Method for rapid screening of solid substances suitable for use in electronic aerosol devices and uses thereof

Abstract

The application discloses a method for rapidly screening solid substances suitable for electronic atomization devices and application thereof. The method comprises the following steps: subjecting a to-be-tested solid sample to temperature rising treatment in a first preset temperature range, observing the morphological changes of the to-be-tested solid sample during the temperature rising treatment, including whether the to-be-tested solid sample is liquefied, whether the color is stable, whether the to-be-tested solid sample is gasified, whether the solid sample is expanded, whether the to-be-tested solid sample is carbonized or whether black substances are generated; subjecting the to-be-tested solid sample to atomization treatment in a second preset temperature range, analyzing the component changes of the to-be-tested solid sample before and after atomization by using a high-resolution mass spectrometer; and judging whether the to-be-tested solid sample is suitable for the electronic atomization device based on the morphological changes and the component changes of the to-be-tested solid sample. By using the method, additive components or atomization liquid combinations with good thermal stability and atomization effect can be rapidly screened, and the use demand and customer experience of the electronic atomization device can be better met.

Description

Technical Field

[0001] This invention belongs to the field of atomized products, and more specifically, relates to a method for rapidly screening solid substances suitable for electronic atomization devices and its uses. Background Technology

[0002] There are many types of electronic atomization products, including medical nebulizers such as asthma treatment devices and e-cigarettes. These products achieve therapeutic effects or provide a pleasurable sensation by atomizing raw materials. To meet the diverse needs of users regarding inhalation sensation and taste, sweeteners and other additives are typically added to the atomizing raw materials. However, there are many types of raw materials and additives that can be used in electronic atomization products. Due to the inherent properties of these materials and additives, different types produce different atomization effects. For example, with sweeteners, the intensity, duration, and irritation level after atomization vary depending on the type of additive. Only by adding suitable types or combinations of sweeteners can a good inhalation or puffing sensation be achieved; otherwise, undesirable results may occur, such as weak sweetness, unsatisfactory sweetness release, easy carbon buildup, burning sensation, or burnt taste. Therefore, selecting suitable raw materials or additives for electronic atomization products is crucial for meeting the usage needs and enhancing customer experience. Summary of the Invention

[0003] This invention aims to at least partially solve one of the technical problems in related technologies. Therefore, one objective of this invention is to provide a method for rapidly screening solid substances suitable for electronic atomization devices and its applications. This method can rapidly screen additive components or atomizing liquid combinations with good thermal stability and atomization effect, better meeting the usage requirements and customer experience of electronic atomization devices.

[0004] In one aspect of the invention, a method for rapidly screening solid materials suitable for electronic atomization devices is provided. According to an embodiment of the invention, the method includes:

[0005] (1) The solid sample to be tested is heated within the first preset temperature range, and the morphological changes of the solid sample to be tested are observed during the heating process. The morphological changes include whether the solid sample to be tested is liquefied, the color depth and color stability, whether it is vaporized, whether there is solid expansion, whether it is carbonized or whether black substances are generated.

[0006] (2) The solid sample to be tested is atomized within a second preset temperature range, and the compositional changes of the solid sample to be tested before and after atomization are analyzed by a high-resolution mass spectrometer.

[0007] (3) Based on the morphological and compositional changes of the solid sample to be tested, determine whether the solid sample to be tested is suitable for an electronic atomization device.

[0008] Wherein, the first preset temperature range does not exceed the extreme temperature threshold that the electronic atomizing device can withstand, and the second preset temperature range does not exceed the operating temperature threshold of the electronic atomizing device.

[0009] According to the above embodiments of the present invention, the method for rapidly screening solid substances suitable for electronic atomization devices can first perform a heating treatment to preliminarily determine the thermal stability of the solid sample based on the color change and expansion rate of the sample. If the stability is low, it can be directly excluded without further atomization treatment. If the stability is relatively good, atomization treatment can be selected based on other characteristics of the solid substance, such as whether it is liquefied and the degree of liquefaction, whether it is vaporized and the degree of vaporization, whether it is carbonized and the degree of carbonization, etc., wherein the higher the degree of liquefaction, the lower the degree of vaporization, and the lower the degree of carbonization, the more suitable it is for use in the atomization device. The atomization treatment is used to further determine whether the composition of the sample changes before and after atomization within the operating temperature range of the electronic atomization device. If the composition of the solid sample before and after atomization remains basically unchanged, it is suitable for use in the electronic atomization device. If the composition changes significantly before and after atomization, such as significant decomposition, it is not suitable for use in the electronic atomization device. This not only allows for the rapid screening of suitable raw materials or additives for electronic atomizing fluids, thus better meeting the usage needs and customer experience of electronic atomizing devices, but also avoids unpleasant experiences such as affecting the normal use of electronic atomizing devices, weak or poor-lasting atomized odor leading to failure to achieve the expected effect, easy carbon buildup, and the generation of burning sensations or pungent odors. At the same time, it also allows for the comparison of various atomizing fluid raw materials or additives to select a superior atomizing fluid composition.

