Rice aroma and method of preparation and use thereof

By freeze-drying and dehydrating glutinous rice leaves, then mixing and grinding them with palm oil to form a pulp, and performing multiple extractions and concentrations, the problem of poor aroma in existing glutinous rice-flavored tobacco products has been solved. This has enabled the efficient extraction of high-quality glutinous rice leaf oil, improving the aroma and aftertaste of cigarettes.

CN117757572BActive Publication Date: 2026-02-13CHINA TOBACCO GUANGXI IND
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Patent Information

Application Number
CN202311837534.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-28
Publication Date
2026-02-13
Estimated Expiration
2043-12-28

AI Technical Summary

Technical Problem

The glutinous rice aroma in existing glutinous rice-flavored tobacco products comes from glutinous rice, resulting in poor aroma, poor aftertaste, and off-flavors and irritation. Existing extraction methods are difficult to effectively extract the aroma of high-quality glutinous rice leaves.

Method used

Glutinous rice leaves were freeze-dried and dehydrated, then mixed with palm oil, ground into a pulp, and then subjected to a first extraction, a second extraction, and concentration to prepare glutinous rice leaf oil.

Benefits of technology

It improves the extraction efficiency and aroma concentration of glutinous rice and basil oil, reduces impurity content and spoilage risk, endows tobacco products with a rich glutinous rice aroma, and improves the aroma and aftertaste of cigarettes.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to the field of tobacco flavor, in particular to a kind of glutinous rice leaf oil and preparation method and purposes thereof, preparation method includes the following steps: glutinous rice leaf is frozen and dried and dehydrated, then mixed with palm oil and grinded to make pulp, then first extraction, second extraction, finally concentrated to obtain glutinous rice leaf oil.The preparation method of the present application is simple, safe and environmentally friendly, and the raw materials are easy to obtain, and industrial production can be realized, through the synergistic effect of freezing drying, dehydration, mixing with palm oil, grinding to make pulp, first extraction, second extraction and concentration, the glutinous rice leaf can be fully extracted, and the glutinous rice leaf oil which can be preserved and not easily spoiled is prepared.The glutinous rice leaf oil is applied in cigarette, can give tobacco product glutinous rice aroma, enrich tobacco product aroma characteristic;Its aroma characteristics are coordinated with cigarette style, aftertaste is pure, obviously reduce the miscellaneous gas and irritability of cigarette, overall enhance the aroma quality of cigarette.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of tobacco flavor, in particular to a kind of waxy rice leaf oil and preparation method and purposes thereof. BACKGROUND

[0002] Waxy rice leaf is a herbaceous plant of the genus of waxy rice in acanthaceae, which emits a rich waxy rice fragrance after drying, has the effects of anti-aging, cooling, spleen and stomach nourishing, food digestion and immunity improvement, and is a natural spice plant with important medicinal, edible and ornamental values. According to the report of the Committee of Flora, waxy rice leaf contains more than 40 aroma components and beneficial amino acids.

[0003] At present, the application of waxy rice leaf is mainly direct use of leaf; for example, CN115836699A discloses a rice flower tea and its preparation method, and CN101138375A discloses a preparation method of waxy rice tea, which directly mixes waxy rice leaf with tea and other materials.

[0004] The existing extraction method of waxy rice leaf is mainly water or ethanol extraction. For example, the study in "Ethanol-water system dissolution of waxy rice components style research [J]. Anhui Agricultural Sciences, 2018, 46(22): 3." uses ethanol and water as solvents to dissolve waxy rice leaf components.

[0005] At present, the waxy rice aroma in tobacco products is mainly realized by waxy rice aroma extraction or synthetic flavor blending, which has poor effect. The natural waxy rice leaf aroma is rich, and the quality of the product obtained by the existing extraction method is insufficient, which is difficult to have good application in tobacco products. Therefore, it is necessary to improve the extraction process of waxy rice leaf at present, and obtain an extract with excellent aroma quality, which will greatly promote the development of waxy rice type tobacco products. SUMMARY

[0006] Therefore, the technical problem to be solved by the present application is to overcome the poor aroma, poor aftertaste, and miscellaneous gas and irritation of the existing waxy rice aroma type tobacco product, so as to provide a waxy rice leaf oil and a preparation method and purposes thereof.

[0007] The technical problem to be solved by the present application is to overcome the current situation that the waxy rice aroma in the existing waxy rice aroma type tobacco product comes from the extraction of waxy rice, so as to provide a waxy rice leaf oil and a preparation method and purposes thereof.

[0008] The present application protects a preparation method of waxy rice leaf oil in the first aspect, wherein the preparation method comprises the following steps: after the waxy rice leaf is freeze-dried and dehydrated, it is mixed with palm oil to grind and make pulp, then first extraction and second extraction are carried out, and finally waxy rice leaf oil is obtained by concentration.

[0009] In the present application, the fresh glutinous rice leaves are washed repeatedly with tap water to remove dust and other sundries attached to the surface of the glutinous rice leaves, the rotten leaves are removed by manual screening, and the fresh glutinous rice leaves are cut to a length of 1-3 cm by using a shearing device commonly used in the food processing field, so as to facilitate subsequent processing. The glutinous rice leaves are conventional glutinous rice leaves in the art, and typically and non-limitingly, the glutinous rice leaves are selected from those planted in Pu'er City, Yunnan, Mengla County, Yunnan, or Hainan. The palm oil is conventional palm oil in the art, and typically and non-limitingly, the palm oil is 24-52° refined palm oil, selected from 24° food-grade palm oil sold by Hubei Qibaojiu Chemical Co., Ltd. or 52° food-grade hydrogenated palm oil sold by Kunshan Sheng'an Biological Technology Co., Ltd.

[0010] In the present application, freeze-drying and dehydration can eliminate a large amount of water contained in the glutinous rice leaves, avoid excessive water content, and prevent water-soluble components from entering the palm oil with water, thereby causing excessive water-soluble impurities and affecting the quality of the prepared glutinous rice leaf oil.

[0011] Grinding and pulping can destroy the cell structure of the glutinous rice leaves, release oil-soluble components in the glutinous rice leaves, and improve the extraction efficiency. The palm oil can dissolve the oil-soluble components and enrich the oil-soluble substances with fragrance.

[0012] According to the present application, the freeze-drying conditions include that the temperature for freeze-drying is-50℃ to-30℃, and the time for freeze-drying is 2-3h.

[0013] In the present application, when the freeze-drying conditions meet the above conditions, freeze-drying can fix the free water present in the leaves, and prevent irreversible changes such as foaming, contraction, concentration, and solute movement caused by the presence of free water during the drying process.

