Preparation method of roasted sweet spice for cigarettes and application of roasted sweet spice in cigarettes
By combining ionic liquid synergistic extraction with gel permeation chromatography, the problems of low efficiency and aroma loss in traditional sweet potato extract preparation methods have been solved, resulting in a rich and stable aroma of roasted sweet flavoring for tobacco, which improves the smoke quality and taste of cigarettes.
Patent Information
- Application Number
- CN202511267602.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-05
- Publication Date
- 2025-11-21
AI Technical Summary
Traditional methods for preparing sweet potato extract suffer from problems such as low extraction rate, high equipment cost, and severe aroma loss. Existing tobacco flavorings have poor roasted sweetness and unstable quality. When applied to cigarettes, they produce dry smoke, are highly irritating, and have poor aroma coordination.
A combination of ionic liquid synergistic extraction and gel permeation chromatography separation process was adopted, including steps such as sweet potato pretreatment, ultrasonic extraction, ionic liquid mixing, oscillation extraction, and gel permeation chromatography separation, to prepare a tobacco-grade sweet flavoring.
The prepared tobacco roasted sweet flavoring has a rich aroma and stable quality. When applied to cigarettes, it significantly improves the smoke concentration and sweetness, reduces the irritation of the smoke, and enhances the richness and harmony of the aroma, thus meeting the flavor and taste requirements of Chinese cigarettes.
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Figure BDA0005583718360000061
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of essence and flavor technology, in particular to a preparation method of a roasted sweet flavor for cigarettes and its application in cigarettes. BACKGROUND
[0002] Edible essence and flavor can enhance the natural flavor of food, compensate for the loss of flavor during food processing, and improve the flavor of food. It can also neutralize or mask the bitter and fishy taste of food, improve the taste of food, and enhance the appetite by properly modifying the aroma and taste. As an important component of Chinese cigarettes, cigarette essence and flavor not only affects the taste of cigarettes, but also changes the style of cigarettes, giving them natural and rich aroma characteristics.
[0003] Jujube flavor raw materials have rich sweet substances and good compatibility with tobacco aroma. They are widely used in cigarettes. The commonly used preparation methods include solvent extraction, which has low extraction rate; supercritical fluid extraction, which has high equipment cost and insufficient flavor substances; and steam distillation, which is only suitable for volatile components, resulting in a large loss of jujube flavor components. Ionic liquids have the advantages of thermal stability, low volatility, strong solubility, safety, and environmental protection. Using ionic liquids to prepare jujube extract, and then through Maillard reaction, a roasted sweet flavor with rich aroma, rich flavor, and stable quality can be obtained. The preparation process is safe and environmentally friendly, and the conditions are controllable, which has good application value. SUMMARY
[0004] The technical problem to be solved by the present application is to provide a preparation method of a roasted sweet flavor for cigarettes and its application in cigarettes, which solves the problems of low solvent extraction rate, high supercritical cost, and loss of flavor in the traditional sweet potato extract preparation method, and the problems of poor roasted sweet flavor, unstable quality, dry smoke, strong stimulation, and poor aroma compatibility of existing sweet potato cigarette flavor.
[0005] The technical problem to be solved by the present application is solved by the following technical solution:
[0006] A preparation method of a roasted sweet flavor for cigarettes, comprising the following steps:
[0007] (1) Raw material pretreatment: select fresh sweet potatoes, wash and peel, and cut into small pieces for use;
[0008] (2) Preparation of sweet potato crude extract: add deionized water to the small pieces of sweet potato treated in step (1) according to the solid-liquid ratio of 1: (10-15) (w / v), and use an extraction tank with ultrasonic assistance to extract at a temperature of 45±5℃ for 2-5h; after extraction, separate by using a plate and frame filter press, and add deionized water to the filter residue according to the solid-liquid ratio of 1:8 (w / v) for secondary extraction at a temperature of 45±5℃ for 1-2h; combine the two extraction liquids, filter through a 10kDa membrane, and then concentrate to a solid content of 25-30% to obtain the sweet potato crude extract;
[0009] (3) Ionic liquid-assisted extraction: mix the sweet potato crude extract obtained in step (2) with 1-butyl-3-methylimidazolium acetate ionic liquid according to the mass ratio of 1: (2-5) (w / w), shake and extract, and then cool to room temperature; then add a mixed solvent of n-butanol and 2-butanol, shake and extract again; centrifuge to separate, collect the supernatant, and remove the solvent by reduced pressure distillation to obtain a paste-like liquid;
[0010] (4) Gel permeation chromatography separation: dilute the paste-like liquid obtained in step (3) with 50% ethanol / water solution to a concentration of 10-25%, and separate by using gel permeation chromatography to collect substances with a molecular weight of 150kDa-300kDa, which are tobacco roasted sweet flavor.
