CN114082217B - Preparation method and application of flos Abelmoschi Manihot extract - Google Patents

Preparation method and application of flos Abelmoschi Manihot extract Download PDF

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CN114082217B
CN114082217B CN202111337231.8A CN202111337231A CN114082217B CN 114082217 B CN114082217 B CN 114082217B CN 202111337231 A CN202111337231 A CN 202111337231A CN 114082217 B CN114082217 B CN 114082217B
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flower
flos abelmoschi
manihot
abelmoschi manihot
extract
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CN114082217A (en
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刘劲芸
常健
杨培香
王夸平
徐重军
张虹娟
刘秀明
杜超
吴恒
王浩雅
蒋卓芳
曹正东
陈婉
徐世涛
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Yunnan China Tobacco New Material Technology Co ltd
China Tobacco Yunnan Industrial Co Ltd
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Yunnan China Tobacco New Material Technology Co ltd
China Tobacco Yunnan Industrial Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/028Flow sheets
    • B01D11/0284Multistage extraction
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0261Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
    • B01D11/0265Applying ultrasound
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0288Applications, solvents
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention belongs to the technical field of production of tobacco essence and spice, and particularly relates to a preparation method and application of an abelmoschus manihot flower extract. The preparation method comprises the following steps: taking the dry flower of abelmoschus manihot, adding wine, stirring, sealing, placing the flower of abelmoschus manihot into a stir-frying container after the wine is absorbed, stirring, stir-frying, taking out, and cooling to obtain pretreated flower of abelmoschus manihot; step (2), adding ethanol into the pretreated flos Abelmoschi Manihot obtained in the step (1), performing twice cell disruption and ultrasonic extraction, combining the two extracted filtrates, refrigerating at 4 ℃ for 6-24 hours, and filtering to obtain clear liquid which is the crude extract of flos Abelmoschi Manihot; and (3) separating the crude extract of the flos Abelmoschi Manihot obtained in the step (2) through an ultrafiltration membrane to obtain a filtrate, and concentrating the filtrate to obtain the flos Abelmoschi Manihot extract. According to the invention, through adding wine into the flower of abelmoschus manihot for stir-frying, the herb smell, bitter taste and green miscellaneous gas of the flower of abelmoschus manihot can be reduced, the irritation is less, the aftertaste is improved, and the sweet and roast aroma of the essence for the flower tobacco of abelmoschus manihot is increased more unexpectedly.

Description

Preparation method and application of flos Abelmoschi Manihot extract
Technical Field
The invention belongs to the technical field of production of tobacco essence and spice, and particularly relates to a preparation method and application of an abelmoschus manihot flower extract.
Background
The additive is an essential substance in cigarette production, and the development of the spice essence is a core technology of the cigarette industry. The natural perfume has the characteristics of ecology, safety, nature and the like, becomes an important component of the cigarette flavoring technology, and the application research of the natural plant extract in improving the smoking quality of cigarettes is always a hotspot of tobacco research at home and abroad. The development and application of the plant spice for the special cigarettes have profound significance for the production and development of cigarettes. The development and application of the natural perfume for the special cigarettes can meet the requirements of the brand style and characteristics of cigarettes, and improve the quality safety and market competitiveness of the cigarettes.
Abelmoschus manihot Abelmoschus manihot (L.) Medikus is a year to year perennial herb of Abelmoschus (Abelmoschus) genus of Malvaceae (Malvaceae), also known as Abelmoschus esculentus. Is widely cultivated in southern areas such as Yunnan and the like. Abelmoschus manihot is used as a traditional folk medicine, has long medicinal history and is received in various edition of pharmacopoeia of the people's republic of China. Is mainly used for treating chronic bronchitis, chronic nephrosis and complications thereof, urinary infection, scald caused by water and fire, dental ulcer, chyluria, pain relieving and other diseases. The flowers of the traditional Chinese herbs are used as medicines, and the seeds, roots, stems and leaves are fewer. It has sweet and cold flavor, and has effects of clearing heat, promoting diuresis, detumescence and removing toxic substances.
