Furfural temperature-sensitive liposome for cigarettes and preparation method of furfural temperature-sensitive liposome
By preparing thermosensitive liposomes containing components such as dipalmitoylphosphatidylcholine, cholesterol, and furfural, the problems of high loss rate and uncoordinated release of flavorings and fragrances in traditional tobacco products during processing and storage have been solved. This has enabled precise controlled release and stable flavor enhancement, thereby improving the user experience of new tobacco products.
Patent Information
- Application Number
- CN202511135601.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-14
- Publication Date
- 2025-11-21
AI Technical Summary
Traditional tobacco flavorings suffer from high loss rates during processing and storage, and their release is uncoordinated, failing to meet consumers' needs for aroma complexity and physiological satisfaction, especially in new tobacco products.
Temperature-sensitive liposomes were prepared using ingredients such as dipalmitoylphosphatidylcholine, cholesterol, and furfural. By controlling temperature changes, aroma release was triggered, increasing the encapsulation rate to 96% and achieving precise controlled release of aroma.
It significantly reduces the volatilization of fragrances and flavorings, prolongs the aroma release time, and enhances the aroma intensity and stability, thus meeting consumer needs and possessing broad market application value.
Smart Images
Figure CN120982773A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of liposome preparation technology, and in particular to a temperature-sensitive liposome for furfural cigarettes and its preparation method. Background Technology
[0002] Currently, the application of flavorings and fragrances in tobacco products mainly relies on physical mixing and flavor capsule technology. These methods have significant shortcomings in the precise control of aroma release. Physical mixing is the most basic flavoring method, where flavorings are directly mixed with the tobacco matrix or filter material. Its release depends entirely on a passive diffusion mechanism, resulting in over 80% of the flavorings being lost through premature evaporation during non-smoking stages (such as storage and transportation). This not only leads to low flavoring utilization but also results in insufficient aroma intensity and rapid decay during actual smoking, with consumers often experiencing a noticeable weakening of the aroma after only 3-5 puffs. While flavor capsule technology allows for artificially triggered release, its reliance on external pressure results in a sudden, instantaneous release of aroma, particularly noticeable in heated tobacco products—where the smoke temperature is only within the 45-55℃ range. However, the rapid release rate of the flavoring after the capsule bursts cannot match the slowly rising smoke temperature curve, leading to an uncoordinated phenomenon where the initial aroma is too strong but subsequent aromas are weak. Temperature-sensitive liposomes, on the other hand, are triggered by temperature changes. When the external temperature reaches or exceeds the phase transition temperature (Tm) of the membrane material, the phospholipid bimolecule transforms from a "gel" state structure to a "liquid crystal" state structure. The increased disorder of the acyl chains at the hydrophobic ends of the phospholipid leads to increased fluidity of the liposome membrane, increasing the release rate of drugs encapsulated in the lipid core and drugs embedded in the bilayer. This technology can prolong the duration of aroma release, thereby achieving a stable aroma enhancement effect.
[0003] Traditional tobacco flavorings face high processing losses and poor storage stability in practical applications, severely limiting their industrial application value. In the processing stage, especially in high-temperature drying reconstituted tobacco production lines, conventional flavorings suffer losses as high as 30-50% due to volatilization or thermal decomposition. Regarding storage stability, unintended reactions between traditional flavorings and complex tobacco components (such as nicotine, alkaloids, and reducing sugars) are the main cause of aroma deterioration. Temperature-sensitive flavoring technology overcomes these limitations through multiple stability designs.
[0004] Traditional flavoring techniques struggle to meet consumers' complex demands for layered aromas, physiological satisfaction, and ease of use in tobacco products, especially in new tobacco products. In traditional cigarettes, directly added flavorings undergo thermal decomposition in the high-temperature combustion zone (>800℃), producing undesirable components such as aldehydes and olefins. For example, the added β-damasne undergoes a 73.2% decomposition rate after combustion, not only losing its characteristic aroma but also generating irritating substances like benzaldehyde. While flavor capsules partially improve aroma release, they suffer from issues such as aroma homogenization and incompatibility with the natural tobacco aroma. For instance, in commercially available alcohol-flavored flavor capsule cigarettes, the strong exogenous flavoring masks the natural tobacco aroma after compression, disrupting the overall balance of the smoke. Temperature-sensitive flavoring technology achieves breakthrough improvements through precise controlled release and sensory synergy design. Summary of the Invention
[0005] The purpose of this invention is to overcome the shortcomings of the prior art and provide a furfural-based thermosensitive liposome and its preparation method.