[0011] Preferably, in the above technical solution, in step (2), the solid-liquid ratio of the first extraction of sweet potato and water is 1:12.5 (w / v), the first extraction time is 3.5h, and the second extraction time is 1.5h; the filter cloth precision of the plate and frame filter press is 5μm.
[0012] Preferably, in the above technical solution, in step (3), the mass ratio of the sweet potato crude extract T0 to 1-butyl-3-methylimidazolium acetate ionic liquid is 1:3.5 (w / w), the first shaking extraction condition is shaking extraction at 40℃ for 1h, the volume ratio of n-butanol to 2-butanol is 2:1, and the second shaking extraction condition is shaking at a frequency of 200rpm for 0.5h at 40℃.
[0013] Preferably, in the above technical solution, in step (3), the centrifugation is performed by using a tubular centrifuge at a speed of 12000r / min for 8min.
[0014] Preferably, in the above technical solution, in step (4), the gel permeation chromatography condition is:
[0015] Chromatographic column: TSKgel G4000PWxl (7.8×300mm);
[0016] Mobile phase: 0.1M phosphate buffer with a pH of 6.8;
[0017] The flow rate is 0.6 mL / min.
[0018] A tobacco roasting sweet flavor obtained according to the preparation method.
[0019] The application of the tobacco roasting sweet flavor in cigarettes is that the tobacco roasting sweet flavor is added into cigarettes by a flavor injection machine at a proportion of 0.01-0.5% of the mass of the cigarettes, and the cigarettes are used after being stored under constant temperature and humidity for 48 h.
[0020] Preferably, in the technical scheme, the addition proportion of the tobacco roasting sweet flavor in cigarettes is 0.1%.
[0021] The technical scheme has the following beneficial effects:
[0022] The tobacco roasting sweet flavor prepared by the combined process of "ionic liquid synergistic extraction + gel permeation chromatography separation" has rich and stable quality, and when it is applied to cigarettes in a specific proportion, it can effectively improve the smoke concentration and sweet and smooth feeling, significantly reduce the smoke irritation and oral residue, enhance the aroma richness and coordination, and perfectly meet the needs of Chinese cigarettes for flavor and taste. The process is safe and environmentally friendly, the parameters are controllable, the raw material utilization rate is high, and it has good industrial application value, effectively making up for the shortcomings of traditional processes and existing flavors. DETAILED DESCRIPTION
[0023] Various exemplary embodiments of the present application will now be described in detail. It should be noted that the relative arrangement of components and steps, numerical expressions, and numerical values set forth in these embodiments are not intended to limit the scope of the present application unless otherwise specifically stated.
[0024] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, and the materials and reagents used are commercially available unless otherwise specified. The equipment used in the experiments is well known to those skilled in the art unless otherwise specified.
[0025] Example 1
[0026] 1. Raw material pretreatment
[0027] Fresh sweet potatoes (tobacco potatoes 25) without mold were selected, washed, peeled, and cut into small pieces for use.
[0028] 2. Preparation of sweet potato crude extract
[0029] Deionized water was added at a material-to-liquid ratio of 1: (10-15) (w / v) (preferably 1:12.5); extraction was performed using an extraction tank with ultrasonic assistance (40 kHz) at an extraction temperature of 45±5℃ for 2-5h (preferably 3.5h); after the first extraction, separation was performed using a plate-and-frame filter press (filter cloth precision 5μm), and the residue was subjected to secondary extraction at a material-to-liquid ratio of 1:8 (w / v) at an extraction temperature of 45±5℃ for 1-2h (preferably 1.5h); the combined extract was concentrated to a solid content of 25-30% by membrane filtration (10 kDa) to obtain sweet potato crude extract T0.
[0030] 3. Ionic liquid synergistic extraction
[0031] (1) The sweet potato crude extract T0 was mixed with 1-butyl-3-methylimidazole acetate ionic liquid at a mass ratio of 1: (2-5) (w / w) (preferably 1:3.5), and subjected to oscillation extraction at 40℃ for 1h, and then cooled to room temperature. The mixture was subjected to secondary oscillation extraction using a mixed solvent of n-butanol:2-butanol=2:1 (volume ratio) at a frequency of 200 rpm and 40℃ for 0.5h.