At present, research on abelmoschus manihot at home and abroad in recent years mainly focuses on chemical components, pharmacological actions, resource distribution, cultivation technology and the like. The main chemical components in the flower of Abelmoschus manihot are flavonols, and the others include organic acids, tannins, steroids, long chain hydrocarbons and other compounds. The pharmacological actions of the flower of Abelmoschus manihot are mainly as follows: protecting liver, protecting kidney, resisting inflammation, resisting oxidation, resisting tumor, protecting cardiovascular and cerebrovascular, etc. At present, the flos Abelmoschi Manihot extract is mainly used in the fields of cosmetics, medicines, health products, etc. The flower of Abelmoschus manihot has a unique flower fragrance and natural faint scent, but the tannins cause the Abelmoschus manihot to have heavier smell, bitter feel and clear miscellaneous gas, and the miscellaneous gas can be brought in the smoking process of cigarettes to cause throat irritation and influence comfort, so the application report of the Abelmoschus manihot extract as a tobacco flavor in cigarettes has not been seen.
The present invention has been made to solve the above problems.
Disclosure of Invention
The first aspect of the invention provides a preparation method of an Abelmoschus manihot flower extract, which comprises the following steps:
taking the dry flower of abelmoschus manihot, adding wine, stirring uniformly, sealing and standing for 10-30min, after the flower of abelmoschus manihot is fully soaked and the wine is absorbed, placing the flower of abelmoschus manihot into a stir-frying container, stirring, stir-frying, taking out, cooling and obtaining pretreated flower of abelmoschus manihot;
step (2), adding ethanol into the pretreated flos Abelmoschi Manihot obtained in the step (1), performing twice cell disruption and ultrasonic extraction, combining the two extracted filtrates, refrigerating at 4 ℃ for 6-24 hours, and filtering to obtain clear liquid which is the crude extract of flos Abelmoschi Manihot;
and (3) separating the crude extract of the flos Abelmoschi Manihot obtained in the step (2) through an ultrafiltration membrane to obtain a filtrate, and concentrating the filtrate to obtain the flos Abelmoschi Manihot extract.
Preferably, in the step (1), the mass ratio of the flos abelmoschus manihot to the wine is as follows: 1:3-1:10, wherein the wine is rum with alcohol content of 35-55%vol, the stir-frying temperature is 50-150 ℃, and the stir-frying time is 20-40min.
Preferably, in step (2), the conditions of the ultrasonic extraction are: ultrasonic power is 300-500W, the feed-liquid ratio is 1:10-1:30, and the extraction temperature is 50-70 ℃;
ultrasonic extraction is carried out for the first time, the solvent is ethanol with the volume concentration of 85-95%, and the extraction time is 2-3 h/time;
performing ultrasonic extraction for the second time, wherein the solvent is ethanol with the volume concentration of 55-75%, and the extraction time is 1-2 h/time;
filtering with 400-500 mesh gauze.
Preferably, in the step (3), conditions for ultrafiltration membrane separation are: selecting ultrafiltration membrane with molecular weight cut-off of 5k-30kDa, operating pressure of 0.1-0.4MPa, temperature of 25deg.C, and time of 30-60min.
Preferably, in the step (3), the concentrating step is: concentrating the filtrate at 55deg.C under 80kPa to relative density of 0.85 to obtain flos Abelmoschi Manihot extract.
The second aspect of the invention provides the use of the flos Abelmoschi Manihot extract in any one of the first aspects, wherein the flos Abelmoschi Manihot extract is used as natural tobacco flavor when being added into cigarettes, and has the effects of increasing special flower fragrance, roasted sweet fragrance, sweet fragrance and herb fragrance of smoke, increasing smooth and coordinated feel of smoke, softening and smoothing smoke, improving aftertaste, ensuring comfortable and clean oral cavity and improving the fragrance quality of cigarettes.
The third aspect of the invention provides the use of the flos Abelmoschi Manihot extract according to any one of the first aspect, wherein the flos Abelmoschi Manihot extract is diluted and then uniformly sprayed into tobacco shreds to prepare cigarettes.
Preferably, the mass ratio of the flos Abelmoschi Manihot extract to the tobacco shred is 1-10:1000.
