CN116622445B - Preparation method, composition and application of oncidium essential oil - Google Patents

Preparation method, composition and application of oncidium essential oil Download PDF

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CN116622445B
CN116622445B CN202310906053.9A CN202310906053A CN116622445B CN 116622445 B CN116622445 B CN 116622445B CN 202310906053 A CN202310906053 A CN 202310906053A CN 116622445 B CN116622445 B CN 116622445B
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oncidium
essential oil
extraction
cigarettes
application
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CN116622445A (en
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田数
赵怡凡
董露
刘永新
王智
李志翔
范大为
王笙
杨婧
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Inner Mongolia Kunming Cigarettes Co ltd
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303Plant extracts other than tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/14Use of materials for tobacco smoke filters of organic materials as additive
    • 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
    • C11B9/02Recovery or refining of essential oils from raw materials
    • 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
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • 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
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
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  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Fats And Perfumes (AREA)

Abstract

The application provides a preparation method, a composition and application of oncidium essential oil, and relates to the technical field of tobacco essence. According to the application, enzymolysis treatment is combined with a flash extraction technology and a supercritical fluid extraction technology for the first time, so that the high-quality oncidium essential oil suitable for cigarettes is obtained. The application also provides a high-stability essential oil composition containing the oncidium essential oil, which can be stored for a long time, and the application of the essential oil composition to cigarettes in preparing the explosive beads can effectively improve the fragrance of the cigarettes, reduce the irritation of smoke, enrich and improve the smoking experience, remarkably improve the sensory quality of the cigarettes and reduce the harm of the cigarettes, is suitable for high-quality cigarettes, and has a certain popularization and application value in the tobacco industry.

