CN116554966A - Bamboo She Xiangliao and preparation method thereof - Google Patents
Bamboo She Xiangliao and preparation method thereof Download PDFInfo
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- CN116554966A CN116554966A CN202310775246.5A CN202310775246A CN116554966A CN 116554966 A CN116554966 A CN 116554966A CN 202310775246 A CN202310775246 A CN 202310775246A CN 116554966 A CN116554966 A CN 116554966A
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a bamboo She Xiangliao and a preparation method thereof, and relates to the technical field of spice preparation. The preparation of the bamboo leaf spice comprises the steps of preparation of a bamboo leaf extract, maillard reaction and molecular distillation, and finally mixing a light component 1#, a light component 2#, a light component 3# and a solvent obtained by the molecular distillation to obtain the bamboo She Xiangliao. The preparation method of the bamboo leaf spice changes the traditional process of extracting the bamboo leaves by a single method, and can fully extract various active ingredients with dissolution property in the bamboo leaves. In addition, the bamboo She Xiangliao prepared by the method can be applied to electronic atomized liquid. The bamboo leaf spice obtained by the invention has no foreign flavor basically, can obviously enhance aftertaste sweet feel, promote salivation feel and increase smoke fullness, and can reduce burnt cores in the use process.
Description
Technical Field
The invention relates to the technical field of spice preparation, in particular to bamboo She Xiangliao and a preparation method thereof.
Background
The electronic atomization liquid is heated by an electronic atomizer to form aerosol similar to the traditional cigarette smoke. The main components of the electronic atomized liquid generally comprise glycerol, propylene glycol, nicotine and special flavors. At present, the development of special flavors for electronic atomized liquid in the market focuses on the unique flavor, for example, patent CN104498186A discloses a flavor formula for electronic atomized liquid, so that a user can feel caramel fragrance; patent CN113243550B discloses a bergamot spice for an electronic atomized liquid, which makes the electronic atomized liquid have bergamot fragrance and rich taste.
Bamboo is perennial evergreen plant of Gramineae and has about more than 60 genus of bamboo plant in the whole world, and 1200 more than one genus. China is the main production area of the world bamboos, is one of the most abundant world bamboos, and the types, areas and accumulation of bamboo forests all stay in the front of the world, so that the utilization value of bamboo leaves is gradually recognized by people. Bamboo She Fuhan polysaccharide, flavone, polyphenol, protein, amino acid, mineral elements and other active substances, and also contains abundant cellulose components. In recent years, the bamboo leaf extract has rich raw material sources, definite functional factors, good edible safety, efficient and stable preparation quality and fresh and sweet bamboo flavor, and is brand-new in the fields of natural functional food additives, medical health products and daily chemicals. The smell of bamboo has the characteristics of complexity and variability, and the faint scent of bamboo mainly comes from the cell structure and the phytochemical property of the bamboo. Many research results show that the faint scent of the bamboo leaves mainly originates from plant organs, especially the alpha-caryophyllene contained in the bamboo leaves and the bamboo stalks. In addition, oxygenates such as plant alcohols, aldehydes, fats and the like also contribute significantly to the freshness flavor. In addition, some plant essential oils in bamboo, such as camphor, camphor mustard essential oil, branched chain fatty acid and zanthoxylum aldehyde, also have strong fragrance.
In the prior art, the extraction mode of the active ingredients of the bamboo leaves comprises hot water extraction, organic solvent extraction, supercritical carbon dioxide extraction or ultrasonic auxiliary extraction and the like. Patent CN110655997B discloses a preparation method of lophatherum gracile health care beer, wherein the lophatherum gracile health care beer is prepared by mixing wort and a lophatherum gracile extracting solution and then fermenting, and the lophatherum gracile extract used in the method is a lophatherum gracile water extract. The preparation method of the bamboo leaf extract in the patent has low extraction efficiency and low content of bamboo leaf flavone; in addition, the aroma substances of the bamboo leaf extract are greatly reduced after the bamboo leaf extract is extracted and dried, and the faint scent of the beer bamboo leaf is difficult to be endowed. The preparation process of the bamboo leaf extract is mainly aimed at the fields of natural functional food additives, medical health products, daily chemical products and the like, and no electronic atomized liquid of bamboo leaf flavor and spice exists in the electronic atomization industry at present.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a preparation method of bamboo leaf spice, which solves the problem of the shortage of the traditional single extraction method, and fully extracts various dissolved substance active ingredients in bamboo leaves. The invention further aims to apply the bamboo She Xiangliao to the atomized liquid, remarkably enhance the aftertaste sweet feeling and the salivation feeling of the electronic atomized liquid, increase the smoke fullness and enrich the flavor of the electronic atomized liquid.
In order to achieve the above purpose, the invention provides a preparation method of bamboo leaf spice, which adopts the following technical scheme.
(1) Preparation of bamboo leaf extract
Preparation of a bamboo leaf extract I: adding the bamboo leaf powder into water, extracting at 80-100 ℃, and separating water from oil after the extraction is finished to obtain a bamboo leaf extract I. Preferably, the extraction adopts reflux extraction, and the reflux extraction time is 6-8 h. More preferably, the extraction temperature is 90℃and the reflux extraction time is 7 hours.