[0010] In addition, the method for rapidly screening solid substances suitable for electronic atomization devices according to the above embodiments of the present invention may also have the following additional technical features:

[0011] In some embodiments of the present invention, the liquefaction temperature of the solid sample to be tested in step (1) is recorded, and the second preset temperature range is determined based on the liquefaction temperature and the operating temperature threshold of the electronic atomizing device.

[0012] In some embodiments of the present invention, the solid sample to be tested is placed in a capillary tube for the heating treatment, wherein the height of the solid sample to be tested in the capillary tube accounts for 2-5% of the height of the capillary tube; and / or, the compaction density of the solid sample to be tested in the capillary tube is 0.0003-0.0006 g / mm². 3 .

[0013] In some embodiments of the present invention, the method for rapidly screening solid substances suitable for electronic atomization devices satisfies at least one of the following conditions: during the heating process, the morphological changes of the solid sample to be tested are observed by video recording and / or photography, and the temperatures corresponding to different morphological change stages are recorded; the heating rate of the heating process is 1℃~10℃ / min; the particle size of the solid sample to be tested is not greater than 0.2mm; the first preset temperature range is 30~300℃; and the solid sample to be tested is heated using an MP-80 melting point apparatus.

[0014] In some embodiments of the present invention, the solid sample to be tested is mixed with propylene glycol and glycerol to obtain an atomized liquid, and the mixture of propylene glycol and glycerol is used as a control liquid. The components of the atomized liquid and the control liquid before and after atomization are analyzed using a quadrupole-time-of-flight LC-MS / MS.

[0015] In some embodiments of the present invention, the atomizing liquid and the control liquid are diluted with ethanol before the atomization treatment, and the components of the atomizing liquid and the control liquid before atomization are analyzed; and / or, during the atomization treatment, a filter is used to collect the atomizing liquid flue gas and the control liquid flue gas, and the filter after absorbing the flue gas is extracted and filtered with ethanol, and the components of the atomizing liquid and the control liquid after atomization are analyzed.

[0016] In some embodiments of the present invention, the filter after absorbing flue gas is a filter after absorbing flue gas 100 to 200 times.

[0017] In some embodiments of the present invention, in step (3), based on the morphological and compositional changes of the solid sample to be tested, and in conjunction with the heat resistance rating evaluation standard, it is determined whether the solid sample to be tested is suitable for the electronic atomization device. The heat resistance rating evaluation standard is based on the morphological changes of the solid sample to be tested after heating treatment, as follows: Level 1: No color change before and after heating treatment, and the volume expansion after heating treatment is not greater than 30%; Level 3: The color changes to black after heating treatment, or the volume expansion after heating treatment is not less than 100%; Level 2: The change is between Level 1 and Level 3; wherein, when the heat resistance rating of the solid sample to be tested is Level 1 or Level 2, it is suitable for use in the electronic atomization device.

[0018] In some embodiments of the present invention, step (3) further includes: comparing the thermal stability of various solid samples to be tested based on the morphological and compositional changes of various solid samples to be tested, and determining the solid sample to be tested most suitable for use in the electronic atomization device.

[0019] In some embodiments of the present invention, the solid sample to be tested is an atomizing liquid additive of the electronic atomizing device, and the atomizing liquid additive includes a sweetener.

[0020] In another aspect, the present invention proposes the application of the above-described method for rapidly screening solid substances suitable for electronic atomization devices in screening atomizing liquid raw materials for electronic atomization devices or comparing the thermal stability of atomizing liquid raw materials for electronic atomization devices. This better meets the usage requirements of electronic atomization devices and customer needs, avoiding unpleasant experiences such as atomizing liquid components affecting the normal use of electronic atomization devices, weak or poor-lasting atomized aroma leading to difficulty in achieving the expected effect, easy carbon buildup, and the generation of burning sensations or pungent odors.