[0006] The technical solution adopted by this invention to solve its technical problem is:
[0007] A method for preparing furfural-based thermosensitive liposomes includes the following steps:
[0008] Weigh out dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, then add them dropwise to PBS buffer. After sonication, the resulting solution is passed through a 0.22 μm organic filter membrane to obtain the furfural-based thermosensitive liposomes for use in cigarettes.
[0009] Furthermore, the ratio of dipalmitoylphosphatidylcholine:cholesterol:furfural:ethyl ether:PBS buffer (mg:mg:μL:mL:mL) is 20-150:10:50-200:2:50.
[0010] Furthermore, the ratio of dipalmitoylphosphatidylcholine:cholesterol:furfural:ethyl ether:PBS buffer (mg:mg:μL:mL:mL) is 50:10:50:2:50.
[0011] Further, using a 1mL syringe, the solution was gradually added dropwise to a stirred PBS buffer while controlling the injection rate. The resulting solution was sonicated for 5-20 minutes and then passed through a 0.22μm organic filter membrane.
[0012] The stirring speed is 10 rpm, the temperature is 20-50℃, and the time is 10 min;
[0013] Alternatively, the pH of the PBS buffer is 7.4.
[0014] Furthermore, the temperature of the PBS buffer was 30°C, and the ultrasonic dispersion time was 10 min.
[0015] The furfural-based thermosensitive liposomes for cigarettes were prepared using the method described above.
[0016] Furthermore, the encapsulation efficiency of the furfural-based thermosensitive liposomes reaches 96%.
[0017] The method for determining the encapsulation efficiency of furfural-containing thermosensitive liposomes as described above includes the following steps:
[0018] Take the sample and put it into a dialysis bag. Place it in PBS buffer for dialysis. After dialysis, add anhydrous ethanol to the sample, sonicate to break the emulsion, add PBS buffer to make up the volume, and then measure the absorbance.
[0019] Furthermore, the molecular weight of the dialysis bag is 8000-14000;
[0020] The dialysis conditions were as follows: temperature 4℃, sample addition of 5mL per 250mL PBS buffer, time 14h, and dialysis solution replacement every 2h, 6h, and 14h.
[0021] The time for ultrasonic demulsification is 10 minutes.
[0022] The advantages and positive effects of this invention are as follows:
[0023] This invention prepares a furfural-based thermosensitive formulation for tobacco use. Optimization of its formulation shows that the thermosensitive liposomes achieve an encapsulation rate as high as 96%, which improves the loss of flavor and fragrance in tobacco products, enhances the aroma enhancement effect and duration, and thus possesses broad market prospects and application value. Attached Figure Description
[0024] Figure 1 This is a graph showing the encapsulation efficiency of furfural thermosensitive liposomes with different formulations in this invention; where groups A to J represent embodiments 1-10 respectively.
[0025] Figure 2 The diagram shows the encapsulation efficiency measured in the embodiments and comparative examples of this invention; where group A represents embodiment 1, and groups K and L represent comparative examples 1-2, respectively. Detailed Implementation
[0026] The present invention will be further described below with reference to the embodiments. The following embodiments are descriptive and not limiting, and should not be used to limit the scope of protection of the present invention.
[0027] The various experimental operations involved in the specific embodiments are all conventional techniques in the field. For parts not specifically annotated in this document, those skilled in the art can refer to various commonly used reference books, scientific and technological documents or related instructions and manuals prior to the filing date of this invention to carry out the operations.
[0028] A method for preparing furfural-based thermosensitive liposomes includes the following steps:
[0029] Weigh out dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, then add them dropwise to PBS buffer. After sonication, the resulting solution is passed through a 0.22 μm organic filter membrane to obtain the furfural-based thermosensitive liposomes for use in cigarettes.
[0030] Preferably, the ratio of dipalmitoylphosphatidylcholine:cholesterol:furfural:ethyl ether:PBS buffer (mg:mg:μL:mL:mL) is 20-150:10:50-200:2:50.