[0032] (2) The mixture was separated using a tubular centrifuge (12000r / min, 8min), and the supernatant was collected and subjected to vacuum distillation to remove the solvent, thereby obtaining a black-brown paste-like liquid G1.
[0033] 4. Effect verification
[0034] The paste-like liquid G1 was added to cigarettes at a proportion of 0.1% of the mass of the cigarettes using a flavor injection machine, and the sample was stored under constant temperature and humidity conditions for 48h before sensory evaluation.
[0035] Example 2
[0036] 1. Raw material pretreatment
[0037] Fresh sweet potatoes (Yanshu 25) without mold were selected, washed, peeled, and cut into small pieces for use.
[0038] 2. Preparation of sweet potato crude extract
[0039] Deionized water was added at a material-to-liquid ratio of 1: (10-15) (w / v) (preferably 1:12.5); extraction was performed using an extraction tank with ultrasonic assistance (40 kHz) at an extraction temperature of 45±5℃ for 2-5h (preferably 3.5h); after the first extraction, separation was performed using a plate-and-frame filter press (filter cloth precision 5μm), and the residue was subjected to secondary extraction at a material-to-liquid ratio of 1:8 (w / v) at an extraction temperature of 45±5℃ for 1-2h (preferably 1.5h); the combined extract was concentrated to a solid content of 25-30% by membrane filtration (10 kDa) to obtain sweet potato crude extract T0.
[0040] 3. Dilute the paste liquid T0 with 50% ethanol / water solution to a concentration of 10-25%, use Gel Permeation Chromatography (GPC) to separate, collect the material with a molecular weight between 150 kDa-300 kDa, which is the roasted sweet flavor K2.
[0041] Chromatographic conditions: Column: TSKgel G4000PWxl (7.8 x 300 mm);
[0042] Mobile phase: 0.1 M phosphate buffer (pH 6.8);
[0043] Flow rate: 0.6 mL / min.
[0044] 4. Effect verification
[0045] Add the flavor liquid K2 to cigarettes at a proportion of 0.1% of the quality of cigarettes using a flavor essence injector, which is sample 2, and store it under constant temperature and humidity conditions for 48 h before sensory evaluation.
[0046] Example 3
[0047] 1. Raw material pretreatment
[0048] Select commercially available fresh sweet potatoes (tobacco potatoes 25) without mildew, wash and peel, and cut into small pieces for use.
[0049] 2. Preparation of sweet potato crude extract
[0050] Add deionized water at a solid-liquid ratio of 1: (10-15) (w / v), preferably 1:12.5; use an extraction tank with ultrasonic assistance (40 kHz) to extract, maintain the extraction temperature at 45±5°C, and the extraction time for 2-5 h (preferably 3.5 h); after the first extraction, use a plate and frame filter press (filter cloth precision 5 μm) to separate, and the filter residue is extracted for the second time at a solid-liquid ratio of 1:8, the extraction temperature is 45±5°C, and the extraction time is 1-2 h (preferably 1.5 h); after the extraction liquid is filtered by membrane (10 kDa), it is concentrated to a solid content of 25-30%, and the sweet potato crude extract T0 is obtained.
[0051] 3. Ionic liquid assisted extraction
[0052] (1) Mix the sweet potato crude extract T0 with 1-butyl-3-methylimidazole acetate ionic liquid at a mass ratio of 1: (2-5) (w / w) (preferably 1:3.5), and extract for 1 hour under 40°C condition, and then cool to room temperature. Then use a mixed solvent of n-butanol:2-butanol=2:1 (volume ratio) to extract for the second time for 0.5 hours under the condition of 200 rpm and 40°C.
[0053] (2) Using a tubular centrifuge (12000 r / min, 8 min) to separate, collect the supernatant, remove the solvent after distillation under reduced pressure, and obtain brown paste liquid G1.
[0054] 4, Dilute the paste liquid G1 to a concentration of 10-25% using a 50% ethanol / water solution, separate using gel permeation chromatography (GPC), and collect the material with a molecular weight of 150 kDa-300 kDa, which is the roasted sweet flavor K3.
[0055] Chromatographic conditions: Column: TSKgel G4000PWxl (7.8x300mm);
[0056] Mobile phase: 0.1M phosphate buffer (pH 6.8);
[0057] Flow rate: 0.6 mL / min.
[0058] 5, Effect verification
[0059] Add the flavor liquid K3 to the cigarette at a proportion of 0.1% of the quality of the cigarette using a flavor essence flavor injector, and record it as sample 3. After 48h of storage under constant temperature and humidity conditions, perform sensory evaluation.