[0014] According to the present application, the dehydration includes first dehydration and second dehydration.

[0015] In the present application, the first dehydration can remove the free water in the leaves, and the second dehydration can remove the un-frozen bound water in the leaves.

[0016] According to the present application, the first dehydration conditions include that the vacuum degree for the first dehydration is 60-80Pa, the temperature for the first dehydration is 30-45℃, and the time for the first dehydration is 5-7h.

[0017] In the present application, when the first dehydration conditions meet the above ranges, the equipment load is small, the ice crystals can be quickly dehydrated by sublimation, good free water removal effect can be achieved, dehydration is sufficient, and energy is saved.

[0018] According to the application, the second dehydration conditions include: the vacuum degree of the second dehydration is 50-60 Pa, the temperature of the second dehydration is 30-40 DEG C, and the time of the second dehydration is 5-8 h.

[0019] In the application, when the second dehydration conditions meet the above range, the dehydration efficiency is high, the equipment load is small, the bound water in the leaf can be completely removed, the volatilization of the oil-soluble components is not caused, the good bound water removal effect can be obtained, and the oil-soluble components in the system are ensured.

[0020] In the application, the vacuum freeze drying equipment is a conventional instrument in the field, and typically and non-limitingly, the vacuum freeze drying equipment is HFD5L-0.5m3 / R vacuum freeze dryer of Shandong Kangbeitai Food Packaging Machinery Co., Ltd.

[0021] According to the application, the weight ratio of the glutinous rice leaf and the palm oil is 1:(1-5).

[0022] In the application, when the weight ratio of the glutinous rice leaf and the palm oil meets the above range, the excellent grinding effect is obtained, when the weight ratio of the glutinous rice leaf and the palm oil is greater than 1:1, the slurry flowability is poor in the grinding process, the grinding is insufficient, the oil-soluble components cannot be fully analyzed, and the extraction efficiency is low; when the weight ratio of the glutinous rice leaf and the palm oil is less than 1:5, the subsequent treatment is complex, and the palm oil is wasted.

[0023] According to the application, the first extraction includes: under the closed condition, the slurry obtained after the pulping is stirred, cooled and filtered and separated to obtain the first extraction liquid.

[0024] In the application, the closed environment comes from a closed heating equipment, and the closed heating equipment is a conventional equipment in the field, and typically and non-limitingly, the closed heating equipment includes a multifunctional electric heating extraction tank, an electric heating stirring and emulsifying tank, a stainless steel reaction kettle stirring tank or a stainless steel heating and stirring tank.

[0025] In the application, the glutinous rice leaf slurry is heated in the closed heating equipment, the oil-soluble components contained in the slurry are volatilized in the heating process, but are not lost due to volatilization, the stirring accelerates the dissolution of the oil-soluble components in the glutinous rice leaf in the palm oil, the cooling reduces the system temperature, at this time, the palm oil is still in a liquid state, and the oil-soluble components from the glutinous rice leaf are contained therein, and the first extraction can dissolve the oil-soluble components with fragrance in the glutinous rice leaf in the palm oil.

[0026] According to the application, the stirring conditions include: the temperature of the stirring is 30-60 DEG C, and the time of the stirring is 12-24 h.

[0027] In the present application, when the stirring condition meets the above range, the palm oil can dissolve the oil-soluble components and does not cause damage to the structure of the oil-soluble components, and has good extraction effect.

[0028] According to the present application, the cooling condition comprises: cooling to a temperature of 25-55℃.

[0029] In the present application, when the cooling temperature meets the above range, the oil-soluble components that overflow from the palm oil during heating can be dissolved in the palm oil again, and the palm oil is still in liquid state, and further processing can be carried out.

[0030] In the present application, the closed heating device is a conventional device in the field, and typically and non-limitingly, the closed heating device is selected from a multifunctional electric heating extraction tank, an electric heating stirring emulsification tank, a stainless steel reaction kettle stirring tank or a stainless steel heating stirring tank, for example, a multifunctional electric heating extraction tank sold by Changshu Chunlai Machinery Co., Ltd. under the trade name of DTQ0.5-6 series dynamic multifunctional extraction tank; an electric heating stirring emulsification tank sold by Guangzhou Maikao Machinery Co., Ltd. under the trade name of MK-JBG-1 food emulsification tank; a stainless steel reaction kettle stirring tank sold by Zhengzhou Fangyuan Instrument Technology Co., Ltd. under the trade name of BSF-30L electric heating double-layer stainless steel reaction kettle; and a stainless steel heating stirring tank sold by Dacheng County Hongsheng Steel and Aluminum Container Co., Ltd. under the trade name of stainless steel stirring tank.

[0031] In the present application, the filtering device is a conventional filtering device used in the technical field.

[0032] According to the present application, the second extraction comprises: extracting the first extraction liquid with an extractant, ultrasonic, freezing, filtering separation, taking the filtrate and repeating the operations of freezing and filtering separation to obtain the second extraction liquid.

[0033] In the present application, the second extraction can separate the oil-soluble components with fragrance from the palm oil to obtain the oil-soluble components dissolved in the extractant; the freezing can make the palm oil solidify at low temperature, and the extractant is still in liquid state, and the two are separated by filtering.

[0034] According to the present application, the volume ratio of the first extraction liquid to the extractant is 1:(1-10), preferably 1:(3-8).

[0035] In the present application, when the first extraction liquid and the extractant meet the above volume ratio, good extraction effect can be obtained; when the volume ratio of the first extraction liquid to the extractant is greater than 1:1, the extraction efficiency is low; and when the volume ratio of the first extraction liquid to the extractant is less than 1:10, too much extractant is used, the operation is complicated and waste is caused.

[0036] According to the present application, the extractant is selected from ethanol or N,N-dimethylacetamide triol.

[0037] In the present application, the ethanol is 95vol% ethanol, the N,N-dimethylacetamide triol is 95vol% N,N-dimethylacetamide triol, typically and non-limitingly, for example, the 95vol% ethanol product sold by Xinxiang Xinxing Biotechnology Co., Ltd. under the trade name of edible ethanol; the 95vol% N,N-dimethylacetamide triol sold by Hubei Kovod Chemical Co., Ltd. under the trade name of 95vol% double-dealcohol alcohol.

[0038] According to the present application, the extraction conditions include: the extraction temperature is 30-60℃, preferably 38-50℃, and the extraction time is 1-2h, preferably 1.2-1.8h.

[0039] In the present application, when the extraction conditions meet the above range, the palm oil can be fully contacted with the extractant, and has good extraction effect.