[0031] Preferably, the ratio of dipalmitoylphosphatidylcholine:cholesterol:furfural:ethyl ether:PBS buffer (mg:mg:μL:mL:mL) is 50:10:50:2:50.
[0032] Preferably, a 1 mL syringe is used to draw the solution, the injection rate is controlled, and the solution is gradually added dropwise to a stirred PBS buffer. The resulting solution is sonicated for 5-20 min and then passed through a 0.22 μm organic filter membrane.
[0033] The stirring speed is 10 rpm, the temperature is 20-50℃, and the time is 10 min;
[0034] Alternatively, the pH of the PBS buffer is 7.4.
[0035] Preferably, the temperature of the PBS buffer is 30°C and the ultrasonic dispersion time is 10 min.
[0036] The furfural-based thermosensitive liposomes for cigarettes were prepared using the method described above.
[0037] Preferably, the encapsulation efficiency of the furfural-based thermosensitive liposomes reaches 96%.
[0038] The method for determining the encapsulation efficiency of furfural-containing thermosensitive liposomes as described above includes the following steps:
[0039] Take the sample and put it into a dialysis bag. Place it in PBS buffer for dialysis. After dialysis, add anhydrous ethanol to the sample, sonicate to break the emulsion, add PBS buffer to make up the volume, and then measure the absorbance.
[0040] Preferably, the molecular weight of the dialysis bag is 8000-14000;
[0041] The dialysis conditions were as follows: temperature 4℃, sample addition of 5mL per 250mL PBS buffer, time 14h, and dialysis solution replacement every 2h, 6h, and 14h.
[0042] The time for ultrasonic demulsification is 10 minutes.
[0043] The formulation optimization of the furfural thermosensitive liposomes includes the following steps:
[0044] (1) Under the conditions of a fixed membrane material ratio of 5:1, a PBS buffer temperature of 30℃, and an ultrasonic dispersion time of 10 min, furfural addition amount (50μL, 100μL, 150μL, 200μL) was changed to prepare furfural thermosensitive liposomes and the encapsulation efficiency was measured.
[0045] (2) Under the conditions of fixed furfural addition of 50 μL, buffer PBS temperature of 30℃ and ultrasonic dispersion time of 10 min, furfural thermosensitive liposomes were prepared by changing the membrane material ratio (2:1, 5:1, 8:1, 10:1) and the encapsulation efficiency was measured.
[0046] (3) Furfural thermosensitive liposomes were prepared under the following conditions: the amount of furfural added was fixed at 50 μL, the membrane material ratio was 5:1, the temperature of the PBS buffer was 20℃, 30℃, 40℃ and 50℃ respectively, and the ultrasonic dispersion time was 10 min. The encapsulation efficiency was then determined.
[0047] (4) Furfural thermosensitive liposomes were prepared under the following conditions: the amount of furfural added was fixed at 50 μL, the membrane material ratio was 5:1, the temperature of the PBS buffer was 30℃, and the ultrasonic dispersion time was controlled at 5 min, 10 min, 15 min and 20 min respectively. The encapsulation efficiency was then determined.
[0048] The preferred technical solution is that the optimal preparation formula for furfural thermosensitive liposomes for cigarettes is as follows: the furfural addition amount is 50 μL, the membrane material ratio is 5:1, the temperature of the PBS buffer is 30℃, and the ultrasonic dispersion time is 10 min. The furfural thermosensitive liposomes prepared under these conditions have the best encapsulation efficiency.