[0021] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description

[0022] The above and / or additional aspects and advantages of the present invention will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which:

[0023] Figure 1 This is a flowchart of a method for rapidly screening solid substances suitable for electronic atomization devices according to an embodiment of the present invention.

[0024] Figure 2 The graph shows the state changes of sucralose in an MP-80 melting point apparatus as the temperature increases, and the final state after the heating treatment, according to Example 1 of the present invention.

[0025] Figure 3 The graph shows the state changes of neotame in an MP-80 melting point apparatus as the temperature increases according to Embodiment 1 of the present invention, and the final state after the heating process is completed.

[0026] Figure 4 The graph shows the state changes of NHDC in an MP-80 melting point apparatus as the temperature increases according to Embodiment 1 of the present invention, and the final state after the heating process is completed. Detailed Implementation

[0027] Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention.

[0028] The inventors discovered that solid substances exhibit different behaviors as the heating temperature increases, and the heat resistance of a substance can be judged based on these different behaviors, thereby inferring whether it is suitable for electronic heating atomization.

[0029] Therefore, in one aspect of this invention, a method for rapidly screening solid substances suitable for electronic atomization devices is proposed. This method involves detecting the bulk thermal stability and related morphological changes of the solid substance, and combining this with high-resolution mass spectrometry to detect the compositional changes of the solid substance before and after atomization in an atomizing liquid, verifying its thermal stability. This verifies the atomization stability of the solid substance or compares the atomization stability of multiple different solid substances, thereby quickly identifying solid substances suitable for electronic atomization devices. This allows for the rapid screening of additive components or atomizing liquid combinations with good thermal stability and atomization effect, better meeting the usage requirements and customer experience of electronic atomization devices. It should be noted that the "solid substances suitable for electronic atomization devices" mentioned in this invention refer to solid substances that can meet both the usage requirements of electronic atomization devices and the user's inhalation experience. These solid substances can be either raw materials for atomizing liquids or additive components of atomizing liquids. The following references... Figure 1 The method for rapidly screening solid substances suitable for electronic atomization devices is described in detail according to embodiments of the present invention, the method comprising:

[0030] S100: The solid sample to be tested is heated within a first preset temperature range. The morphological changes of the solid sample to be tested during the heating process are observed. The morphological changes include whether the solid sample to be tested liquefies, changes in color intensity and color stability, whether it vaporizes, whether there is solid expansion, whether it carbonizes, or whether black substances are generated. The first preset temperature range does not exceed the extreme temperature threshold that the electronic atomization device can withstand.

[0031] According to embodiments of the present invention, by heating the solid sample to be tested within the extreme temperature threshold range that the electronic atomization device can withstand, the thermal stability of the solid sample can be preliminarily judged based on the color change and expansion rate of the sample. If the stability is low, it indicates that the solid sample is not suitable for the electronic atomization device and can be directly excluded without further atomization. If the stability is relatively good, further atomization can be selected based on other characteristics of the solid material, such as whether it is liquefied and the degree of liquefaction, whether it is vaporized and the degree of vaporization, whether it is carbonized and the degree of carbonization, etc. Specifically, if the color change of the solid sample during the heating process is significant (e.g., from colorless to black or close to black), its thermal stability can be preliminarily judged to be poor. If it undergoes significant volume expansion during the heating process, and the volume expansion rate exceeds a preset threshold (e.g., 100%), its thermal stability can also be preliminarily judged to be poor. If the color change during the heating process is not significant (e.g., remaining colorless or slightly discolored) and its volume expansion rate is not greater than the preset threshold, its thermal stability can be preliminarily judged to be relatively good. In addition, if the solid sample to be tested can be liquefied during the heating process, it is more conducive to meeting the basic requirements of the atomizing liquid. The higher the degree of liquefaction, the more beneficial it is for the use of electronic atomization devices. If the solid sample to be tested vaporizes or carbonizes during the heating process, it is not conducive to the use of electronic atomization devices. The lower the degree of vaporization or carbonization, the more beneficial it is for the use of electronic atomization devices.

[0032] According to embodiments of the present invention, it should be noted that the first preset temperature range is not particularly limited. Those skilled in the art can select it based on actual needs such as the specific type of electronic atomizing device, the highest and lowest temperatures it can withstand, the application scenario, and the commonly used operating temperature range. For example, taking an electronic cigarette or medical atomizer as an example, the first preset temperature range can be 0℃ to 300℃, preferably 30℃ to 300℃. That is, the temperature can be continuously increased from room temperature or room temperature until it reaches 300℃. The atomization temperature of an electronic cigarette or medical atomizer is usually not greater than 300℃. Determining the first preset temperature range to the above range can narrow the temperature range based on selecting solid samples suitable for use in electronic cigarettes or medical atomizers, thereby accelerating the screening rate and reducing the screening workload.