[0040] According to the present application, the ultrasonic conditions include: the ultrasonic power is 400-800W, preferably 500-700W; the ultrasonic temperature is 30-60℃, preferably 36-54℃; and the ultrasonic time is 15-30min, preferably 18-26min.

[0041] In the present application, when the ultrasonic meets the above range, good physical shock and cavitation effect can be provided, the palm oil has good fluidity and does not accumulate in the equipment, and the extraction effect is enhanced, typically and non-limitingly, the equipment used is a dynamic countercurrent ultrasonic equipment, for example, the product sold by Jining Jinbaitie Biomechanical Co., Ltd. under the trade name of TNC1-300 single-stage continuous countercurrent reflux ultrasonic extraction machine.

[0042] According to the present application, the freezing conditions include: the freezing temperature is-5℃ to 0℃, and the freezing time is 6-12h.

[0043] In the present application, when the freezing conditions meet the above range, good freezing effect is obtained, the palm oil can be completely solidified, and energy is saved.

[0044] According to the present application, the number of repetitions is 2-5 times.

[0045] In the present application, the repetition is to more fully remove the palm oil in the system.

[0046] According to the present application, the concentration is reduced pressure concentration.

[0047] In the present application, the concentration equipment used is a conventional equipment in the art, typically and non-limitingly, the concentration equipment sold by Sichuan Taide Pharmaceutical Equipment Co., Ltd. under the trade name of spherical concentrator.

[0048] According to the application, the concentration condition includes: the concentration temperature is 30-40 DEG C, and the concentration pressure is -0.07MPa to -0.02MPa.

[0049] In the application, when the concentration condition meets the above range, the extractant removal is more sufficient, the separation effect of the extractant is good, the efficiency is high, the equipment load is small, and the energy is saved.

[0050] The application also discloses a preparation method of the waxy rice leaf oil.

[0051] According to the application, the waxy rice leaf oil comprises 2-propionyl-3,4,5,6-tetrahydropyridine, 2-propionyl-1,4,5,6-tetrahydropyridine, 2-acetyl-3,4,5,6-tetrahydropyridine and water.

[0052] According to the application, the content of 2-propionyl-3,4,5,6-tetrahydropyridine is 1-3wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 1-2wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.1-0.5wt%, and the content of water is 0.1wt% or less, based on the weight of the waxy rice leaf oil.

[0053] The application also discloses a use of the waxy rice leaf oil in a filter rod bursting bead for cigarettes.

[0054] According to the application, the content of the waxy rice leaf oil is 0.01-10wt%, based on the weight of the filter rod bursting bead for cigarettes.

[0055] In the application, when the content of the waxy rice leaf oil meets the above range, based on the weight of the filter rod bursting bead for cigarettes, the flavor is appropriate, and the cost is low.

[0056] The technical scheme of the application has the following advantages:

[0057] 1. The application provides a preparation method of waxy rice leaf oil, which overcomes the problem that the waxy rice aroma in the existing waxy rice aroma type tobacco product is derived from waxy rice, and comprises the following steps: freezing and drying waxy rice leaves, mixing and grinding the waxy rice leaves with palm oil to prepare pulp, performing first extraction and second extraction, and finally concentrating to obtain waxy rice leaf oil. The preparation method is simple, safe and environmentally friendly, the raw materials are easy to obtain, and industrial production can be realized. In the application, through the synergistic effect of the multiple steps of freezing and drying, mixing and grinding the waxy rice leaves with palm oil to prepare pulp, performing first extraction, second extraction and concentration, the waxy rice leaves can be fully extracted, and waxy rice leaf oil which can be preserved and is not prone to corruption is prepared. When the waxy rice leaf oil is applied in cigarettes, it can impart waxy rice aroma to tobacco products and enrich the aroma characteristics of tobacco products; its aroma characteristics are coordinated with the style of cigarettes, significantly reducing the offensive odor and irritation of cigarettes, and enhancing the aroma and aftertaste of cigarettes as a whole.

[0058] 2. Freezing and drying can eliminate a large amount of water contained in the waxy rice leaves, avoid excessive water content, and prevent water-soluble components from entering the palm oil with water; the waxy rice leaf oil prepared has low impurity content and long storage time, and when the waxy rice leaf oil is applied in cigarettes, the aroma is harmonious, the offensive odor and irritation are low, and the aftertaste is pure and long.

[0059] 3. Grinding to prepare pulp can destroy the cell structure of the waxy rice leaves, release oil-soluble components in the waxy rice leaves, and improve the extraction efficiency; the palm oil can dissolve the oil-soluble components and increase the aroma concentration of the extract; when the waxy rice leaf oil is applied in cigarettes, the aroma is harmonious, the offensive odor and irritation are low, and the aftertaste is pure and long.

[0060] 4. The first extraction can dissolve the oil-soluble components with aroma in the waxy rice leaves in the palm oil; the second extraction can separate the oil-soluble components with aroma from the palm oil to obtain oil-soluble components dissolved in the extraction solvent; when the waxy rice leaf oil is applied in cigarettes, the aroma is harmonious, the offensive odor and irritation are low, and the aftertaste is pure and long. DETAILED DESCRIPTION

[0061] The following examples are provided to better further understand the application and are not limited to the best mode of the application, and do not constitute a limitation on the content and scope of protection of the application. Any person under the inspiration of the application or the combination of the application with other prior art features can obtain any product identical or similar to the application, which falls within the protection scope of the application.

[0062] If the specific experimental steps or conditions are not specified in the examples, the operations or conditions can be performed according to the conventional experimental steps described in the literature in the art. If the reagents or instruments are not specified by the manufacturer, they are conventional reagent products that can be obtained by purchase.

[0063] The content of organic components in the waxy rice leaf oil is tested by GC / MS testing method. Specifically, 1 g of waxy rice leaf oil is uniformly mixed with 9 g of methanol, filtered, and then detected and analyzed by GC / MS gas chromatography-mass spectrometry instrument to obtain a component spectrum, screen a target spectrum, and calculate the content of organic components by computer. The content calculation formula is: organic component content (%) = organic component determination amount / total mass of waxy rice leaf oil x 100.

[0064] The water content in the waxy rice leaf oil is tested by Karl Fischer water determination method. Specifically, 50 mL of methanol is taken in a Karl Fischer water determination instrument reactor, and Karl Fischer reagent is titrated until the pointer is equivalent to the calibration and remains unchanged for 1 min. Then, the sample to be tested is added, stirred, and then Karl Fischer reagent is added to the end point. The reaction is considered to be completed when the color remains unchanged for 1 min. The water content (%) = water equivalent of Karl Fischer reagent x Karl Fischer reagent consumed by titration / weight of sample to be tested x 100.