[0049] Specifically, the relevant preparation and testing methods are as follows:
[0050] Example 1: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0051] The preparation steps of furfural thermosensitive liposomes are as follows:
[0052] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0053] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0054] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0055] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0056] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0057] Example 2: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0058] The preparation steps of furfural thermosensitive liposomes are as follows:
[0059] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0060] In the above steps, the amount of furfural added is 100 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0061] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0062] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0063] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0064] Example 3: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0065] The preparation steps of furfural thermosensitive liposomes are as follows:
[0066] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0067] In the above steps, the amount of furfural added is 150 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0068] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0069] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0070] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0071] Example 4: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0072] The preparation steps of furfural thermosensitive liposomes are as follows:
[0073] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0074] In the above steps, the amount of furfural added is 200 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0075] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0076] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0077] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0078] Example 5: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0079] The preparation steps of furfural thermosensitive liposomes are as follows:
[0080] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0081] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 20 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0082] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0083] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0084] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0085] Example 6: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0086] The preparation steps of furfural thermosensitive liposomes are as follows:
[0087] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0088] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 80 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0089] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0090] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0091] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0092] Example 7: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0093] The preparation steps of furfural thermosensitive liposomes are as follows:
[0094] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0095] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 100 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0096] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0097] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0098] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0099] Example 8: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0100] The preparation steps of furfural thermosensitive liposomes are as follows:
[0101] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0102] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0103] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 20 °C, and the stirring time is 10 min.
[0104] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0105] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0106] Example 9: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0107] The preparation steps of furfural thermosensitive liposomes are as follows:
[0108] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0109] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0110] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 40 °C, and the stirring time is 10 min.
[0111] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0112] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0113] Example 10: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0114] The preparation steps of furfural thermosensitive liposomes are as follows:
[0115] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, and then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0116] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0117] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 50 °C, and the stirring time is 10 min.
[0118] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0119] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0120] Comparative Example 1: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0121] The preparation steps of furfural thermosensitive liposomes are as follows:
[0122] Weigh out appropriate amounts of trehalose, cholesterol, and furfural, add ether to dissolve them completely, then add them dropwise to a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0123] In the above steps, the amount of furfural added is 50 μL, the mass of trehalose is 50 mg, the mass of cholesterol is 10 mg, and the volume of ether added is 2 mL.
[0124] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0125] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0126] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0127] Comparative Example 2: Preparation of a furfural-based thermosensitive liposome for cigarettes
[0128] The preparation steps of furfural thermosensitive liposomes are as follows:
[0129] Weigh out appropriate amounts of dipalmitoylphosphatidylcholine, iron tetroxide nanoparticles, and furfural, add diethyl ether to completely dissolve them, and then drop them into a stirred PBS buffer. After sonicating the resulting solution, pass it through a 0.22 μm organic filter membrane to obtain the furfural thermosensitive liposomes.
[0130] In the above steps, the amount of furfural added is 50 μL, the mass of dipalmitoylphosphatidylcholine is 50 mg, the mass of iron oxide nanoparticles is 10 mg, and the volume of ether added is 2 mL.
[0131] In the above steps, the PBS buffer volume is 50 mL, the pH is 7.4, the stirring speed is 10 rpm, the temperature is 30 °C, and the stirring time is 10 min.
[0132] The completely dissolved solution in the above steps is drawn with a 1 mL syringe, and the injection rate is controlled. It is then gradually added dropwise to the stirred PBS buffer. The resulting solution is sonicated for 10 min and then passed through a 0.22 μm organic filter membrane.
[0133] The encapsulation efficiency of the furfural thermosensitive liposomes prepared in the above steps was determined.
[0134] Test Implementation Example:
[0135] This invention provides a method for preparing furfural thermosensitive liposomes for cigarettes, and optimizes its formulation. The encapsulation efficiency of the furfural thermosensitive liposomes provided in the examples was determined, and the results are as follows:
[0136] Add 5 mL of sample to a dialysis bag (MW8000-14000) and dialyze in 250 mL of PBS buffer (4℃) for 14 h (replace the dialysis buffer every 2 h, 6 h, and 14 h). After dialysis, add 5 mL of anhydrous ethanol to the sample, sonicate to break the emulsion for 10 min, and then add PBS buffer to a final volume of 25 mL. Measure the absorbance. Perform the same treatment on 5 mL of the undialyzed sample and measure the absorbance. Calculate the encapsulation efficiency. The encapsulation efficiency is calculated using the following formula:
[0137]
[0138] Where: CE—the amount of furfural encapsulated by liposomes; CT—the total amount of furfural in liposomes directly measured without treatment.