In some embodiments, the first bamboo leaf extract is prepared by drying and pulverizing bamboo leaves, sieving with a 100-mesh sieve, adding into water, and reflux-extracting at 80-100deg.C for 6-8 h, and separating water and oil to obtain the first bamboo leaf extract.
Preparing a second bamboo leaf extract: adding the bamboo leaf powder into petroleum ether, extracting at 60-80 ℃, concentrating under reduced pressure after the extraction is finished, washing with absolute ethyl alcohol, and concentrating under reduced pressure to obtain a bamboo leaf extract II. Preferably, the extraction adopts reflux extraction, and the reflux extraction time is 4-5 h. More preferably, the extraction temperature is 70℃and the reflux extraction time is 4.5h.
In some embodiments, the preparation method of the second bamboo leaf extract comprises the steps of drying and crushing bamboo leaves, sieving the bamboo leaves with a 100-mesh sieve, adding the bamboo leaves into petroleum ether, carrying out heat preservation and reflux extraction for 4-5 hours at 60-80 ℃, filtering, concentrating under reduced pressure, washing with absolute ethyl alcohol, and concentrating under reduced pressure to obtain the second yellow oily bamboo leaf extract.
Preparation of bamboo leaf extract III: soaking bamboo leaf powder and cellulase in water, adding water to extract at 35-45 deg.c to obtain extractive solution, concentrating the extractive solution to specific gravity of 1.3-1.7, adding ethanol, letting stand, evaporating supernatant to obtain light yellow thick oil bamboo leaf extract III.
The cell walls of the bamboo leaves are treated by utilizing enzymatic reaction, so that the active ingredients in the bamboo leaf cells can be extracted as much as possible.
Preferably, the weight ratio of the cellulase to the bamboo leaf powder is 1: (4000-6000). The enzyme activity of the cellulase ranges from 400U/mg to 800U/mg.
In some embodiments, the preparation method of the bamboo leaf extract III comprises the steps of soaking bamboo leaf powder and cellulase in water at 26-30 ℃ for 15-18 h; then adding water for extraction for 2-4 times, extracting at the temperature of 35-45 ℃, filtering, and combining the filtrates to obtain an extracting solution; concentrating the extractive solution to a specific gravity of 1.3-1.7, adding 3-5 times of ethanol, standing for 22-28 h, collecting supernatant, and concentrating under reduced pressure to obtain herba Lophatheri extract III.
More preferably, in some embodiments, the bamboo leaf extract III is prepared by soaking bamboo leaf powder and cellulase in 1-3 times of water at 26-30deg.C for 15-18 h; then adding water for extraction for 2-4 times, extracting at the temperature of 35-45 ℃, filtering, and combining the filtrates to obtain an extracting solution; concentrating the extract to a specific gravity of 1.5, adding 3-5 times of ethanol for precipitation, standing for 24h, and concentrating the supernatant under reduced pressure to obtain a light yellow viscous oily bamboo leaf extract III.
Further, the preparation method of the bamboo leaf extract III comprises the steps of placing bamboo leaf powder and cellulase in 2 times of water at 26-30 ℃ for soaking for 16 hours; extracting with water for 3 times at 40deg.C, wherein the water extraction temperature is 5 times that of the first time for 3 hr, filtering to obtain extractive solution A, the water extraction temperature is 3 times that of the second time for 2 hr, filtering to obtain extractive solution B, and the water extraction temperature is 1 time that of the third time for 1 hr, filtering to obtain extractive solution C; mixing the extract A, the extract B and the extract C to obtain an extract; concentrating the extractive solution to specific gravity of 1.5, adding 4 times of ethanol for precipitation, standing for 24 hr, collecting supernatant, and concentrating under reduced pressure to obtain light yellow viscous oily herba Lophatheri extract III.
(2) Maillard reaction
Mixing the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract to obtain an extraction mixture, dispersing the extraction mixture with propylene glycol, adding amino acid and reducing sugar, and mixing and reacting at 60-80 ℃ to obtain a reaction solution.
In some embodiments, the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract are mixed to obtain an extraction mixture, 3-5 times of propylene glycol is used for stirring and dispersing, then amino acid and reducing sugar are added, and the mixture is stirred in a water bath at the temperature of 60-80 ℃ for 3-5 hours to obtain a reaction solution.
Preferably, the amino acid is selected from one or more of aspartic acid, glutamic acid and proline; the reducing sugar is selected from one or more of glucose, fructose and maltose. More preferably, the weight ratio of amino acid to extraction mixture is 1: (20-50); the weight ratio of the reducing sugar to the extraction mixture is 1: (20-50).
Preferably, the extraction mixture is obtained by mixing the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract prepared by adopting equal amount of bamboo leaf powder in the step (1).
(3) Molecular distillation
Carrying out first molecular distillation on the reaction liquid obtained in the step (2), wherein the molecular distillation temperature is 30-50 ℃ and the vacuum degree is 5000-8000 Pa, so as to obtain a light component 1# and a heavy component 1#;
taking heavy component 1# to carry out second molecular distillation, wherein the molecular distillation temperature is 50-80 ℃ and the vacuum degree is 1000-3000 Pa, so as to obtain light component 2# and heavy component 2#;
and (3) carrying out third molecular distillation on the heavy component 2# at the molecular distillation temperature of 80-110 ℃ and the vacuum degree of 18-300 Pa to obtain a light component 3# and a heavy component 3#.