[0033] According to an embodiment of the present invention, the solid sample to be tested can be placed in a capillary tube for heating. The height percentage of the solid sample in the capillary tube can be 2% to 5% of the capillary height, for example, 2.5%, 3%, 3.5%, 4%, or 4.5% of the capillary height. The inventors have found that the solid sample may melt and expand or vaporize during the heating process. If its height percentage in the capillary tube is too large, the risk of melting, expanding, or vaporizing during the heating process, leading to overflow, is also greater. In this invention, by controlling the height percentage of the solid sample in the capillary tube to the above-mentioned range, it is not only convenient to observe its morphological changes before and after heating, but also significantly reduces its overflow risk. Furthermore, the compaction density of the solid sample in the capillary tube can be 0.0003 to 0.0006 g / mm³. 3 For example, it can be 0.0004 g / mm 3 or 0.0005g / mm 3 This allows for a more pronounced change in the morphology of the solid sample before and after heating. It should be noted that when comparing the atomization stability of multiple different solid samples, the compaction density of each sample in the capillary should be kept consistent. This can be achieved by controlling the mass of the solid sample and its proportion of height in the capillary, thus avoiding the problem of decreased accuracy of test results due to different compaction densities.

[0034] According to an embodiment of the present invention, when the solid sample to be tested is placed in a capillary tube for heating treatment, the solid sample to be tested can be pre-dried to keep the sample dry. This avoids the problem of large errors or significant decrease in accuracy of the test results due to sample moisture or high moisture content. If the solid sample to be tested is damp, it can be placed in a desiccator to dry for 6-8 hours until there is no weight loss.

[0035] According to an embodiment of the present invention, when the solid sample to be tested is placed in a capillary tube for heating treatment, the particle size of the solid sample to be tested can be no greater than 0.2 mm, for example, 100-150 μm. This facilitates the smooth entry of the sample powder into the capillary tube and helps control the compaction density. If the sample is a coarse-grained material or granular, it can be placed in a grinding chamber and ground until the particle size meets the requirements.

[0036] According to an embodiment of the present invention, when placing the solid sample to be tested in a capillary for heating treatment, the solid sample powder to be tested can be carried on a glass slide, the open end of the capillary is pressed into the sample powder, then the capillary is flipped over, and then the bottom of the capillary is tapped on the hard surface to move the sample powder to the bottom of the capillary (if the sample powder is not moved to the bottom of the capillary, the bottom of the capillary can be moved along the ridged part of the tweezers, or the provided packing wire can be used to pack it downwards with minimal force); then the sample powder is tapped several times on the hard surface at the bottom of the capillary to compact it; after compaction, the height ratio of the sample powder in the capillary is checked with a ruler to see if it reaches the preset ratio. If it is less than the preset ratio, the above operation is repeated.

[0037] According to embodiments of the present invention, a melting point apparatus can be used to heat the solid sample under test, preferably an MP-80 melting point apparatus (i.e., a METTLER TOLEDO series melting point apparatus). This allows for the observation of morphological changes in the solid sample by placing it in a capillary tube and heating it. Preferably, during the heating process, the morphological changes of the solid sample can be observed by video recording and / or photography, and the temperatures corresponding to different stages of morphological change can be recorded. This provides a more intuitive and accurate understanding of the morphological changes and bulk thermal stability of the solid sample. Preferably, the heating rate can be 1℃ to 10℃ / min, such as 3℃ / min, 5℃ / min, or 8℃ / min, etc. This avoids problems such as difficulty in capturing morphological changes or inaccurate observation results due to excessively rapid heating rates, ensuring the accuracy and reliability of the detection results.

[0038] According to an embodiment of the present invention, the solid sample to be tested can be an atomizing liquid additive for an electronic atomizing device. It is understood that the types of atomizing liquid additives in the present invention are not particularly limited, and those skilled in the art can flexibly select according to actual needs. For example, the atomizing liquid additives may include, but are not limited to, sweeteners, thereby allowing for better selection of sweetener types that are suitable for electronic atomizing devices and can achieve the expected sweetness requirements, have good sweetness persistence, are not prone to carbon buildup, do not produce a burning sensation, and do not produce unpleasant odors such as burnt taste.