[0060] Table 1. Sensory evaluation results
[0061]
[0062] The sensory evaluation results in Table 1 show that the products of Examples 1-3 differ significantly in improving the flavor and taste of cigarettes: sample 1 (G1) extracted only by an ionic liquid can improve the sweetness of smoke, but has problems of dry smoke, strong irritation, and obvious oral residue; sample 2 (K2) separated only by gel permeation chromatography has general sweet and smooth feeling of smoke, and weak roasted sweet notes and insufficient aroma richness; sample 3 (K3) prepared by the complete process of "ionic liquid cooperative extraction + gel permeation chromatography separation" performs best in smoke concentration, sweet and smooth feeling, and roasted sweet notes, while significantly reducing the irritation of smoke, and the aroma richness more meets the needs of cigarettes, which confirms the key role of the complete process in improving the application effect of roasted sweet flavor for cigarettes.
[0063] Although the present application has been disclosed as above with examples, it is not intended to limit the present application, and any person skilled in the art can make various selections and modifications without departing from the spirit and scope of the present application, therefore the protection scope of the present application is defined by the claims and their equivalent forms.
Claims
1. A process for the preparation of a roasted sweet tobacco flavouring, characterised in that, The method comprises the following steps: (1) raw material pretreatment: fresh sweet potato is selected, washed, peeled and cut into small pieces for standby; (2) preparation of sweet potato extract: deionized water is added to the small pieces of sweet potato treated in step (1) according to the solid-liquid ratio of 1: (10-15) (w / v), and an extraction tank with ultrasonic assistance is used for extraction, the extraction temperature is 45±5℃, and the extraction time is 2-5h; after extraction, a plate and frame filter press is used for separation, the filter residue is added with deionized water according to the solid-liquid ratio of 1:8 (w / v) for secondary extraction, the extraction temperature is 45±5℃, and the extraction time is 1-2h; the two extraction liquids are combined, filtered through a 10kDa membrane, and concentrated to a solid content of 25-30% to obtain a sweet potato extract; (3) ionic liquid assisted extraction: the sweet potato extract obtained in step (2) is mixed with 1-butyl-3-methylimidazolium acetate ionic liquid at a mass ratio of 1: (2-5) (w / w), shaken and extracted, and then cooled to room temperature; then a mixed solvent of n-butanol and 2-butanol is added, and the second shaking and extraction is performed; centrifugal separation, collection of supernatant, removal of solvent by reduced pressure distillation to obtain a paste-like liquid; (4) gel permeation chromatography separation: the paste-like liquid obtained in step (3) is diluted to a concentration of 10-25% with 50% ethanol / water solution, and separated by gel permeation chromatography, and the material with a molecular weight of 150kDa-300kDa is collected, which is a tobacco baking sweet flavor.
2. A process for the preparation of a tobacco roasting flavouring according to claim 1, characterized in that, In step (2), the solid-liquid ratio of the first extraction of sweet potato and water is 1:12.5 (w / v), the first extraction time is 3.5h, the second extraction time is 1.5h, and the filter cloth precision of the plate and frame filter press is 5μm.
3. A process for the preparation of a tobacco roasting flavouring according to claim 1, characterized in that, In step (3), the mass ratio of the sweet potato extract T0 and 1-butyl-3-methylimidazolium acetate ionic liquid is 1:3.5 (w / w), the first shaking and extraction condition is 40℃ for 1h, the volume ratio of n-butanol and 2-butanol is 2:1, and the second shaking and extraction condition is 200rpm for 0.5h at 40℃.
4. A process for the preparation of a tobacco roasting flavouring according to claim 1, characterized in that, In step (3), the centrifugation is performed by using a tubular centrifuge at a speed of 12000r / min for 8min.
5. A process for the preparation of a tobacco roasting flavouring according to claim 1, characterized in that, In step (4), the gel permeation chromatography conditions are as follows: Chromatographic column: TSKgel G4000PWxl (7.8×300mm); Mobile phase: 0.1M phosphate buffer with pH of 6.8; Flow rate: 0.6mL / min.
6. A tobacco baking sweet flavor prepared by the preparation method according to any one of claims 1-5.
7. Use of a tobacco roasting flavouring according to claim 6 in a cigarette, characterized in that, The application is that the tobacco baking sweet flavor is added into cigarettes by a flavor injection machine according to a proportion of 0.01-0.5% of the mass of cigarettes, and used after being stored for 48h under constant temperature and humidity conditions.
8. Use of a tobacco roasting flavouring according to claim 6 in a cigarette, characterized in that, The addition proportion of the tobacco baking sweet flavor in cigarettes is 0.1%.