(4) Mixing light component 1#, light component 2#, light component 3# and solvent to obtain bamboo She Xiangliao.
Light component 1#, light component 2#, and light component 3# are target perfume substances, which are bamboo fragrance 1#, bamboo fragrance 2#, and bamboo fragrance 3#, respectively.
The bamboo She Xiangliao obtained by the preparation method comprises the following components in percentage by weight:
5% -15% of light component 1# (bamboo fragrance 1 #);
10% -22% of light component No. 2 (bamboo fragrance No. 2);
18% -28% of light component 3# (bamboo fragrance 3#);
the balance being solvent.
The preparation method of the bamboo leaf spice comprises stirring bamboo fragrance No. 1, bamboo fragrance No. 2, bamboo fragrance No. 3 and solvent until the mixture is clear and uniform to obtain bamboo She Xiangliao.
Preferably, the solvent in the bamboo leaf flavor is food-grade propylene glycol and/or food-grade glycerol.
By adopting the technical scheme, three bamboo fragrance components have better solubility in food-grade propylene glycol and/or food-grade glycerol, and aromatic substances in the bamboo leaf perfume are not easy to volatilize when the bamboo leaf perfume is placed at normal temperature.
Preferably, in the bamboo She Xiangliao, the weight ratio of the bamboo fragrance 1#, the bamboo fragrance 2#, and the bamboo fragrance 3# is (8-12): (16-18): (22-24).
The bamboo She Xiangliao can be applied to electronic atomized liquid. The bamboo She Xiangliao compounded by the three bamboo fragrance components in the technical scheme has the advantages of rich fragrance in the early fresh and sweet period and good connection of the fragrance in each stage when the fragrance volatilizes, mellow fragrance, less miscellaneous fragrance and long fragrance holding effect.
The preparation method of the bamboo leaf spice changes the traditional process of extracting the bamboo leaves by a single method, and can fully extract various active ingredients with dissolution property in the bamboo leaves. After extraction, amino acid and reducing sugar are added into the extract for Maillard reaction, secondary processing is carried out on active substances, aroma substances are generated by using the Maillard reaction, then molecular distillation is carried out for a plurality of times, active ingredients of the bamboo leaf extract are separated, and a part of components which are unfavorable to the quality of electronic atomized liquid are removed, so that the quality of the bamboo leaf spice is improved to a certain extent, the obtained bamboo leaf spice has no unpleasant taste basically, the aftertaste sweet taste, the body fluid production feeling and the smoke fullness are obviously enhanced, and the paste core is reduced in the use process.
The bamboo leaf spice has the advantages that the front sweet taste stage and the rear sweet taste stage are rich, the aroma level is rich, the aroma is mellow, and the aftertaste is long; meanwhile, the bamboo leaf spice has more active ingredients extracted from phenolic acid compounds, anthraquinone compounds, terpene lactones, special amino acids, microelements such as manganese, zinc and selenium and the like, has better antioxidation effect, and can reduce the generation of miscellaneous flavor in the spice.
In addition, the bamboo She Xiangliao is applied to the electronic atomized liquid for the first time, so that the flavor of the electronic atomized liquid can be enriched, the electronic atomized liquid has a health care function, the psychological requirement of a smoker on smoke is met, and the physical health of the smoker is protected.
Detailed Description
The technical scheme of the invention is further described and illustrated by the following specific examples. The raw materials used in the examples of the present invention are all those commonly used in the art unless otherwise specified. It should be understood that the specific embodiments described herein are merely to aid in the understanding of the present invention and are not intended to be limiting in any way.
Example 1
(1) Preparation of bamboo leaf extract
Pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding into 1000ml of water, reflux-extracting at 90deg.C for 7 hr, cooling to 20deg.C, and oil-water separating to obtain pale yellow oily bamboo leaf extract I;
pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding into 600ml petroleum ether, heating to 70deg.C, reflux extracting for 4.5 hr, cooling to 20deg.C, filtering, and concentrating the filtrate under reduced pressure at 40deg.C to obtain crude bamboo leaf extract II; adding 300mL of absolute ethanol into the second crude bamboo leaf extract, stirring for dissolving, and concentrating under reduced pressure at 40 ℃ to obtain a second yellow oily bamboo leaf extract;
pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding 100ml of water and 10mg of cellulase, soaking at 26 deg.C for 16h, extracting with water for 3 times at 40 deg.C, adding 250ml of water for the first time, extracting for 3h, and filtering to obtain extract A; adding 150ml of water for the second time, extracting for 2 hours, and filtering to obtain an extract B; adding 50ml of water for the third time, extracting for 1h, filtering to obtain an extract C, mixing the extract A, the extract B and the extract C, concentrating to a specific gravity of 1.5, adding 300ml of ethanol for precipitation, standing for 24h, taking supernatant, and concentrating under reduced pressure to obtain a light yellow viscous oily bamboo leaf extract III.