[0065] The test method for the degree of spoilage of waxy rice leaf oil is to calculate by testing the peroxide value. 2 g of waxy rice leaf oil is added to 30 mL of mixture, 1 mL of saturated potassium iodide solution is added, and it is placed in the dark for 3 min. Then, 50 mL of distilled water is added, and 0.01 mol / L sodium thiosulfate is titrated to light yellow. Then, 1 mL of starch indicator is added, and the titration is continued until the blue color disappears. At the same time, a blank control is performed. The degree of spoilage (%) = (volume of sodium thiosulfate solution consumed by the sample - volume of sodium thiosulfate consumed by the control) x equivalent concentration of sodium thiosulfate x 0.1269 / oil sample weight x 100, wherein 0.1269 is the number of grams of iodine corresponding to 1 mg equivalent of sodium thiosulfate.

[0066] The waxy rice leaf is purchased from Wukui Food (Shenzhen) Co., Ltd. and is planted in Mengla County, Yunnan.

[0067] The palm oil is purchased from Hubei Qibaoji Chemical Co., Ltd. and is a 24° food-grade palm oil.

[0068] Example 1

[0069] This example provides a preparation method of waxy rice leaf oil. The specific preparation steps and operation parameters are as follows:

[0070] A. Preparation of waxy rice leaf slurry

[0071] The fresh waxy rice leaves are washed, rotten leaves are removed, and the waxy rice leaves are cut into 1 cm long. The waxy rice leaves are frozen in a HFD5L-0.5m³ / R vacuum freeze dryer at a freezing temperature of -30℃ for 2.6h, then first dehydrated at a vacuum degree of 76Pa and a dehydration temperature of 36℃ for 6.6h, and then second dehydrated at a vacuum degree of 50Pa and a dehydration temperature of 32℃ for 5.6h. The dehydrated waxy rice leaves are mixed and ground with palm oil at a weight ratio of 1:4 to obtain waxy rice leaf slurry A1.

[0072] B, first extraction

[0073] The waxy rice leaf slurry A1 is stirred in a multifunctional electric heating extraction tank sealed freezing equipment at a temperature of 48℃ for 16h, and then cooled to a temperature of 20℃. Filtration separation is performed to obtain a filtrate as a first extraction liquid B1.

[0074] C, second extraction

[0075] The first extraction liquid B1 is extracted at a volume ratio of 1:8 of the first extraction liquid B1 to 95vol% ethanol, an extraction temperature of 42℃, and an extraction time of 1.4h. Then, a TNC1-300 single-stage continuous countercurrent reflux ultrasonic extractor is used at a temperature of 42℃ and an ultrasonic power of 400W for 27min to obtain an extraction liquid. The extraction liquid is frozen at a temperature of 0℃ for 9h, and filtration separation is performed. After repeating the freezing and filtration separation operations 4 times, a filtrate is obtained as a second extraction liquid C1.

[0076] D, concentration

[0077] The second extraction liquid C1 is concentrated in a concentration equipment at a temperature of 38℃ and a pressure of -0.07MPa to obtain waxy rice leaf oil D1.

[0078] Based on the weight of the waxy rice leaf oil D1, the content of 2-propionyl-3,4,5,6-tetrahydropyridine is 1.41wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 1.13wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.12wt%, and the content of water is 0.06wt%. After being placed for 90 days, the degree of corruption is 0.03%.

[0079] Based on the weight of the filter rod burst beads for cigarettes, the amount of the waxy rice leaf oil is 0.01wt%. Cigarettes prepared from the filter rod burst beads for cigarettes are evaluated, and the results are shown in Table 1.

[0080] Example 2

[0081] The embodiment provides a preparation method of waxy rice leaf oil, and specific preparation steps and operation parameters are as follows.

[0082] A. Preparation of waxy rice leaf slurry

[0083] Fresh waxy rice leaves are washed, rotten leaves are removed, and the waxy rice leaves are cut into leaves with a length of 3 cm; the waxy rice leaves are frozen in an HFD5L-0.5m³ / R vacuum freeze dryer at a freezing temperature of-30°C for 2h, and then subjected to first dehydration under conditions of a vacuum degree of 60Pa and a dehydration temperature of 42°C for 7h; then, the waxy rice leaves are subjected to second dehydration in the vacuum freeze dryer under conditions of a vacuum degree of 58Pa and a dehydration temperature of 34°C for 6.2h, and then mixed and ground with palm oil at a weight ratio of 1:1 to prepare a waxy rice leaf slurry A2.

[0084] B. First extraction

[0085] The waxy rice leaf slurry A2 is stirred in a multifunctional electric heating extraction tank airtight freezing equipment at a temperature of 54°C for 16h, and then cooled to a temperature of 25°C, filtered and separated, to obtain a filtrate as a first extraction liquid B2.

[0086] C. Second extraction

[0087] The first extraction liquid B2 is extracted, the first extraction liquid B2 and 95vol% N,N-dimethylacetamide triol are mixed at a volume ratio of 1:10, the extraction temperature is 48°C, and the extraction time is 1.6h; then, the TNC1-300 single-stage continuous countercurrent reflux ultrasonic extractor is used to ultrasonically treat the mixture at a temperature of 48°C and an ultrasonic power of 800W for 30min, the obtained extraction liquid is frozen at a temperature of 0°C for 8h, filtered and separated, the filtrate is repeatedly frozen, filtered and separated for 3 times, and the obtained filtrate is a second extraction liquid C2.

[0088] D. Concentration

[0089] The second extraction liquid C2 is concentrated in a concentration equipment under reduced pressure at a temperature of 40°C and a pressure of-0.06MPa, to obtain waxy rice leaf oil D2.

[0090] The content of 2-propionyl-3,4,5,6-tetrahydropyridine is 2.31wt% based on the weight of the waxy rice leaf oil D2, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 1.33wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.35wt%, and the content of water is 0.05wt%, and the degree of corruption is 0.08% after being placed for 90 days.

[0091] The amount of the fragrant leaf oil of the waxy rice is 3wt% based on the weight of the filter rod burst beads, and the filter rod burst beads are used to prepare cigarettes, and the cigarettes are tasted, and the results are shown in Table 1.

[0092] Example 3

[0093] The embodiment provides a preparation method of a fragrant leaf oil of waxy rice, and specific preparation steps and operation parameters are as follows.