[0039] S200: The solid sample to be tested is nebulized within a second preset temperature range, and the compositional changes of the solid sample before and after nebulization are analyzed using a high-resolution mass spectrometer. The second preset temperature range does not exceed the operating temperature threshold of the electronic nebulizer.

[0040] According to embodiments of the present invention, given that the solid sample to be tested may undergo chemical changes that are not observable to the naked eye during the heating process, nebulization can be used to further verify whether the solid sample screened after heating is truly suitable for an electronic nebulization device. Specifically, nebulization can be used to further determine whether the composition of the sample changes before and after nebulization within the operating temperature range of the electronic nebulization device. This can be determined by comparing spectra. If the composition of the solid sample remains essentially unchanged before and after nebulization, it indicates that it is suitable for use in an electronic nebulization device. If the composition changes significantly before and after nebulization, such as significant decomposition, it indicates that it is not suitable for use in an electronic nebulization device.

[0041] According to an embodiment of the present invention, a second preset temperature range can be determined based on the liquefaction temperature of the solid sample to be tested recorded during the heating process and the operating temperature threshold of the electronic atomization device. This allows for a better identification of the atomization temperature range of the solid sample to be tested when used in the electronic atomization device, thereby accelerating the screening rate and reducing the screening workload while meeting the atomization processing detection requirements.

[0042] According to embodiments of the present invention, when preparing an atomizing solution using a solid sample to be tested for atomization, the combination of atomizing solutions, including solvents, is not particularly limited. Those skilled in the art can choose according to actual needs. For example, the solid sample to be tested can be mixed with propylene glycol and glycerol to obtain a flavorless atomizing solution without added fragrances or flavorings. The mixture of propylene glycol and glycerol can be used as a control solution. The components of the atomizing solution and the control solution before and after atomization can be analyzed using a quadrupole-time-of-flight LC-MS / MS. This is convenient to operate and allows for better comparison of the component changes of the sample before and after atomization, avoiding interference from other additives that may affect the detection results.

[0043] According to embodiments of the present invention, before nebulization, the nebulizing liquid and the control liquid can be diluted with ethanol to a fixed volume, and the components of the nebulizing liquid and the control liquid before nebulization can be analyzed. This volume dilution further ensures the consistency between the nebulizing liquid with the added solid sample and the control liquid without the added solid sample. Furthermore, during the nebulization process, a filter can be used to collect the nebulizing liquid flue gas and the control liquid flue gas. Ethanol is then used to extract and filter the filter after absorbing the flue gas, and the components of the nebulized nebulizing liquid and the control liquid are analyzed. To avoid insufficient flue gas absorption by the filter, making it difficult to effectively extract enough flue gas components, the filter can absorb flue gas 100-200 times before extraction and filtration. This ensures that the extracted sample meets the detection limit requirements.

[0044] S300: Based on the morphological and compositional changes of the solid sample to be tested, determine whether the solid sample is suitable for an electronic atomization device.

[0045] According to embodiments of the present invention, the suitability of a solid sample for an electronic atomization device can be determined based on the morphological changes of the solid sample during the heating process and the changes in composition before and after atomization, combined with a heat resistance rating evaluation standard. The heat resistance rating evaluation standard can be based on the morphological changes of the solid sample after heating, as specifically as follows:

[0046] Level 1: No color change or slight color change before and after heating treatment, and volume expansion of no more than 30% after heating treatment (if this condition is met, it can be preliminarily judged that the solid sample to be tested has high thermal stability, and further atomization treatment can be carried out to study the changes in composition before and after atomization for verification).

[0047] Level 3: The color changes to black or close to black after heating, or the volume expansion rate is not less than 100% after heating (if either of these two conditions is met, it can be initially judged that the material has low thermal stability and is not suitable for use in electronic atomization devices. No further atomization treatment is required unless there is a special reason).

[0048] Level 2: Changes within Level 1 and Level 2 (within this range, it can be preliminarily judged that the thermal stability of the solid sample to be tested is generally good. Further atomization studies can be decided based on other properties of the substance, such as whether it is liquefied and the degree of liquefaction, whether it is vaporized and the degree of vaporization, whether it is carbonized and the degree of carbonization, etc.).