(2) Maillard reaction
Mixing the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract to obtain 85g of an extraction mixture, stirring and dispersing the mixture with 400g of propylene glycol, adding 3.5g of aspartic acid and 4g of glucose, and stirring and reacting the mixture in a water bath at the temperature of 75 ℃ for 5h to obtain a reaction liquid.
(3) Molecular distillation
Taking the reaction liquid in the step (2) for carrying out first molecular distillation: the molecular distillation temperature is 45 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 6000Pa, so that the light component 1# and the heavy component 1# are obtained;
taking heavy component 1# for second molecular distillation: the molecular distillation temperature is 75 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 2000Pa, so that the light component 2# and the heavy component 2# are obtained;
taking heavy component 2# and carrying out third molecular distillation: the molecular distillation temperature is 110 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 50Pa, so that the light component 3# and the heavy component 3# are obtained.
(4) Molecular distillation of the bamboo leaf extract to obtain light component 1#, light component 2#, and light component 3# as target perfume substances, which are bamboo fragrance 1#, bamboo fragrance 2#, and bamboo fragrance 3#, respectively; 10g of bamboo fragrance No. 1, 16g of bamboo fragrance No. 2 and 23g of bamboo fragrance No. 3 are weighed, 51g of food-grade propylene glycol is added, and the mixture is stirred and mixed until the solution is clear, thus obtaining bamboo She Xiangliao.
Example 2
(1) Preparation of bamboo leaf extract
Pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding into 1000ml of water, reflux-extracting at 80deg.C for 6 hr, cooling to 20deg.C, and oil-water separating to obtain pale yellow oily bamboo leaf extract I;
pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding into 600ml petroleum ether, heating to 60deg.C, reflux extracting for 4 hr, cooling to 20deg.C, filtering, and concentrating the filtrate under reduced pressure at 40deg.C to obtain crude bamboo leaf extract II; adding 300mL of absolute ethanol into the second crude bamboo leaf extract, stirring for dissolving, and concentrating under reduced pressure at 40 ℃ to obtain a second yellow oily bamboo leaf extract;
pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding 100ml of water and 8mg of cellulase, soaking at 26 deg.C for 16h, extracting with water for 3 times at 35 deg.C, adding 250ml of water for the first time, extracting for 3h, and filtering to obtain extract A; adding 150ml of water for the second time, extracting for 2 hours, and filtering to obtain an extract B; adding 50ml of water for the third time, extracting for 1h, filtering to obtain an extract C, mixing the extract A, the extract B and the extract C, concentrating to a specific gravity of 1.3, adding 300ml of ethanol for precipitation, standing for 24h, recovering ethanol from the supernatant under reduced pressure, and evaporating to obtain a light yellow viscous oily bamboo leaf extract III.
(2) Maillard reaction
Mixing the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract to obtain 90g of an extraction mixture, stirring and dispersing the mixture with 400g of propylene glycol, adding 3.5g of glutamic acid and 4g of maltose, and stirring and reacting the mixture in a water bath at the temperature of 60 ℃ for 5h to obtain a reaction liquid.
(3) Molecular distillation
Taking the reaction liquid in the step (2) for carrying out first molecular distillation: the molecular distillation temperature is 45 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 6000Pa, so that the light component 1# and the heavy component 1# are obtained;
taking heavy component 1# for second molecular distillation: the molecular distillation temperature is 75 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 2000Pa, so that the light component 2# and the heavy component 2# are obtained;
taking heavy component 2# and carrying out third molecular distillation: the molecular distillation temperature is 110 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 50Pa, so that the light component 3# and the heavy component 3# are obtained.
(4) Molecular distillation of the bamboo leaf extract to obtain light component 1#, light component 2#, and light component 3# as target perfume substances, which are bamboo fragrance 1#, bamboo fragrance 2#, and bamboo fragrance 3#, respectively; 11g of bamboo fragrance No. 1, 16g of bamboo fragrance No. 2 and 22g of bamboo fragrance No. 3 are weighed, 51g of food-grade propylene glycol is added, and the mixture is stirred and mixed until the solution is clear, thus obtaining bamboo She Xiangliao.
Example 3
(1) Preparation of bamboo leaf extract
Pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding into 1000ml of water, reflux-extracting at 100deg.C for 7 hr, cooling to 20deg.C, and separating oil from water to obtain pale yellow oily bamboo leaf extract I;
pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding into 600ml petroleum ether, heating to 80deg.C, reflux extracting for 4.5 hr, cooling to 20deg.C, filtering, and concentrating the filtrate under reduced pressure at 40deg.C to obtain crude bamboo leaf extract II; adding 300mL of absolute ethanol into the second crude bamboo leaf extract, stirring for dissolving, and concentrating under reduced pressure at 40 ℃ to obtain a second yellow oily bamboo leaf extract;
pulverizing 50g of dried bamboo leaves, sieving with 100 mesh sieve to obtain bamboo leaf powder, adding 100ml of water and 10mg of cellulase, soaking at 26deg.C for 16h, extracting with water for 3 times at 45deg.C, adding 250ml of water for the first time, extracting for 3h, and filtering to obtain extract A; adding 150ml of water for the second time, extracting for 2 hours, and filtering to obtain an extract B; adding 50ml of water for the third time, extracting for 1h, filtering to obtain an extract C, mixing the extract A, the extract B and the extract C, concentrating to a specific gravity of 1.7, adding 300ml of ethanol for precipitation, standing for 24h, recovering ethanol from the supernatant under reduced pressure, and evaporating to obtain a light yellow viscous oily bamboo leaf extract III.