[0094] A, preparation of waxy rice fragrant leaf slurry

[0095] Fresh fragrant leaves of waxy rice are washed, rotten leaves are removed, and the fragrant leaves of waxy rice are cut into 2cm in length; the fragrant leaves of waxy rice are frozen in a HFD5L-0.5m³ / R vacuum freeze dryer at a freezing temperature of-30℃ for 2.4h, then first dehydration is performed at a vacuum degree of 64Pa and a dehydration temperature of 45℃ for 5h, then second dehydration is performed at a vacuum degree of 56Pa and a dehydration temperature of 36℃ for 5h in the vacuum freeze dryer, and the dehydrated fragrant leaves of waxy rice are mixed and ground with palm oil at a weight ratio of 1:3 to prepare a fragrant leaf slurry A3 of waxy rice.

[0096] B, first extraction

[0097] The fragrant leaf slurry A3 of waxy rice is stirred in a multifunctional electric heating extraction tank airtight freezing equipment at a temperature of 30℃ for 24h, and then cooled to a temperature of 23℃, filtered and separated, and the obtained filtrate is a first extraction liquid B3;

[0098] C, second extraction

[0099] The first extraction liquid B3 is extracted, the volume ratio of the first extraction liquid B3 to 95vol% ethanol is 1:5, the extraction temperature is 53℃, and the extraction time is 1h, then a TNC1-300 single-stage continuous countercurrent reflux ultrasonic extractor is used, the extraction is performed at a temperature of 54℃ and an ultrasonic power of 550W for 18min, the obtained extraction liquid is frozen at a temperature of 0℃ for 11h, filtered and separated, the filtrate is repeatedly frozen, filtered and separated for 2 times, and the obtained filtrate is a second extraction liquid C3;

[0100] D, concentration

[0101] The second extraction liquid C3 is concentrated in a concentration equipment at a temperature of 34℃ and a pressure of-0.04MPa, and the fragrant leaf oil D3 of waxy rice is obtained.

[0102] The content of 2-propionyl-3,4,5,6-tetrahydropyridine is 2.37wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 1.51wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.36wt%, and the content of water is 0.04wt%, based on the weight of the rice leaf oil D3, and the degree of corruption is 0.05% after being placed for 90 days.

[0103] The amount of the rice leaf oil is 1wt% based on the weight of the filter plug of a smoking article, and the filter plug of a smoking article prepared by the rice leaf oil is tasted, and the results are shown in Table 1.

[0104] Example 4

[0105] The present embodiment provides a preparation method of a rice leaf oil, and the specific preparation steps and operation parameters are as follows:

[0106] A, preparation of rice leaf slurry

[0107] Fresh rice leaf is washed, rotten leaves are removed, and the rice leaf is cut into 2cm long; the rice leaf is frozen in a HFD5L-0.5m³ / R vacuum freeze dryer at a freezing temperature of-30℃ for 3h, then first dehydration is performed at a vacuum degree of 80Pa and a dehydration temperature of 30℃ for 5.8h, then second dehydration is performed at a vacuum degree of 60Pa and a dehydration temperature of 38℃ for 8h, and the dehydrated rice leaf is mixed and ground with palm oil at a weight ratio of 1:2 to prepare a rice leaf slurry A4.

[0108] B, first extraction

[0109] The rice leaf slurry A4 is stirred in a multifunctional electric heating extraction tank airtight freezing equipment at a temperature of 36℃ for 21h, then cooled to a temperature of 20℃, and filtered and separated to obtain a filtrate as a first extraction liquid B4;

[0110] C, second extraction

[0111] The first extraction liquid B4 is extracted, the volume ratio of the first extraction liquid B4 to 95vol% N,N-dimethylacetamide triol is 1:8, the extraction temperature is 60℃, and the extraction time is 1.2h, then a TNC1-300 single-stage continuous countercurrent reflux ultrasonic extraction machine is used at a temperature of 60℃ and an ultrasonic power of 500W for 21min, the obtained extraction liquid is frozen at a temperature of 0℃ for 6h, filtered and separated, the filtrate is repeatedly frozen, filtered and separated for 3 times, and the obtained filtrate is a second extraction liquid C4;

[0112] D, concentration

[0113] The second extraction liquid C4 was concentrated in a concentration device under reduced pressure, with a temperature of 30°C and a pressure of -0.03 MPa, to obtain glutinous rice leaf oil D4.

[0114] The content of 2-propionyl-3,4,5,6-tetrahydropyridine was 1.42 wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine was 1.21 wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine was 0.32 wt%, and the content of water was 0.08 wt%, based on the weight of the glutinous rice leaf oil D4. The glutinous rice leaf oil was placed for 90 days, and the degree of corruption was 0.07%.

[0115] The amount of the glutinous rice leaf oil was 10 wt% based on the weight of the filter plug of the cigarette, and the cigarette prepared from the filter plug was tasted, and the results are shown in Table 1.

[0116] Example 5

[0117] The present embodiment provides a preparation method of glutinous rice leaf oil, and the specific preparation steps and operation parameters are as follows:

[0118] A. Preparation of glutinous rice leaf slurry

[0119] Fresh glutinous rice leaves were washed, rotten leaves were removed, and the glutinous rice leaves were cut into 1 cm long. The glutinous rice leaves were frozen in a HFD5L-0.5m³ / R vacuum freeze dryer at a freezing temperature of -30°C for 2.8 h, then first dehydrated at a vacuum degree of 68 Pa and a dehydration temperature of 39°C for 6.2 h, and then second dehydrated at a vacuum degree of 52 Pa and a dehydration temperature of 30°C for 6.8 h in the vacuum freeze dryer. The dehydrated glutinous rice leaves were mixed and ground with palm oil at a weight ratio of 1:5 to prepare a glutinous rice leaf slurry A5.

[0120] B. First extraction

[0121] The glutinous rice leaf slurry A5 was stirred in a multifunctional electric heating extraction tank in a closed freezing device at a temperature of 42°C for 18 h, and then cooled to a temperature of 20°C. The obtained filtrate was a first extraction liquid B5.

[0122] C. Second extraction

[0123] The first extraction liquid B5 is extracted with 95vol% N,N-dimethylacetamide triol at a volume ratio of 1:4, the extraction temperature is 30°C, the extraction time is 1.8h, then the TNC1-300 single-stage continuous countercurrent reflux ultrasonic extraction machine is used, the temperature is 30°C, the ultrasonic power is 700W, the ultrasonic time is 24min, the obtained extraction liquid is frozen at a temperature of 0°C for 7h, filtration separation is carried out, the filtrate is repeatedly frozen and filtration separation for 4 times, and the obtained filtrate is a second extraction liquid C5.

[0124] D, concentration

[0125] The second extraction liquid C5 is subjected to vacuum concentration in a concentration device, the temperature is 32°C, the pressure is-0.02MPa, and the waxy leaf oil D5 is obtained.