[0139] Depend on Figure 1 It can be seen that the encapsulation efficiency of furfural thermosensitive liposomes prepared with different formulations varies considerably. The formulation described in Example 1 yielded furfural thermosensitive liposomes with an encapsulation efficiency of 96%, significantly higher than other groups. Figure 2 It was found that the encapsulation efficiency of furfural thermosensitive liposomes prepared by replacing dipalmitoylphosphatidylcholine with trehalose was only 82.5%; while the encapsulation efficiency of furfural thermosensitive liposomes prepared by replacing cholesterol with iron oxide nanoparticles was 80%, both significantly lower than the encapsulation efficiency measured in Example 1. Therefore, the optimal encapsulation efficiency was obtained by preparing furfural thermosensitive liposomes under the following conditions: a fixed furfural addition amount of 50 μL, a membrane material ratio of 5:1, a PBS buffer temperature of 30°C, and an ultrasonic dispersion time of 10 min. This is the optimal formulation.
[0140] Meanwhile, by comparing Example 1, Comparative Example 1, and Comparative Example 2, it can be seen that dipalmitoylphosphatidylcholine and cholesterol have a synergistic effect in this invention, which can synergistically improve the relevant properties of the prepared furfural-based thermosensitive liposomes. In particular, when the mass ratio of dipalmitoylphosphatidylcholine to cholesterol is 5:1, dipalmitoylphosphatidylcholine and cholesterol in this invention have a significant synergistic effect, which can significantly improve the relevant properties of the prepared furfural-based thermosensitive liposomes.
[0141] In summary, the furfural thermosensitive liposome for tobacco products of this invention has a good encapsulation efficiency, which can significantly reduce the volatilization of traditional tobacco flavorings and fragrances, and can be well applied to the development of new tobacco flavorings and fragrances.
[0142] Although embodiments of the invention have been disclosed for illustrative purposes, those skilled in the art will understand that various substitutions, variations, and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the scope of the invention is not limited to the contents disclosed in the embodiments.
Claims
1. A method for preparing furfural-based thermosensitive liposomes, characterized in that: Includes the following steps: Weigh out dipalmitoylphosphatidylcholine, cholesterol, and furfural, add ether to dissolve them completely, then add them dropwise to PBS buffer. After sonication, the resulting solution is passed through a 0.22 μm organic filter membrane to obtain the furfural-based thermosensitive liposomes for use in cigarettes.
2. The preparation method according to claim 1, characterized in that: The ratio of dipalmitoylphosphatidylcholine:cholesterol:furfural:ethyl ether:PBS buffer (mg:mg:μL:mL:mL) is 20-150:10:50-200:2:
50.
3. The preparation method according to claim 1, characterized in that: The ratio of dipalmitoylphosphatidylcholine:cholesterol:furfural:diethyl ether:PBS buffer (mg) The ratio of mg:μL:mL:mL is 50:10:50:2:
50.
4. The preparation method according to any one of claims 1 to 3, characterized in that: Using a 1mL syringe, the solution is gradually added dropwise to a stirred PBS buffer solution, controlled at the injection rate. The resulting solution is sonicated for 5-20 minutes and then passed through a 0.22μm organic filter membrane. The stirring speed is 10 rpm, the temperature is 20-50℃, and the time is 10 min; Alternatively, the pH of the PBS buffer is 7.
4.
5. The preparation method according to claim 4, characterized in that: The temperature of the PBS buffer was 30°C, and the ultrasonic dispersion time was 10 min.
6. Furfural-based thermosensitive liposomes for cigarettes prepared by the preparation method according to any one of claims 1 to 5.
7. The furfural-based thermosensitive liposome for cigarettes according to claim 6, characterized in that: The encapsulation efficiency of the furfural-based thermosensitive liposomes reached 96%.
8. The method for determining the encapsulation efficiency of furfural-based thermosensitive liposomes as described in claim 6, characterized in that: Includes the following steps: Take the sample and put it into a dialysis bag. Place it in PBS buffer for dialysis. After dialysis, add anhydrous ethanol to the sample, sonicate to break the emulsion, add PBS buffer to make up the volume, and then measure the absorbance.
9. The determination method according to claim 7, characterized in that: The molecular weight of the dialysis bag is 8000-14000; The dialysis conditions were as follows: temperature 4℃, sample addition of 5mL per 250mL PBS buffer, time 14h, and dialysis solution replacement every 2h, 6h, and 14h. The time for ultrasonic demulsification is 10 minutes.