(2) Maillard reaction
Mixing the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract to obtain 86g of an extraction mixture, stirring and dispersing the mixture with 400g of propylene glycol, adding 3.5g of proline and 4g of fructose, and stirring and reacting the mixture in a water bath at the water bath temperature of 80 ℃ for 5h to obtain a reaction liquid.
(3) Molecular distillation
Taking the reaction liquid in the step (2) for carrying out first molecular distillation: the molecular distillation temperature is 45 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 6000Pa, so that the light component 1# and the heavy component 1# are obtained;
taking heavy component 1# for second molecular distillation: the molecular distillation temperature is 75 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 2000Pa, so that the light component 2# and the heavy component 2# are obtained;
taking heavy component 2# and carrying out third molecular distillation: the molecular distillation temperature is 110 ℃, the condensation temperature is 8 ℃, the film scraping rotating speed is 150rpm, and the vacuum degree is 50Pa, so that the light component 3# and the heavy component 3# are obtained.
(4) Molecular distillation of the bamboo leaf extract to obtain light component 1#, light component 2#, and light component 3# as target perfume substances, which are bamboo fragrance 1#, bamboo fragrance 2#, and bamboo fragrance 3#, respectively; 10g of bamboo fragrance No. 1, 17g of bamboo fragrance No. 2 and 23g of bamboo fragrance No. 3 are weighed, 50g of food-grade propylene glycol is added, and the mixture is stirred and mixed until the solution is clear, thus obtaining bamboo She Xiangliao.
Examples 4 to 10
Examples 4-10 differ from example 1 in that in step (4) the quality of bamboo fragrance 1#, bamboo fragrance 2#, bamboo fragrance 3#, food grade propylene glycol was different, and the other steps were the same as in example 1, and specific qualities of bamboo fragrance 1#, bamboo fragrance 2#, bamboo fragrance 3#, food grade propylene glycol of examples 4-10 are shown in table 1 below.
Table 1 quality of the three bamboo fragrance components of examples 4-10
Examples | Bamboo fragrance 1#/g | Bamboo fragrance 2#/g | Bamboo fragrance 3#/g | Food grade propylene glycol/g |
Example 4 | 9 | 18 | 24 | 49 |
Example 5 | 8 | 18 | 22 | 52 |
Example 6 | 8 | 17 | 23 | 52 |
Example 7 | 9 | 16 | 24 | 51 |
Example 8 | 10 | 18 | 23 | 49 |
Example 9 | 11 | 16 | 24 | 49 |
Example 10 | 12 | 17 | 22 | 49 |
Examples 11 to 15
Examples 11 to 15 are different from the preparation method of the bamboo She Xiangliao of example 1 in that the preparation parameters of the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract are different, and the specific preparation parameters of the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract of examples 11 to 15 are shown in the following table 2, which are the same as those of example 1.
TABLE 2 preparation parameters of the first, second and third bamboo leaf extracts of examples 11-15
To further verify the effect of the preparation of the bamboo leaf extract of the present invention on the effect of bamboo She Xiangliao, the present invention conducted the following comparative experiments.
Comparative examples 1 to 6
Bamboo She Xiangliao of comparative examples 1-6 was prepared using bamboo fragrance 1#, bamboo fragrance 2#, bamboo fragrance 3#, and food grade propylene glycol of comparative examples 1-6 bamboo She Xiangliao were as shown in table 3.
TABLE 3 comparative examples 1-6 Components of bamboo She Xiangliao
Bamboo fragrance component | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
Bamboo fragrance 1#/g | 40 | / | / | 20 | 20 | / |
Bamboo fragrance 2#/g | / | 40 | / | 20 | / | 20 |
Bamboo fragrance 3#/g | / | / | 40 | / | 20 | 20 |
Food grade propylene glycol/g | 60 | 60 | 60 | 60 | 60 | 60 |
Comparative examples 7 to 9
The preparation method of the bamboo She Xiangliao of comparative examples 7 to 9 and the preparation method of the bamboo leaf perfume of comparative examples 7 to 9 are different from example 1 in that whether the composition of the extract mixture in the Maillard reaction of step (2) includes the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract or not, and specifically, as shown in the following table 4, other steps are the same as in example 1.
TABLE 4 comparative examples 7-9 bamboo She Xiangliao composition of the extract mixture in the Maillard reaction of step (2)
Extracting the mixture | Comparative example 7 | Comparative example 8 | Comparative example 9 |
Bamboo leaf extract I | Whether or not | Is that | Is that |
Bamboo leaf extract II | Is that | Whether or not | Is that |
Bamboo leaf extract III | Is that | Is that | Whether or not |
Comparative examples 10 to 12
Bamboo She Xiangliao of comparative examples 10 to 12 was prepared, and the bamboo leaf flavor of comparative examples 10 to 12 was different from that of example 1 in whether the molecular distillation of step (3) was performed for the first molecular distillation, the second molecular distillation, and the third molecular distillation, as shown in Table 5, and the other steps were the same as those of example 1.