[0126] The content of 2-propionyl-3,4,5,6-tetrahydropyridine is 1.21wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 1.02wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.31wt%, and the content of water is 0.02wt% based on the weight of the waxy leaf oil D5, and the waxy leaf oil is placed for 90 days, and the degree of corruption is 0.06%.

[0127] The amount of the waxy leaf oil is 8wt% based on the weight of the filter plug of the cigarette, and the cigarette prepared from the filter plug is tasted, and the results are shown in Table 1.

[0128] Example 6

[0129] The embodiment provides a preparation method of a waxy leaf oil, and specific preparation steps and operation parameters are as follows:

[0130] A, preparation of waxy leaf slurry

[0131] Fresh waxy leaf is washed, rotten leaves are removed, and the waxy leaf is cut into a length of 3cm; the waxy leaf is frozen in an HFD5L-0.5m³ / R vacuum freeze dryer at a freezing temperature of-30°C for 2.2h, is subjected to first dehydration at a vacuum degree of 72Pa and a dehydration temperature of 33°C for 5.4h, is subjected to second dehydration at a vacuum degree of 54Pa and a dehydration temperature of 40°C for 7.4h in the vacuum freeze dryer, and is mixed and ground with palm oil at a weight ratio of 1:3 to prepare a waxy leaf slurry A6.

[0132] B, first extraction

[0133] The waxy rice leaf paste A6 was stirred in a multifunctional electric heating extraction tank closed freezing equipment at a temperature of 60°C for 12 h, and then cooled to a temperature of 22°C. The filtrate obtained by filtration separation was the first extraction liquid B6.

[0134] C. Second extraction

[0135] The first extraction liquid B6 was extracted at a volume ratio of 1:6 of the first extraction liquid B6 to 95 vol% N,N-dimethylacetamide triol, an extraction temperature of 37°C, and an extraction time of 2 h. Then, using a TNC1-300 single-stage continuous countercurrent reflux ultrasonic extraction machine, ultrasonic extraction was performed at a temperature of 38°C and an ultrasonic power of 600 W for 15 min. The obtained extraction liquid was frozen at a temperature of 0°C for 12 h, and then filtered and separated. After repeating the freezing and filtration separation operation 5 times, the filtrate obtained was the second extraction liquid C6.

[0136] D. Concentration

[0137] The second extraction liquid C6 was concentrated under reduced pressure in a concentration equipment at a temperature of 36°C and a pressure of -0.05 MPa to obtain the waxy rice leaf oil D6.

[0138] Based on the weight of the waxy rice leaf oil D6, the content of 2-propionyl-3,4,5,6-tetrahydropyridine was 2.02 wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine was 1.25 wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine was 0.18 wt%, and the content of water was 0.1 wt%. After being placed for 90 days, the degree of corruption was 0.09%.

[0139] Based on the weight of the filter plug of the filter rod, the amount of the waxy rice leaf oil used was 1 wt%. The cigarettes prepared from the filter plug of the filter rod were evaluated, and the results are shown in Table 1.

[0140] Example 7

[0141] The present embodiment provides a preparation method of a waxy rice leaf oil, and the specific preparation steps and operation parameters are as follows:

[0142] In the same manner as in Example 1, except that in Step A, "dehydration was performed at a vacuum of 50 Pa and a dehydration temperature of 32°C for 11.2 h" was used in place of "first dehydration was performed at a vacuum of 76 Pa and a dehydration temperature of 36°C for 6.6 h, and then second dehydration was performed at a vacuum of 50 Pa and a dehydration temperature of 32°C for 5.6 h in the vacuum freeze drying apparatus," to obtain a leaf of canna indica oil D7, the content of 2-propionyl-3,4,5,6-tetrahydropyridine was 1.05 wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine was 1.01 wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine was 0.1 wt%, and the content of water was 0.1 wt% based on the weight of the leaf of canna indica oil D7, and the leaf of canna indica oil D7 was left to stand for 90 days, and the degree of spoilage was 0.09%.

[0143] The amount of the leaf of canna indica oil was 0.01 wt% based on the weight of the filter plug of a cigarette, and the cigarette prepared from the filter plug of a cigarette was tasted, and the results are shown in Table 1.

[0144] Example 8

[0145] The present example provides a preparation method of a leaf of canna indica oil, and the specific preparation steps and operation parameters are as follows:

[0146] In the same manner as in Example 1, except that in Step A, "the weight ratio of the dehydrated leaf of canna indica to palm oil was 2:1" was used in place of "the weight ratio of the dehydrated leaf of canna indica to palm oil was 1:4" to obtain a leaf of canna indica oil D8, the content of 2-propionyl-3,4,5,6-tetrahydropyridine was 1.0 wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine was 0.9 wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine was 0.07 wt%, and the content of water was 0.8 wt% based on the weight of the leaf of canna indica oil D8, and the leaf of canna indica oil D8 was left to stand for 90 days, and the degree of spoilage was 1.2%.

[0147] The amount of the leaf of canna indica oil was 0.01 wt% based on the weight of the filter plug of a cigarette, and the cigarette prepared from the filter plug of a cigarette was tasted, and the results are shown in Table 1.

[0148] Example 9

[0149] The present example provides a preparation method of a leaf of canna indica oil, and the specific preparation steps and operation parameters are as follows:

[0150] In the same manner as in Example 1 except that in Step C, "the extraction liquid obtained under the conditions of ultrasonic power 400 W at a temperature of 42℃ for 27 min was filtered, and the filtrate was repeatedly frozen and filtered for separation 4 times" was used to replace "the extraction liquid obtained under the conditions of ultrasonic power 400 W at a temperature of 42℃ for 27 min was frozen at a temperature of 0℃ for 9 h, and then filtered and separated, and the filtrate was repeatedly frozen and filtered for separation 4 times", a patchouli oil D9 was obtained, the content of 2-propionyl-3,4,5,6-tetrahydropyridine was 0.4wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine was 0.8wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine was 0.07wt%, and the content of water was 0.3wt% based on the weight of the patchouli oil D9, and the degree of corruption was 0.13% after being placed for 90 days.

[0151] The amount of the patchouli oil was 0.1wt% based on the weight of the filter plug of the cigarette, and the cigarette prepared from the filter plug was tasted, and the results are shown in Table 1.