The principle of the invention is as follows:
the pretreatment of the flos Abelmoschi Manihot in the step (1) aims at inhibiting the enzymatic oxidation of tannins such as protocatechuic acid in flos Abelmoschi Manihot and removing bitter taste by destroying and inactivating the enzymatic activity in flos Abelmoschi Manihot at high temperature in the rapid parching process. The green miscellaneous gas can be emitted through the evaporation of the wine during heating and stir-frying, and the remained residue after the evaporation of the wine can promote the formation of good aroma, so that the flower of abelmoschus manihot obtains the sweet aroma and sweet aroma.
In the step (2), the pretreated flower of the abelmoschus manihot obtained in the step (1) is subjected to further cell disruption and ultrasonic extraction so as to achieve the purpose of fully disrupting the cell wall of the flower of the abelmoschus manihot. In the ultrasonic treatment process, the propagation of ultrasonic waves in the ethanol of the extraction medium can enable the medium to vibrate in the propagation space of the extraction medium, so that the diffusion and mass transfer of the medium are enhanced, the mutual collision and friction effects of materials are achieved, the plant cells of the abelmoschus manihot are deformed, and the extraction medium can be effectively promoted to enter plant tissues and cells. Microbubbles dissolved in the medium are increased under the action of ultrasonic waves to form a resonant cavity, and then the resonant cavity is closed instantaneously, so that the cells of the flower of abelmoschus manihot can be broken instantaneously, and intracellular active ingredients are released. In addition, in the transmission process of ultrasonic waves, the acoustic energy is continuously absorbed by the extraction medium, most of the acoustic energy is converted into heat energy, the temperature of the medium and plant tissues can be rapidly increased, and the target components in the cell walls of the abelmoschus manihot flowers are promoted to be dissolved into the solvent.
In the step (3), the flos Abelmoschi Manihot extract is separated and purified by ultrafiltration membrane, and the purpose is to effectively separate and remove macromolecular substances such as protein, pigment, wax, etc. in flos Abelmoschi Manihot, which are main substances for causing cigarette miscellaneous gas and irritation. The separation process of the ultrafiltration membrane is a sieve mesh separation process, and is a method for separating according to the size difference of the molecules of the separated substances. The molecular diameter of the flower fragrance substance of the abelmoschus manihot is smaller than the pore diameter of the ultrafiltration membrane under the preferable condition, and the molecules can reach the permeation side through the ultrafiltration membrane layer. And macromolecular substances such as proteins, pigments, waxes and the like are trapped on the surface of the membrane or returned to the main body of the feed liquid. The separation process has the advantages of no phase change, less energy consumption, no consumption of chemical reagents, no pollution to products, no damage to the flower fragrance components of the abelmoschus manihot, and improvement of the purity of the fragrance substances.
The technical proposal can be freely combined on the premise of no contradiction.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a preparation method of a flower tobacco flavor of abelmoschus manihot, which is characterized in that wine is added into flower of abelmoschus manihot for stir-frying, so that the smell, bitter and astringent taste and green miscellaneous gas of the herb of abelmoschus manihot can be reduced, the irritation is reduced, the aftertaste is improved, and the sweet and roast aroma of the flower tobacco flavor of abelmoschus manihot is increased more unexpectedly. The natural flower of abelmoschus manihot only has the characteristics of flower fragrance and faint scent, but in the preparation process of the invention, the spice for the abelmoschus manihot tobacco obtains the sweet aroma and sweet fragrance, and can coordinate the aroma of the tobacco and improve the aftertaste, and the effect cannot be expected by the person skilled in the art.
2. In addition, the invention combines the cell disruption ultrasonic extraction method and the ultrafiltration membrane separation and purification method, the ultrasonic extraction method breaks the cells of the abelmoschus manihot, the intracellular active ingredients are released rapidly, and the product yield and the extraction efficiency are improved. The directivity selects ultrafiltration membrane with cut-off molecular weight of 5k-30kDa to separate and purify flos Abelmoschi Manihot flower extract, and macromolecular impurities such as protein, pigment, wax, etc. are effectively separated and removed under room temperature condition, so as to avoid the damage of thermosensitive and aroma components, and improve the aroma and aroma quality of the product. The extraction process is simple, short in period, environment-friendly, safe, wide in application range, convenient for large-scale and industrialized production, and high in economic benefit.