[0049] The lower the heat resistance rating of the solid sample being tested, the more suitable it is for use in an electronic atomization device; a heat resistance rating of level one or two makes the solid sample suitable for use in an electronic atomization device. According to a specific example of the present invention, it is preferred to use "no color change before and after heating treatment and volume expansion of no more than 30% after heating treatment" as the evaluation criterion for level one; alternatively, "color change to black after heating treatment, or volume expansion rate of no less than 100% after heating treatment" can also be used as the evaluation criterion for level three.

[0050] According to embodiments of the present invention, the thermal stability of various solid samples to be tested can be compared based on the morphological and compositional changes of various solid samples to be tested, and the most suitable solid sample to be tested (such as atomizing liquid raw materials or additive components) for use in electronic atomization devices can be determined. This allows for optimization of the atomizing liquid composition of electronic atomization devices to obtain a better customer experience.

[0051] In summary, the method for rapidly screening solid substances suitable for electronic atomization devices according to the above embodiments of the present invention can first perform a heating treatment to preliminarily determine the thermal stability of the solid sample based on the color change and expansion rate of the sample. If the stability is low, it can be directly excluded without further atomization treatment. If the stability is relatively good, atomization treatment can be selected based on other characteristics of the solid substance, such as whether it is liquefied and the degree of liquefaction, whether it is vaporized and the degree of vaporization, whether it is carbonized and the degree of carbonization, etc. Among these, the higher the degree of liquefaction, the lower the degree of vaporization, and the lower the degree of carbonization, the more suitable it is for use in the atomization device. The atomization treatment is used to further determine whether the composition of the sample changes before and after atomization within the operating temperature range of the electronic atomization device. If the composition of the solid sample before and after atomization remains basically unchanged, it is suitable for use in the electronic atomization device. If the composition changes significantly before and after atomization, such as significant decomposition, it is not suitable for use in the electronic atomization device. This not only allows for the rapid screening of suitable raw materials or additives for electronic atomizing fluids, thus better meeting the usage needs and customer experience of electronic atomizing devices, but also avoids unpleasant experiences such as affecting the normal use of electronic atomizing devices, weak or poor-lasting atomized odor leading to failure to achieve the expected effect, easy carbon buildup, and the generation of burning sensations or pungent odors. At the same time, it also allows for the comparison of various atomizing fluid raw materials or additives to select a superior atomizing fluid composition.

[0052] In another aspect, this invention proposes the application of the above-described method for rapidly screening solid substances suitable for electronic atomization devices in screening atomizing liquid raw materials for electronic atomization devices or comparing the thermal stability of atomizing liquid raw materials for electronic atomization devices. This better meets the usage requirements and customer needs of electronic atomization devices, avoiding unpleasant experiences such as atomizing liquid components affecting the normal use of electronic atomization devices, weak or poor-lasting atomized aroma leading to failure to achieve the desired effect, easy carbon buildup, and the generation of burning sensations or pungent odors. It should be noted that the features and effects described in the above-described method for rapidly screening solid substances suitable for electronic atomization devices also apply to this application, and will not be repeated here.

[0053] The embodiments of the present invention are described in detail below. These embodiments are exemplary and are only used to explain the present invention, and should not be construed as limiting the invention. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in the art or according to the product instructions. Reagents or instruments used, unless otherwise specified, are all commercially available conventional products.

[0054] Example 1

[0055] Sweeteners suitable for use in closed-system e-cigarettes are selected from sucralose (approximately 600 times sweeter than sucrose), neotame (approximately 8000 times sweeter than sucrose), and neohesperidin dihydrochalcone (NHDC, approximately 1500 times sweeter than sucrose).

[0056] (1) The solid samples to be tested were heated in the range of 30 to 300℃ using an MP-80 melting point apparatus, and the morphological changes of sucralose, neotame, and NHDC were observed during the heating process:

[0057] Common methods include:

[0058] 1) Preparation of dried sweetener fine powder:

[0059] The sweetener sample was dried until no weight loss occurred, and the sweetener was ground into a fine powder of about 100 mesh (no larger than 0.2 mm).

[0060] 2) Filled with melting point capillary tubes (100mm in length)

[0061] a. Place the dry, finely powdered sweetener onto a glass slide;

[0062] b. Press the open end of the capillary into the sweetener powder;

[0063] c. Flip the melting capillary over and tap the bottom of the melting capillary on the hard surface to move the sweetener powder to the bottom of the melting capillary. If the sweetener powder does not move to the bottom of the capillary, move the bottom of the capillary along the ribbed part of the tweezers, or use the provided packing wire to pack it downwards with minimal force.