[0152] Comparative Example 1

[0153] The present comparative example provides a preparation method of a patchouli oil, and the specific preparation steps and operation parameters are as follows:

[0154] In the same manner as in Example 1 except that in Step A, "the fresh patchouli leaves were washed, and the rotten leaves were removed, and the patchouli leaves were cut into 1cm long, and then the first dehydration was performed under the conditions of a vacuum degree of 76Pa and a dehydration temperature of 36℃" was used to replace "the fresh patchouli leaves were washed, and the rotten leaves were removed, and the patchouli leaves were cut into 1cm long, and then the patchouli leaves were frozen in a HFD5L-0.5m³ / R vacuum freeze dryer under the conditions of a freezing temperature of -30℃ for 2.6h, and then the first dehydration was performed under the conditions of a vacuum degree of 76Pa and a dehydration temperature of 36℃", a patchouli oil DD1 was obtained, the content of 2-propionyl-3,4,5,6-tetrahydropyridine was 0.5wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine was 0.2wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine was 0.06wt%, and the content of water was 0.54wt% based on the weight of the patchouli oil DD1, and the degree of corruption was 0.41% after being placed for 90 days.

[0155] The amount of the patchouli oil was 0.1wt% based on the weight of the filter plug of the cigarette, and the cigarette prepared from the filter plug was tasted, and the results are shown in Table 1.

[0156] Comparative Example 2

[0157] The present comparative example provides a preparation method of waxy rice leaf oil, and specific preparation steps and operation parameters are as follows:

[0158] A, preparation of waxy rice leaf slurry

[0159] The fresh waxy rice leaf is washed, rotten leaves are removed, and the waxy rice leaf is cut into 1 cm long; the waxy rice leaf is frozen in a HFD5L-0.5m³ / R vacuum freeze dryer at a freezing temperature of-30℃ for 2.6h, then first dehydration is performed at a vacuum degree of 76Pa and a dehydration temperature of 36℃ for 6.6h, then second dehydration is performed in the vacuum freeze dryer at a vacuum degree of 50Pa and a dehydration temperature of 32℃ for 5.6h, and the dehydrated waxy rice leaf is mixed and ground with palm oil at a weight ratio of 1:4 to prepare a waxy rice leaf slurry DA2.

[0160] B, extraction

[0161] The waxy rice leaf slurry DA2 is extracted, the volume ratio of the waxy rice leaf slurry DA2 to 95vol% ethanol is 1:8, the extraction temperature is 42℃, and the extraction time is 1.4h, then a TNC1-300 single-stage continuous countercurrent reflux ultrasonic extraction machine is used for ultrasonic extraction at a temperature of 42℃ and an ultrasonic power of 400W for 27min, the obtained extraction liquid is frozen at a temperature of 0℃ for 9h, filtration separation is performed, and after the filtration separation operation is repeated 4 times, the obtained filtrate is an extraction liquid DB2.

[0162] C, concentration

[0163] The extraction liquid DB2 is concentrated in a concentration device at a temperature of 38℃ and a pressure of-0.07MPa, the content of 2-propionyl-3,4,5,6-tetrahydropyridine is 0.7wt% based on the weight of the waxy rice leaf oil DC2, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 0.4wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.04wt%, and the content of water is 0.29wt%, the product is placed for 90 days, and the degree of corruption is 0.34%.

[0164] The amount of the waxy rice leaf oil is 0.1wt% based on the weight of the filter plug of a cigarette filter rod, and the cigarette prepared from the filter plug of the cigarette filter rod is tasted, and the results are shown in Table 1.

[0165] Comparative example 3

[0166] The present comparative example provides a preparation method of waxy rice leaf oil, and specific preparation steps and operation parameters are as follows:

[0167] A, preparation of waxy rice leaf slurry

[0168] Fresh glutinous rice leaf is washed, rotten leaves are removed, and the glutinous rice leaf is cut into 1 cm in length; the glutinous rice leaf is frozen in a HFD5L-0.5m³ / R vacuum freeze-drying machine at a freezing temperature of -30°C for 2.6 h, and then first dehydration is performed at a vacuum degree of 76 Pa and a dehydration temperature of 36°C for 6.6 h, and then second dehydration is performed at a vacuum degree of 50 Pa and a dehydration temperature of 32°C for 5.6 h in the vacuum freeze-drying machine, and the dehydrated glutinous rice leaf is mixed and ground with palm oil at a weight ratio of 1:4 to obtain glutinous rice leaf pulp DA3.

[0169] B. Extraction

[0170] The glutinous rice leaf pulp A1 is stirred in a multifunctional electric heating extraction tank sealed freezing equipment at a temperature of 48°C for 16 h, and then cooled to a temperature of 20°C, filtered and separated, and the obtained filtrate is an extract DB3;

[0171] C. Concentration

[0172] The extract DB3 is concentrated in a concentration equipment under reduced pressure at a temperature of 38°C and a pressure of -0.07 MPa, and the content of 2-propionyl-3,4,5,6-tetrahydropyridine is 0.9 wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 0.1 wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.09 wt%, and the content of water is 0.3 wt% based on the weight of the glutinous rice leaf oil DC3, and the degree of corruption is 0.19% after being placed for 90 days.

[0173] The amount of the glutinous rice leaf oil is 0.1 wt% based on the weight of the filter plug of the filter rod, and the cigarettes prepared from the filter plug of the filter rod are evaluated, and the results are shown in Table 1.

[0174] The cigarettes including the filter plug of the filter rod prepared from the glutinous rice leaf oil of the example and the comparative example are evaluated, and the specific evaluation method is that an evaluation group consisting of 7 evaluators is organized according to GB 5606.4-2005 Cigarettes Part 4: Sensory Technical Requirements, and the evaluation results are shown in Table 1.

[0175] The control group is the cigarettes prepared from the filter plug of the filter rod without adding the glutinous rice leaf oil.

[0176] Table 1

[0177]

[0178] Table 1 (continued)

[0179]

[0180] Table 1 (continued)

[0181]

[0182] Table 1 (continued)

[0183]

[0184] The present application overcomes the current situation that the glutinous rice aroma in existing glutinous rice aroma type tobacco products comes from extraction of glutinous rice, adopts glutinous rice leaf for extraction, and obtains a material with glutinous rice aroma, and the preparation method is simple, safe and environmentally friendly, raw materials are easy to obtain, and industrial production can be realized.

[0185] As can be seen from the above examples, the glutinous rice leaf oil prepared by the preparation method of the present application has good storage stability and is not prone to corruption, and when applied in cigarettes, it can improve the sensory quality of the cigarettes, significantly improve the aroma quality of the cigarettes compared with the blank control group, impart the cigarettes with the aroma flavor of glutinous rice, in addition, the aroma characteristics thereof are coordinated with the style of the cigarettes, the aftertaste is pure, the offensive odor and irritation of the cigarettes are obviously reduced, and the overall aroma quality of the cigarettes is enhanced.