3. According to the invention, through a unique preparation method, the flower of abelmoschus manihot is used for preparing the tobacco flavor in the cigarette product for the first time, and the flower flavor has the effects of increasing special flower flavor, roasted sweet flavor, sweet flavor and herbal fragrance, increasing smooth feel and coordination feel, enabling smoke to be soft and smooth, improving aftertaste, enabling oral cavity to be comfortable and clean and improving the fragrance quality of the cigarette. Therefore, the natural sources and the types of the tobacco essence and the perfume are enriched, the style characteristics of Chinese cigarettes are enhanced, and the demands of individuation and diversification of consumers are met.
Drawings
Fig. 1 is a total ion flow chart of the flower tobacco flavor of abelmoschus manihot prepared in example 1 of the present invention.
FIG. 2 shows the fragrance style characteristics of the Abelmoschus manihot flower fragrance obtained in example 1, comparative example 2 and comparative example 3 in test example 2 according to the present invention.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited to the examples. Experimental methods, in which specific conditions are not specified in examples, are generally available commercially according to conventional conditions as well as those described in handbooks, or according to general-purpose equipment, materials, reagents, etc. used under conditions suggested by manufacturers, unless otherwise specified. The raw materials required in the following examples and comparative examples are all commercially available.
Example 1
A preparation method of flos Abelmoschi Manihot extract comprises the following steps:
step 1, taking dried Yunnan flos Abelmoschi Manihot as a raw material, removing leaves and impurities, then placing the flos Abelmoschi Manihot into a container, adding 5 times of rum with the alcohol content of 40% vol, stirring uniformly, covering a container cover, standing for 30min, placing the flos Abelmoschi Manihot into a stir-frying container after the flos Abelmoschi Manihot is fully soaked, stirring at 100 ℃ for stir-frying for 30min, taking out, cooling, and obtaining pretreated flos Abelmoschi Manihot.
Step 2, adding the pretreated flos Abelmoschi Manihot obtained in the step 1 into ethanol with the volume concentration of 95% and the feed liquid ratio of 1:20, performing cell disruption ultrasonic extraction, wherein the ultrasonic power is 300W, and the ultrasonic temperature is 50 ℃ for 2 hours; then filtering with 400 mesh filter cloth, performing second ultrasonic extraction with residue at a feed-liquid ratio of 1:10, wherein the solvent is 70% ethanol with volume concentration, the extraction temperature is 50deg.C, the extraction time is 1h, filtering with 400 mesh filter cloth, mixing the two filtrates, refrigerating at 4deg.C for 12h, and filtering with 500 mesh gauze to obtain clear solution as flos Abelmoschi Manihot crude extract.
And 3, passing the crude extract of the abelmoschus manihot obtained in the step 2 through an ultrafiltration membrane with a molecular weight cut-off of 30kDa, wherein the operation pressure is 0.2MPa, the temperature is room temperature, filtering is carried out for 30min to obtain filtrate, and then concentrating the filtrate to a relative density of 0.85 under the conditions of 55 ℃ and 80kPa to obtain the extract of the abelmoschus manihot.
Comparative example 1
A preparation method of flos Abelmoschi Manihot extract comprises, compared with example 1, directly extracting flos Abelmoschi Manihot with 80% ethanol by volume concentration twice, concentrating the extractive solution at 55deg.C under 80kPa to relative density of 0.85 to obtain flos Abelmoschi Manihot extract.
Comparative example 2
A preparation method of flos Abelmoschi Manihot extract is compared with example 1, and the preparation method does not perform pretreatment in step 1, and step 2 and step 3 are the same to obtain flos Abelmoschi Manihot extract.
Comparative example 3
A preparation method of flos Abelmoschi Manihot extract comprises pretreating flos Abelmoschi Manihot extract in step 1 with wine with alcoholicity of 38% vol, and processing in step 2 and step 3 to obtain flos Abelmoschi Manihot extract.
Test example 1
The extract of Abelmoschus manihot prepared in example 1 was detected by gas chromatography-mass spectrometry combined with GC-MS analysis:
(1) Gas chromatography conditions: chromatographic column: DB-5MS quartz capillary column (30 m x 0.25mm,0.25 μm); programming temperature: the initial temperature is 60 ℃, kept for 1min, and raised to 170 ℃ at a speed of 8 ℃/min, and kept for 3min; raising the temperature to 260 ℃ at a speed of 12 ℃/min, and keeping for 18min; sample inlet temperature: 200 ℃; column box temperature: 60 ℃; sample injection mode: splitting; column flow rate: 1mL/min; purge flow rate: 3mL/min; split ratio: 5:1; carrier gas: high purity helium; sample injection amount: 1 μl; solvent delay: 2min.