[0064] d. Tap the hard surface at the bottom of the melting capillary multiple times to compact the sweet powder;

[0065] f. Use a ruler to check that the height of the sample inside the capillary is 3mm. If it is less than 3mm, repeat the above steps.

[0066] Among them, the compaction density in the capillaries of different sweeteners is kept consistent.

[0067] 3) Temperature setting:

[0068] Based on the existing atomization temperature and possible fluctuation range of electronic cigarettes, the test temperature of the melting point apparatus was set to increase from 30℃ to 300℃.

[0069] 4) During the heating process, the morphological changes of different sweeteners were recorded on video and photographed to preliminarily determine the thermal stability of the three sweeteners. The test results are shown in [the table below]. Figures 2-4 ,in, Figure 2 The graph shows the state changes of sucralose in an MP-80 melting point apparatus as the temperature increases, and its final state after the heating treatment. Figure 3 The graph shows the state changes of neotame as temperature increases in an MP-80 melting point apparatus, and its final state after the heating treatment. Figure 4 The graph shows the state changes of NHDC in an MP-80 melting point apparatus as temperature increases and its final state after the heating process. Figures 2-4 The state changes shown in the multiple subgraphs are arranged in order of increasing temperature, combined with... Figures 2-4 The specific test results are as follows:

[0070] Sucralose: In the MP-80 melting point apparatus test, it was shown that sucralose began to turn yellow at around 121℃ (due to local cracking), and the melting point was around 124.51℃. After melting, it underwent violent expansion and carbonization, turning black.

[0071] Neotame: The MP-80 melting point apparatus test showed that neotame has a melting point of 86.76℃, and after melting, it is a transparent liquid (with a small amount of cracking).

[0072] NHDC: The MP-80 melting point apparatus showed that the melting point of NHDC is 149.06℃. After melting, the liquid is yellow and shows signs of vaporization.

[0073] The above tests and observations show that among these three sweeteners, sucralose exhibits the most severe carbonization and expands during carbonization, completely carbonizing before reaching the average atomization temperature of 250°C in a closed-loop e-cigarette. Therefore, it is speculated that sucralose has poor thermal stability, and this characteristic suggests that excessive use of sucralose may increase the likelihood of a more pronounced burnt taste during vaping.

[0074] Neotame has the lowest melting point among the three sweeteners, but it showed virtually no decomposition in the initial stage of the heating process. Only at near the average atomization temperature of 250°C in a closed-loop e-cigarette did it undergo slight decomposition and discoloration, exhibiting vaporization and leaving a liquid residue, but no carbonization was observed. Therefore, it is preliminarily judged that neotame has good thermal stability and is a suitable sweetener for e-cigarette products.

[0075] NHDC exhibits moderate thermal stability. Although it underwent significant discoloration during heating, no obvious carbonization was observed. Therefore, from a thermal stability perspective, NHDC is superior to sucralose but inferior to neotame, placing it in the middle range.

[0076] (2) The changes of the above three sweeteners before and after atomization in e-liquid were analyzed by high resolution mass spectrometry to verify the heat resistance of the above sweeteners.

[0077] Common methods include:

[0078] 1) Using propylene glycol and glycerin at a volume ratio of 1:1 as a solvent, three sweeteners were formulated into flavorless e-liquids without added flavorings or fragrances. A solvent with a propylene glycol and glycerin volume ratio of 1:1 was used as a control. Q-TOF (quadrupole-time-of-flight liquid chromatography-mass spectrometry) was used to analyze the e-liquid components and the vapor components after atomization of the flavorless e-liquids formulated with the three sweeteners. This study aimed to understand the changes in the components of the three sweeteners before and after atomization and to conduct a more thorough investigation into the applicability of the three sweeteners in closed-system electronic cigarettes.

[0079] 2) Sample preparation:

[0080] E-liquid / control sample: Weigh 1.0g, dilute to 10ml with ethanol, and shake well.

[0081] Flue gas sample: Collect using a Cambridge filter, take 100-200 puffs, extract with 10 ml of ethanol solution, shake at 200 rpm for 20 min, and then filter.

[0082] 3) Sample preparation:

[0083] The components of the e-liquid before and after atomization were tested using Q-TOF (quadrupole-time-of-flight LC-MS / MS). The obtained spectra show that:

[0084] Sucralose: After atomization, many extraneous peaks appear in the spectrum, including peaks that have undergone dehydration reaction with glycerol. After the glucose in sucralose undergoes ring opening, one or two cls are lost.

