prepared in Example 1 was used to prepare atomized liquids with different caffeine contents. The atomized liquid was injected into an electronic atomizer, such as a Cerulean smoking machine, for suction, and captured by a single Cambridge filter. The parameters were a suction volume of 55 mL, a suction frequency of 30 s, a suction duration of 3 s, 50 puffs of Cambridge filter collection, and an initial mobile phase oscillation extraction. The atomization conversion rate of the caffeine extract was tested with caffeine as an indicator.

[0073] The atomization conversion rate is calculated by the formula: A = w1 / w2*100%

[0074] A = atomization conversion rate

[0075] w1=mass percentage of caffeine in aerosol

[0076] w2=mass percentage of caffeine in the electronic atomization liquid

[0077] As shown in Table 4, Examples 7-12 are the atomization conversion rates of caffeine in atomized liquids with different caffeine contents.

[0078] Table 4 Atomization conversion rate of caffeine in atomized liquid with different caffeine contents

[0079]

[0080] It can be seen that the caffeine content in the atomized liquid of the present application is in the range of 0.111-11.061%, and the atomization efficiency of the atomized liquid is 93.74%-99.08%.

[0081] In some embodiments of the present application, the atomized liquid further includes edible flavors, cooling agents, and sweeteners. Edible flavors include, but are not limited to: coffee flavor essence, tea flavor essence, cocoa flavor essence, fruit flavor essence, plant flavor essence, and other food flavor essences. Cooling agents include, but are not limited to: N,2,3-trimethyl-2-isopropylbutyramide, menthamide, N-(ethoxycarbonylmethyl)-p-menthane-3-carboxamide, N-(4-methoxyphenyl)-p-menthane-3-carboxamide, menthol, menthol derivatives, menthone derivatives, menthyl ether derivatives, and menthyl ester derivatives. Sweeteners include, but are not limited to: sodium cyclamate, xylitol, mogroside, acesulfame potassium, sodium saccharin, sucralose, aspartame, alitame, neohesperidin dihydrochalcone, neotame, and stevioside.

[0082] In some embodiments of the present application, the addition amount of the edible flavor is 0.01-10%. The addition amount of the cooling agent is 0.01-10%. The addition amount of the sweetener is 0.01-10%.

[0083] In some embodiments of the present application, the addition amount of the edible flavor is 5%. The addition amount of the cooling agent is 2%. The addition amount of the sweetener is 1%.

[0084] It should be noted that the description and drawings of the present application provide preferred embodiments of the present application, but are not limited to the embodiments described in this specification. Further, for those of ordinary skill in the art, improvements or changes can be made based on the above description, and all such improvements and changes should fall within the protection scope of the appended claims of the present application.

Claims

1. A preparation method of an atomizing liquid containing caffeine extract, characterized in that it includes: crushing coffee, mixing with water and extracting to obtain a first extract; concentrating the first extract, adjusting to 10 ≤ pH ≤ 11 with sodium hydroxide, and extracting with ethyl acetate to obtain a second extract; evaporating and recovering the ethyl acetate to obtain a third extract containing caffeine; taking a certain amount of the third extract containing caffeine and adding a solvent to obtain the atomizing liquid.

2. The preparation method of the atomizing liquid containing caffeine extract according to claim 1, characterized in that, in the step of obtaining the first extract, the liquid-solid ratio of the water to the coffee is 4:1 - 20:

1.

3. The preparation method of the atomizing liquid containing caffeine extract according to claim 1, characterized in that, in the step of obtaining the second extract, it further includes concentrating the first extract to the same mass as the coffee.

4. The preparation method of the atomizing liquid containing caffeine extract according to claim 1, characterized in that, the volume ratio of the first extract to the ethyl acetate in the ethyl acetate extraction process is 0.5 - 2, and the extraction times are 3 - 10 times.

5. The preparation method of the atomizing liquid containing caffeine extract according to claim 1, characterized in that, the mass content of caffeine in the third extract is 95.0% - 99.7%.

6. The preparation method of the atomizing liquid containing caffeine extract according to claim 1, characterized in that, the solvent is a combination of one or more of propylene glycol, glycerol and ethanol.

7. The preparation method of the atomizing liquid containing caffeine extract according to claim 1, characterized in that, the atomization efficiency of caffeine in the atomizing liquid is 93.74% - 99.08%.

8. An atomizing liquid, characterized in that, the atomizing liquid includes caffeine extract, benzoic acid and a solvent, wherein the mass content of caffeine in the added caffeine extract is 95.0% - 99.7%.

9. The atomizing liquid according to claim 8, characterized in that, the mass content of caffeine in the atomizing liquid is 0.111 - 11.061%.

10. The atomizing liquid according to claim 8, characterized in that, the mass ratio of the benzoic acid to the caffeine extract is 1:1 - 3:

1.

11. The atomizing liquid according to claim 8, characterized in that, the atomization efficiency of caffeine in the atomizing liquid is 93.74% - 99.08%.

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