[0186] As can be seen from the comparison of Example 1 and Example 7, a specific number of dehydration enables the glutinous rice leaf oil to have a specific content of ingredients, and when applied in cigarettes, it improves the nature of tobacco products, the aroma is harmonious, the aftertaste is pure, and the offensive odor and irritation are small.

[0187] As can be seen from the comparison of Example 1 and Example 8, the preparation method of the present application can successfully prepare the pulp on the basis of reducing waste, and realizes green and environmentally friendly preparation process.

[0188] As can be seen from the comparison of Example 1 and Example 9, after extraction, the palm oil is used for high-temperature dissolution and low-temperature cooling, and through temperature adjustment, the glutinous rice leaf oil is successfully separated from the palm oil and dissolved in a non-polluting and convenient-to-handle extraction agent, and when the glutinous rice leaf oil of the present application is applied in cigarettes, the aroma is harmonious, the offensive odor and irritation are small, and the aftertaste is pure and long.

[0189] As can be seen from the comparison of Example 1 and Comparative Example 1, freeze-drying can eliminate a large amount of water in the glutinous rice leaf, prevent water-soluble ingredients from entering the palm oil with water, and cause the content of water-soluble impurities to be too high, and when the glutinous rice leaf oil of the present application is applied in cigarettes, the aroma is harmonious, the offensive odor and irritation are small, and the aftertaste is pure and long.

[0190] Comparing example 1 with comparative example 2, the first extraction makes the oil-soluble components in the waxy rice leaf slurry to be separated and dissolved in palm oil again, realizing purification of the waxy rice leaf oil; comparing example 1 with comparative example 3, the synergistic effect of extraction, ultrasonic, freezing and filtration separation can further improve the purity of the nano rice leaf oil, and the waxy rice leaf oil of the application has the advantages of harmonious flavor, less miscellaneous odor and stimulation, and pure and long-lasting aftertaste when applied in cigarettes.

[0191] Obviously, the above examples are only examples for clearly illustrating but not limiting the embodiments. Based on the above description, other different forms of changes or variations can be made by those skilled in the art. Here, all the embodiments are not required to be exhausted, and the obvious changes or variations derived therefrom are still within the protection scope of the present application.

Claims

1. A process for the preparation of glutinous rice leaf oil characterized in that, The preparation method comprises the following steps: The glutinous rice leaf is freeze-dried and dehydrated, mixed with palm oil, ground into pulp, and then extracted for the first time and the second time, and finally concentrated to obtain glutinous rice leaf oil; The dehydration comprises first dehydration and second dehydration; The first dehydration comprises the following conditions: the vacuum degree of the first dehydration is 60-80 Pa, the temperature of the first dehydration is 30-45 DEG C, and the time of the first dehydration is 5-7 h; The second dehydration comprises the following conditions: the vacuum degree of the second dehydration is 50-60 Pa, the temperature of the second dehydration is 30-40 DEG C, and the time of the second dehydration is 5-8 h; The first extraction comprises the following steps: under a closed condition, the pulp obtained after the pulp preparation is stirred, cooled and filtered to obtain a first extraction liquid; The second extraction comprises the following steps: the first extraction liquid is extracted with an extractant, then ultrasonic, frozen, filtered and separated, and the filtrate is repeatedly frozen and filtered to obtain a second extraction liquid.

2. The production method according to claim 1, characterized by, The freeze-drying conditions comprise the following: the temperature of the freeze-drying is-50 DEG C to-30 DEG C, and the time of the freeze-drying is 2-3 h.

3. The production method according to claim 1 or 2, characterized by, The weight ratio of the glutinous rice leaf to the palm oil is 1:(1-5).

4. The production method according to claim 1, characterized by, The stirring conditions comprise the following: the temperature of the stirring is 30-60 DEG C, and the time of the stirring is 12-24 h; And / or, the cooling conditions comprise the following: the temperature is cooled to 25-55 DEG C.

5. The preparation method according to claim 1, characterized in that, The volume ratio of the first extraction liquid to the extractant is 1:(1-10); And / or, the extractant is selected from ethanol or N, N-dimethylacetamide triol; And / or, the extraction conditions comprise the following: the temperature of the extraction is 30-60 DEG C, and the time of the extraction is 1-2 h; And / or, the ultrasonic conditions comprise the following: the ultrasonic power is 400-800 W, the temperature of the ultrasonic is 30-60 DEG C, and the time of the ultrasonic is 15-30 min; And / or, the freezing conditions comprise the following: the temperature of the freezing is-5 DEG C to 0 DEG C, and the time of the freezing is 6-12 h; And / or, the number of repetitions is 2-5 times.

6. The preparation method according to claim 5, characterized in that, The volume ratio of the first extraction liquid to the extractant is 1:(3-8); And / or, the extraction conditions comprise the following: the temperature of the extraction is 38-50 DEG C, and the time of the extraction is 1.2-1.8 h; And / or, the ultrasonic conditions comprise the following: the ultrasonic power is 500-700 W, the temperature of the ultrasonic is 36-54 DEG C, and the time of the ultrasonic is 18-26 min; And / or, the freezing conditions comprise the following: the temperature of the freezing is-5 DEG C to 0 DEG C, and the time of the freezing is 6-12 h.

7. The preparation method according to claim 1, characterized in that, The concentration is reduced pressure concentration.

8. The production method according to claim 7, characterized by, The concentration conditions comprise the following: the temperature of the concentration is 30-40 DEG C, and the pressure of the concentration is-0.07 MPa to-0.02 MPa.

9. The glutinous rice leaf oil prepared by the preparation method of any one of claims 1-8.

10. The Cymbopogon flexuosus oil as claimed in claim 9, wherein, The glutinous rice leaf oil comprises 2-propionyl-3, 4, 5, 6-tetrahydropyridine, 2-propionyl-1, 4, 5, 6-tetrahydropyridine, 2-acetyl-3, 4, 5, 6-tetrahydropyridine and water.

11. The Cymbopogon flexuosus oil as claimed in claim 10, wherein, The content of 2-propionyl-3,4,5,6-tetrahydropyridine is 1-3 wt%, the content of 2-propionyl-1,4,5,6-tetrahydropyridine is 1-2 wt%, the content of 2-acetyl-3,4,5,6-tetrahydropyridine is 0.1-0.5 wt%, and the content of water is 0.1 wt% or less, based on the weight of the oryzae japonica leaf oil.

12. Use of the oryzae japonica leaf oil according to any one of claims 9 to 11 in filter plug beads for cigarettes.

13. Use according to claim 12, characterized in that, The amount of the oryzae japonica leaf oil is 0.01-10 wt%, based on the weight of the filter plug beads for cigarettes.

Citation Information

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