[0085] Neotame: A component that produces trace amounts of hydrolysate after atomization.

[0086] NHDC: After atomization, partial pyrolysis occurred, and the pyrolysis product was HDC.

[0087] The test results above show that neotame and NHDC have better stability than sucralose before and after atomization, and neotame is better than NHDC. NHDC underwent partial pyrolysis, and the pyrolysis product HDC is also a sweetener.

[0088] (3) Based on the test results of steps (1) and (2) above, it can be determined that neotame is the most suitable for closed electronic atomizers, followed by NHDC, and sucralose is the worst.

[0089] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0090] Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present invention.

Claims

1. A method for rapidly screening solid substances suitable for electronic atomization devices, characterized in that, include: (1) The solid sample to be tested is heated within the first preset temperature range, and the morphological changes of the solid sample to be tested are observed during the heating process. The morphological changes include whether the solid sample to be tested is liquefied, the color depth and color stability, whether it is vaporized, whether there is solid expansion, whether it is carbonized or whether black substances are generated. (2) The solid sample to be tested is atomized within a second preset temperature range, and the compositional changes of the solid sample before and after atomization are analyzed by a high-resolution mass spectrometer. (3) Based on the morphological and compositional changes of the solid sample to be tested, determine whether the solid sample to be tested is suitable for an electronic atomization device. Wherein, the first preset temperature range does not exceed the extreme temperature threshold that the electronic atomizing device can withstand, and the second preset temperature range does not exceed the operating temperature threshold of the electronic atomizing device. In step (1), the solid sample to be tested is placed in a capillary tube for the heating treatment, and the height of the solid sample to be tested in the capillary tube accounts for 2-5% of the height of the capillary tube; and / or, the compaction density of the solid sample to be tested in the capillary tube is 0.0003-0.0006 g / mm. 3 , Step (1) satisfies at least one of the following conditions: during the heating process, the morphological changes of the solid sample to be tested are observed by video recording and / or photography, and the temperatures corresponding to different morphological change stages are recorded; The heating rate of the heating process is 1℃~10℃ / min; The particle size of the solid sample to be tested is no greater than 0.2 mm; The first preset temperature range is 30~300℃; The solid sample to be tested was heated using an MP-80 melting point apparatus. In step (2), the solid sample to be tested is mixed with propylene glycol and glycerol to obtain an nebulizer, and the mixture of propylene glycol and glycerol is used as a control solution. The components of the nebulizer and the control solution before and after nebulization are analyzed using a quadrupole-time-of-flight LC-MS / MS. In step (3), based on the morphological and compositional changes of the solid sample to be tested, and in conjunction with the heat resistance rating evaluation standard, it is determined whether the solid sample to be tested is suitable for the electronic atomization device. The heat resistance rating evaluation standard is based on the morphological changes of the solid sample to be tested after being heated, as shown below: Level 1: No discoloration before and after heating treatment, and volume expansion after heating treatment is no more than 30%; Level 3: The color changes to black after heating, or the volume expands by no less than 100% after heating. Level 2: The change is between Level 1 and Level 3; Wherein, when the heat resistance level of the solid sample to be tested is Class I or Class II, it is suitable for use in the electronic atomization device. Step (3) further includes: comparing the thermal stability of various solid samples based on morphological and compositional changes, and determining the most suitable solid sample for use in the electronic atomization device. The solid sample to be tested is the atomizing liquid additive of the electronic atomizing device, and the atomizing liquid additive includes a sweetener.

2. The method according to claim 1, characterized in that, Record the liquefaction temperature of the solid sample to be tested in step (1), and determine the second preset temperature range based on the liquefaction temperature and the operating temperature threshold of the electronic atomization device.

3. The method according to claim 1, characterized in that, Before the atomization process, the atomizing liquid and the control liquid are diluted to a final volume with ethanol, and the components of the atomizing liquid and the control liquid before atomization are analyzed; and / or, during the atomization process, a filter is used to collect the atomizing liquid flue gas and the control liquid flue gas, and the filter after absorbing the flue gas is extracted and filtered with ethanol, and the components of the atomizing liquid and the control liquid after atomization are analyzed.

4. The method according to claim 3, characterized in that, The filter used to absorb flue gas is the filter that has absorbed flue gas 100 to 200 times.

5. Use of the method according to any one of claims 1 to 4 in screening atomizing fluid raw materials for electronic atomizing devices or comparing the thermal stability of atomizing fluid raw materials for electronic atomizing devices.

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