Table 5 comparative examples 10-12 bamboo She Xiangliao step (3) molecular distillation Process
Comparative example 13
Bamboo She Xiangliao of comparative example 13 was prepared, and the bamboo leaf perfume of comparative example 13 was different from the preparation method of example 1 in that the Maillard reaction of step (2) was not performed, the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract obtained in step (1) were mixed to obtain an extract mixture, and then the extract mixture was directly subjected to the molecular distillation of step (3).
Performance test
The bamboos She Xiangliao prepared in examples 1 to 15 and comparative examples 1 to 13 were weighed out and 28 test samples were prepared as follows.
20g of bamboo She Xiangliao, 8g of organic acid-nicotine salt (containing 20% of nicotine), 22g of propylene glycol and 50g of glycerol were stirred and mixed uniformly to prepare a test sample.
The detection method comprises the following steps: the sensory evaluation of the following items was performed on 28 test specimens by each of 20 professional electronic atomizer sensory evaluators, and the evaluation indexes are shown in table 6 below.
Table 6 evaluation index
The sensory evaluation results of the bamboo leaf fragrances of examples 1 to 15 and the bamboo She Xiangliao of comparative examples 1 to 13 are shown in Table 7 below.
TABLE 7 sensory evaluation results of bamboo She Xiangliao of examples 1-15 and comparative examples 1-13
Detection sample | Bamboo She Xiangqi | Miscellaneous flavor | Tuning of | Sweet taste | Total score |
Example 1 | 4.3 | 4.2 | 4.1 | 3.9 | 16.5 |
Example 2 | 4.1 | 4.3 | 3.9 | 3.8 | 16.1 |
Example 3 | 4.3 | 4.1 | 3.9 | 4.1 | 16.4 |
Example 4 | 4.3 | 4.3 | 3.8 | 3.7 | 16.1 |
Example 5 | 4.2 | 4.5 | 3.9 | 3.9 | 16.5 |
Example 6 | 4.4 | 4.1 | 4.1 | 3.8 | 16.4 |
Example 7 | 4.1 | 4.3 | 4 | 3.9 | 16.3 |
Example 8 | 3.9 | 4.1 | 3.9 | 4.2 | 16.1 |
Example 9 | 3.9 | 4.2 | 3.9 | 4.2 | 16.2 |
Example 10 | 4.2 | 4.1 | 4.1 | 4 | 16.4 |
Example 11 | 4.1 | 4.2 | 4.1 | 3.9 | 16.3 |
Example 12 | 4.1 | 3.9 | 4.2 | 4.2 | 16.4 |
Example 13 | 4.2 | 3.9 | 3.9 | 4.3 | 16.3 |
Example 14 | 3.9 | 4.1 | 3.9 | 4.2 | 16.1 |
Example 15 | 3.8 | 4.2 | 3.9 | 4.2 | 16.1 |
Comparative example 1 | 1.9 | 2.1 | 2.2 | 2.6 | 8.8 |
Comparative example 2 | 2.6 | 2.3 | 2.3 | 2.1 | 9.3 |
Comparative example 3 | 1.9 | 2.5 | 1.9 | 3.5 | 9.8 |
Comparative example 4 | 3.2 | 3.2 | 2.3 | 2.3 | 11.0 |
Comparative example 5 | 1.9 | 2.3 | 2.6 | 3.2 | 10.0 |
Comparative example 6 | 3.1 | 2.1 | 3.5 | 3.1 | 11.8 |
Comparative example 7 | 1.8 | 2.6 | 3.1 | 2.8 | 10.3 |
Comparative example 8 | 2.3 | 2.1 | 3.1 | 2.9 | 10.4 |
Comparative example 9 | 2.1 | 3.2 | 2.9 | 2.8 | 11.0 |
Comparative example 10 | 2.3 | 1.9 | 2.6 | 2.9 | 9.7 |
Comparative example 11 | 2.8 | 1.8 | 2.8 | 3.1 | 10.5 |
Comparative example 12 | 2.6 | 2.3 | 3.1 | 2.5 | 10.5 |
Comparative example 13 | 3.5 | 3.2 | 3.5 | 3.8 | 14.0 |
Fragrance durability test was performed on the bamboo leaf fragrances of examples 1 to 15 and the bamboo She Xiangliao of comparative examples 1 to 13, and the test results are shown in Table 8 below.