(2) Mass spectrometry conditions: ionization mode: EI; electron energy: 70eV; interface temperature: 250 ℃; ion source temperature: 200 ℃; the acquisition mode is as follows: scanning; scanning range: 40-500amu.
(3) Qualitative analysis: by using mass spectrum as a detector and gas chromatography and utilizing NIST spectrum library to search, aroma components in the particle-flavored cigarette sample can be identified in a short time, and qualitative analysis can be performed.
(4) Quantitative analysis: the internal standard is 99% naphthalene, and semi-quantitative analysis is carried out on the aroma components by adopting an internal standard method. The content of the aroma-generating component was calculated as follows.
Figure BDA0003351010060000061
Wherein:
x-content of each compound, μg/g; as—integrated peak area for each compound; ai-integral peak area of internal standard substance; mi-mass of internal standard substance, g; m, the mass of the perfumed cigarette sample, g.
The specific component contents are shown in Table 1.
TABLE 1 analysis of the composition and relative content of Abelmoschus manihot flower extract prepared in EXAMPLE 1
Figure BDA0003351010060000062
Figure BDA0003351010060000071
Figure BDA0003351010060000081
Note that: "-" indicates that the component was not detected.
As is clear from Table 1, the Abelmoschus manihot flower extract prepared in example 1 contains a large amount of carboxylic acid aroma substances, which can adjust the pH value of tobacco and increase the richness and harmony of smoke. The alcohol compound content is also higher, and the alcohol compound has stronger influence on the odor absorption and aftertaste improvement of the fine and soft smoke. In addition, the aldehyde and ketone compounds have special aromatic smell, so that the richness and the concentration of the smoke can be effectively increased.
Test example 2
Sensory evaluation of cigarettes: the flos Abelmoschi Manihot flower extracts prepared in the invention examples 1, comparative example 2 and comparative example 3 are diluted by 0.5% of tobacco shreds of cigarettes respectively, and are injected into cigarettes respectively by an essence and spice injector to obtain cigarettes-example 1 (50 cigarettes), cigarettes-comparative example 2 (50 cigarettes) and cigarettes-comparative example 3 (50 cigarettes) respectively. Blank cigarettes (50 cigarettes) without perfume were used as control.
All the cigarettes are placed in a constant temperature and humidity box (the temperature is 22+/-1 ℃ and the humidity is 60+/-2%) and balanced for 48 hours, and the cigarettes are evaluated by an expert with the qualification of cigarette smoking according to the sensory technical requirements of the 4 th part of the cigarettes of GB 5606.4-2005.
The results show that: the flower fragrance for the flower tobacco of the Abelmoschus manihot has the effects of increasing special flower fragrance, roasted sweet fragrance, sweet fragrance and herb fragrance, increasing smooth feel and coordination feel, enabling smoke to be soft and smooth, improving aftertaste, enabling oral cavity to be comfortable and clean and improving the fragrance quality of cigarettes.
Analysis of cigarette smoking evaluation results of spice for Abelmoschus manihot flower cigarette
Figure BDA0003351010060000082
The sensory evaluation results of example 1 and comparative examples 1-3 in table one correspond to the cigarette aroma style characteristic network diagrams shown in figure two, respectively.
As can be seen from the first table and the second drawing, the cigarette added with the flower tobacco flavor of the abelmoschus manihot prepared by the invention has particularly outstanding sweet and roasted sweet style characteristics, soft and coordinated smoke, obvious improvement of miscellaneous gas, reduced irritation and comfortable aftertaste compared with the cigarette added with the flower extract of the abelmoschus manihot in the proportion of 1-3.
The roasted sweet flavor is expressed as a product formed by mixing the sweet flavor, the roasted flavor and other flavors in a cigarette flavor style characteristic diagram.