TABLE 8 results of fragrance durability test for bamboo She Xiangliao of examples 1-15 and comparative examples 1-13
Detection sample | After 1min, there is no bamboo She Xiangqi | After 2min, there is no bamboo She Xiangqi | After 3min, there is no bamboo She Xiangqi |
Example 1 | Has the following components | Without any means for | Without any means for |
Example 2 | Has the following components | Without any means for | Without any means for |
Example 3 | Has the following components | Has the following components | Without any means for |
Example 4 | Has the following components | Without any means for | Without any means for |
Example 5 | Has the following components | Without any means for | Without any means for |
Example 6 | Has the following components | Has the following components | Without any means for |
Example 7 | Has the following components | Without any means for | Without any means for |
Example 8 | Has the following components | Has the following components | Without any means for |
Example 9 | Has the following components | Has the following components | Has the following components |
Example 10 | Has the following components | Has the following components | Has the following components |
Example 11 | Has the following components | Has the following components | Has the following components |
Example 12 | Has the following components | Has the following components | Has the following components |
Example 13 | Has the following components | Has the following components | Without any means for |
Example 14 | Has the following components | Without any means for | Without any means for |
Example 15 | Has the following components | Without any means for | Without any means for |
Comparative example 1 | Has the following components | Has the following components | Without any means for |
Comparative example 2 | Has the following components | Has the following components | Without any means for |
Comparative example 3 | Has the following components | Has the following components | Without any means for |
Comparative example 4 | Has the following components | Without any means for | Without any means for |
Comparative example 5 | Has the following components | Without any means for | Without any means for |
Comparative example 6 | Has the following components | Without any means for | Without any means for |
Comparative example 7 | Without any means for | Has the following components | Without any means for |
Comparative example 8 | Has the following components | Without any means for | Without any means for |
Comparative example 9 | Without any means for | Without any means for | Without any means for |
Comparative example 10 | Without any means for | Without any means for | Has the following components |
Comparative example 11 | Has the following components | Without any means for | Without any means for |
Comparative example 12 | Has the following components | Without any means for | Without any means for |
Comparative example 13 | Has the following components | Without any means for | Without any means for |
From examples 1 and comparative examples 1 to 13, and in combination with tables 7 and 8, it can be seen that the electronic atomized liquid prepared in comparative example 1 was not affected by the organic acid-nicotine salt smell during the suction, and the front-stage α -caryophyllene, the plant alcohol, the plant essential oil and the like exhibited faint scent, but the rear-stage was able to feel a distinct unpleasant smell, and had slightly astringent and bitter taste in taste, and the suction taste of the electronic atomized liquid was single and uncomfortable.
The electronic atomized liquid prepared in comparative example 2 has faint scent.
The electronic atomized liquid prepared in the comparative example 3 has light fragrance at the early stage of suction, gradually has strong and mellow fragrance at the later stage, has light miscellaneous flavor, and can still feel the flavor fragrance of the bamboo leaves after 1 min.
The electronic atomized liquid prepared in the comparative example 4 has more prominent faint scent at the front stage during suction, but has heavy miscellaneous scent in the scent, and has shorter lasting scent, and the scent cannot be felt after 1 min.
The electronic atomized liquid prepared in the comparative example 5 has obvious distinction between front-stage aroma and rear-stage aroma during suction, and the rear-stage aroma has strong irritation, and the reason is that volatile substances in the rear-stage aroma volatilize in a large amount in a short time, so that the concentration is high, the irritation to the oral cavity and the nasal cavity of a human body is large, and the human body feels uncomfortable.
The electronic atomized liquid prepared in the comparative example 6 has slightly fresh fragrance at the front stage during suction, but the later fragrance is gradually rich, the harmony is better, and the fragrance durability is better.
The electronic atomized liquid prepared in the comparative example 7 has the advantages of light bamboo She Xiangqi in the early stage, no fragrance in the later stage, heavy miscellaneous flavor, obvious astringent taste and bitter taste in sweetness, slightly lack of harmony and short fragrance duration during suction.
The electronic atomized liquid prepared in the comparative example 8 is thin in the early stage of sucking, and is not strong in the later stage, so that the electronic atomized liquid has slightly heavy impurity taste and sweet taste, and is good in harmony.
The electronic atomized liquid prepared in the comparative example 9 has moderate fragrance at the front stage, lighter middle stage, no messy taste, astringent taste, sweet aftertaste and short fragrance duration during the suction.
The electronic atomized liquid prepared in the comparative example 10 has weak bamboo leaf fragrance, less miscellaneous flavor, harmony deficiency, astringent taste and sweet taste, but slightly short sweet taste and light faint scent after 3 min.
The electronic atomized liquid prepared in the comparative example 11 has moderate bamboo She Xiangqi, less miscellaneous flavor, good harmony, sweet taste, no astringent taste and weak fragrance in the later period when being pumped.
The electronic atomized liquid prepared in the comparative example 12 has moderate bamboo She Xiangqi, slightly heavy miscellaneous flavor, good harmony, astringent sweet taste, but no obvious sweet return.
The electronic atomized liquid prepared in the comparative example 13 is rich in bamboo She Xiangqi, free of foreign flavor, good in harmony, sweet and sweet in taste, excellent in overall performance and good in fragrance durability during suction.
The electronic atomized liquid prepared in the embodiment 1 gradually transits the front section fragrance to the strong fragrance during the suction, the fragrance characteristics of each section are obvious, the connection between each section is good, the human body feels comfortable, the three bamboo leaf extracts can form the front-stage sweet fragrance and the later-stage mellow fragrance according to the proportion, the taste is rich, the comfortable feeling can be brought to the user, and meanwhile, the contained active ingredients have better antioxidation, so that the miscellaneous flavor of the electronic atomized liquid is not obvious, and the fragrance of the bamboo leaves can still be felt after 1 min.
From examples 1-15, in combination with tables 7 and 8, it can be seen that the bamboo leaf perfume prepared from three bamboo leaf extracts according to the proportion is added into the electronic atomized liquid, so that the fragrance gradually transiting from faint scent to intense burnt scent can be formed, and the electronic atomized liquid has a rich taste for users, and meanwhile, the electronic atomized liquid has a good taste during suction, can feel slightly sweet at the early stage, returns sweet at the later stage, has rich taste levels, is not easy to oxidize and rancid, has lighter impurity taste and has pure taste.
Finally, it should be noted that: the above examples are not intended to limit the present invention in any way. Modifications and improvements will readily occur to those skilled in the art upon the basis of the present invention. Accordingly, any modification or improvement made without departing from the spirit of the invention is within the scope of the invention as claimed.
Claims (10)
1. The preparation method of the bamboo leaf spice is characterized by comprising the following steps of:
(1) Preparation of bamboo leaf extract
Preparing a bamboo leaf extract I: adding bamboo leaf powder into water, extracting at 80-100 ℃, and separating water from oil after the extraction is finished to obtain a bamboo leaf extract I;
preparing a second bamboo leaf extract: adding the bamboo leaf powder into petroleum ether, extracting at 60-80 ℃, concentrating under reduced pressure after the extraction is finished, washing with absolute ethyl alcohol, and concentrating under reduced pressure to obtain a bamboo leaf extract II;
preparing a bamboo leaf extract III: soaking bamboo leaf powder and cellulase in water, adding water to carry out water extraction at 35-45 ℃ to obtain an extracting solution, concentrating the extracting solution to a specific gravity of 1.3-1.7, adding ethanol, standing, taking supernatant and evaporating to dryness to obtain a bamboo leaf extract III;
(2) Maillard reaction
Mixing the first bamboo leaf extract, the second bamboo leaf extract and the third bamboo leaf extract to obtain an extraction mixture, dispersing the extraction mixture with propylene glycol, adding amino acid and reducing sugar, and mixing and reacting at 60-80 ℃ to obtain a reaction solution;
(3) Molecular distillation
Carrying out first molecular distillation on the reaction liquid obtained in the step (2), wherein the molecular distillation temperature is 30-50 ℃ and the vacuum degree is 5000-8000 Pa, so as to obtain a light component 1# and a heavy component 1#;
taking heavy component 1# to carry out second molecular distillation, wherein the molecular distillation temperature is 50-80 ℃ and the vacuum degree is 1000-3000 Pa, so as to obtain light component 2# and heavy component 2#;
carrying out third molecular distillation on heavy component 2# at the molecular distillation temperature of 80-110 ℃ and the vacuum degree of 18-300 Pa to obtain light component 3# and heavy component 3#;
(4) Mixing light component 1#, light component 2#, light component 3# and solvent to obtain bamboo She Xiangliao.
2. The method of claim 1, wherein in the step (1) of preparing the first bamboo leaf extract, the reflux extraction is performed for 6-8 hours.
3. The method for preparing bamboo leaf spice as defined in claim 1, wherein in the step (1) of preparing the second bamboo leaf extract, reflux extraction is adopted, and the reflux extraction time is 4-5 h.
4. The method for preparing bamboo leaf spice according to claim 1, wherein in the step (1), three specific steps of preparing bamboo leaf extract are that bamboo leaf powder and cellulase are placed in water for soaking for 15-18 h at 26-30 ℃; then adding water for extraction for 2-4 times, extracting at the temperature of 35-45 ℃, filtering, and combining the filtrates to obtain an extracting solution; concentrating the extractive solution to a specific gravity of 1.3-1.7, adding 3-5 times of ethanol, standing for 22-28 h, collecting supernatant, and concentrating under reduced pressure to obtain herba Lophatheri extract III.
5. The method of claim 4, wherein in the step (1) of preparing the third bamboo leaf extract, the weight ratio of the cellulase to the bamboo leaf powder is 1: (4000-6000).
6. The method of claim 1, wherein in step (1), the same amount of the bamboo leaf powder is used to prepare the first bamboo leaf extract, the second bamboo leaf extract, and the third bamboo leaf extract.
7. The method for preparing bamboo leaf flavor according to claim 1, wherein in the step (2), the amino acid is one or more selected from aspartic acid, glutamic acid and proline.
8. The method for preparing bamboo leaf flavor according to claim 1, wherein in the step (2), the reducing sugar is one or more selected from glucose, fructose, and maltose.
9. The method of claim 1, wherein in step (2), the weight ratio of the amino acid to the extract mixture is 1: (20-50); the weight ratio of the reducing sugar to the extraction mixture is 1: (20-50).
10. Bamboo She Xiangliao obtained by the method according to any one of claims 1 to 9, characterized by comprising the following components in percentage by weight:
1#5% -15% of light component;
10% -22% of light component 2#;
18% -28% of light component 3#;
the balance being solvent.
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