The spice for the abelmoschus manihot tobacco, which is prepared by the invention, has pleasant sweet aroma and sweet aroma, can coordinate the tobacco aroma, reduce the irritation and improve the aftertaste, and is possibly related to adding the rum in the stir-frying process, because the rum is brewed by distilling and fermenting sugarcane juice, the spice has fine and sweet taste, fragrant aroma is obtained, the residue after the evaporation of the wine and the abelmoschus manihot flowers are mixed to form good aroma, and the cigarette added with the abelmoschus manihot flowers obtains the sweet aroma and sweet aroma in the synergistic action sucking process of the two. The wine of comparative example 3 does not have the above effect in the present invention.

Claims (1)

1. The application of the flos Abelmoschi Manihot extract is characterized in that the flos Abelmoschi Manihot extract is used as natural tobacco flavor when being added into cigarettes, and has the effects of increasing special flower fragrance, baked sweet fragrance, sweet fragrance and herb fragrance of smoke, increasing smooth and coordinated feel of smoke, softening and smoothing smoke, improving aftertaste, comfort and cleanliness of oral cavity and improving fragrance quality of cigarettes;
the preparation method of the flower extract of abelmoschus manihot comprises the following steps:
step (1), taking dry flos Abelmoschi Manihot flower in the shade, adding wine, stirring, sealing and standing for 10-30min, parching flos Abelmoschi Manihot flower after the wine is absorbed by flos Abelmoschi Manihot flower, taking out, and cooling to obtain pretreated flos Abelmoschi Manihot flower;
step (2), adding ethanol into the pretreated flos Abelmoschi Manihot obtained in the step (1), performing twice cell disruption and ultrasonic extraction, combining the two extracted filtrates, refrigerating at 4 ℃ for 6-24 hours, and filtering to obtain clear liquid which is the crude extract of flos Abelmoschi Manihot;
step (3), separating the crude extract of the flos Abelmoschi Manihot obtained in the step (2) through an ultrafiltration membrane to obtain a filtrate, and concentrating the filtrate to obtain the extract of the flos Abelmoschi Manihot;
in the step (1), the mass ratio of the flos Abelmoschi Manihot to the wine is as follows: 1:3-1:10, wherein the wine is rum with alcohol content of 35-55%vol, the stir-frying temperature is 50-150 ℃, and the stir-frying time is 20-40min;
in the step (2), the conditions of ultrasonic extraction are as follows: ultrasonic power is 300-500W, the feed-liquid ratio is 1:10-1:30, and the extraction temperature is 50-70 ℃;
ultrasonic extraction is carried out for the first time, the solvent is ethanol with the volume concentration of 85-95%, and the extraction time is 2-3 h/time;
performing ultrasonic extraction for the second time, wherein the solvent is ethanol with the volume concentration of 55-75%, and the extraction time is 1-2 h/time;
filtering with 400-500 mesh gauze;
in the step (3), conditions for ultrafiltration membrane separation are as follows: selecting ultrafiltration membrane with molecular weight cutoff of 5k-30kDa, operating pressure of 0.1-0.4MPa, temperature of 25deg.C, and time of 30-60min;
step (3), the concentration step is: concentrating the filtrate at 55deg.C under 80kPa to relative density of 0.85 to obtain flos Abelmoschi Manihot extract.
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CN103989247B (en) * 2014-05-20 2016-04-27 河南中烟工业有限责任公司 Sunset abelmoschus flower alcohol extract and the application in cigarette thereof
CN105062678A (en) * 2015-07-31 2015-11-18 湖北中烟工业有限责任公司 Preparation method of cigarette fenugreek concrete
CN109722341A (en) * 2019-01-04 2019-05-07 云南中烟工业有限责任公司 A kind of preparation method and application of Golden flower tobacco aromaticss
CN111808681A (en) * 2020-07-20 2020-10-23 广西中烟工业有限责任公司 Preparation method of lycium ruthenicum murr spice for cigarettes and application of lycium ruthenicum murr spice in cigarettes
CN111849636A (en) * 2020-08-03 2020-10-30 湖北中烟工业有限责任公司 Spice for wine-roasted Chinese angelica cigarette and preparation method and application thereof
CN112189875A (en) * 2020-10-23 2021-01-08 湖北中烟工业有限责任公司 Polysweet fruit refined extract for cigarettes as well as preparation method and application thereof

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