Description

Preparation method, composition and application of oncidium essential oil
Technical Field
The application relates to the field of tobacco essence, in particular to a preparation method, a composition and application of oncidium essential oil.
Background
With the increasing attention of people to the relationship between smoking and health, the cigarette tar reduction gradually goes into the vision of consumers. At present, various tar reduction measures are adopted at home and abroad, but new problems are brought, such as poor smoking experience of consumers caused by light smoke, lack of fragrance and the like.
In order to improve the smoking experience of low tar cigarettes, the smoke flavor is often increased by perfuming the cigarettes. The traditional cigarette flavoring mode is to add spice additive into the cut tobacco of the cigarette, thereby achieving the purpose of improving the smoking quality of the smoke, but the reaction of a complex substance system at high temperature is difficult to expect due to the complexity of the smoke of the cigarette, and partial spice has negative influence on the sensory quality of the cigarette. Therefore, it is needed to find a tobacco essence which can be used for low-tar cigarettes and has no stimulation, no miscellaneous gas, good harmony and clean aftertaste.
The oncidium belongs to a double-stem aerial orchid, is one of important cut flowers in the world, and is distributed in the south-middle-south Mei-tropical areas such as Mexico, brazil and Jamaica. At present, most of researches on the oncidium at home and abroad are the volatile component identification and tissue culture researches. Zhang Ying and the like respectively measure the volatile aroma components and the relative contents of different florescence and different positions of flowers of the aromatic hydrographic cymbidium by adopting solid-phase microextraction and gas chromatography-mass spectrometry combined technology, and discuss the changes thereof. Cui Anrong and the like take buds of oncidium at different development periods as explants, and the main factors influencing cluster bud induction, proliferation, rooting and seedling strengthening are studied. ( Reference is made to: [1] zhang Ying, li Xinlei, wang Yan, etc. the change of aroma components of different flowers at different flowering phases [ J ]. Chinese agricultural science, 2011,44 (001): 110-117 [2] Cui Anrong, liu Yunbing, zhang Junchang, etc. the culture of tissue of Wenyan orchid was studied [ J ]. Gardening school newspaper, 2004,31 (2): 253-255. )
At present, no report on the extraction method of the oncidium essential oil suitable for cigarettes exists.
Disclosure of Invention
The application combines enzymolysis treatment with flash extraction technology and supercritical fluid extraction technology for the first time, and aims to provide high-quality oncidium essential oil suitable for cigarettes.
In one aspect, the application provides a method for preparing a oncidium essential oil, which comprises the following steps:
step one, drying and crushing the petals of the oncidium into 40-100 meshes to obtain oncidium powder;
mixing the oncidium powder and water according to the mass ratio of 1 (1-5), stirring to slurry, adding an enzyme preparation, wherein the enzyme preparation comprises cellulase, pectase, ficin, xylanase and beta-glucanase with the enzyme activity ratio of 1-9 to 2-5 to 1-5, and the enzymolysis reaction is carried out at the temperature of 30-60 ℃ and the pH value of 4-7 for 1-5 h to obtain an enzymolysis product;
step three, performing flash extraction on the zymolyte at the temperature of 10-40 ℃ and the rotating speed of 1000-10000 r/min for 1-5 min to obtain an extracting solution;
and step four, extracting the extracting solution by using supercritical fluid to obtain extracting solution, concentrating and inactivating to obtain the oncidium essential oil.
Preferably, the enzyme preparation contains an enzyme activity ratio of 5:4:4:2:3, pectinase, ficin, xylanase and beta-glucanase.
More preferably, the enzyme preparation is a food grade liquid enzyme preparation having an enzyme activity of 5-20 mu/g.
Preferably, the flash extraction is carried out at 25 ℃ and at 6000 r/min for 2 min.
Preferably, the concentration is 50 ℃ concentration and the inactivation is 5 minutes at 100 ℃.
Further, the addition amount of the enzyme preparation is 1-1.5% of the mass of the oncidium powder in percentage by mass.
Preferably, the addition amount of the enzyme preparation is 1.2% of the mass of the oncidium powder.
Further, the flash extraction extractant is 50% -75% ethanol, and the mass ratio of the extractant to the enzymolysis product is (1-10): 1.
preferably, the flash extraction extractant is 70% ethanol, and the mass ratio of the extractant to the enzymolysis product is 5:1.
further, the supercritical fluid extraction temperature is 30-60 ℃, the extraction pressure is 20-35 MPa, the carbon dioxide flow is 15-25 kg/h, and the extraction is 1-5 h.
Preferably, the supercritical fluid extraction temperature is 45 ℃, the extraction pressure is 30 MPa, the carbon dioxide flow is 20 kg/h, and the extraction is 2 h.
Further, the supercritical fluid extraction also comprises a separation step of a separation kettle, wherein the pressure of the separation kettle is 5-10 MPa, and the separation temperature is 50-60 ℃.
Preferably, the pressure of the separation kettle is 6 MPa, and the separation temperature is 55 ℃.
In a preferred embodiment, the preparation method of the oncidium essential oil comprises the following steps:
step one, drying and crushing petals of the oncidium in a full bloom stage to 40-100 meshes to obtain oncidium powder;
mixing the oncidium powder and water according to the mass ratio of 1 (1-5), stirring to slurry, adding an enzyme preparation with the mass of 1-1.5% of the oncidium powder, wherein the enzyme preparation comprises cellulase, pectase, ficin, xylanase and beta-glucanase with the enzyme activity ratio of 1-9 to 2-5 to 1-5, and carrying out enzymolysis reaction of 1-5 h under the conditions that the temperature is 30-60 ℃ and the pH is 4-7 to obtain an enzymolysis product;
step three, placing the zymolyte in a flash extractor, adding 50% -75% ethanol which is 1-10 times of the zymolyte in mass for flash extraction, wherein the extraction temperature is 10-40 ℃, the rotation speed is 1000-10000 r/min, and extracting for 1-5 min to obtain an extracting solution;
and fourthly, placing the extracting solution into a supercritical fluid extraction kettle, extracting at the extracting temperature of 30-60 ℃, the extracting pressure of 20-35 MPa and the carbon dioxide flow of 15-25 kg/h, separating by a separation kettle at the separating pressure of 5-10 MPa, extracting at the separating temperature of 50-60 ℃ for 1-5 h to obtain an extracting solution, concentrating, and inactivating at 100 ℃ for 5 minutes to obtain the oncidium essential oil.
On the other hand, the application also provides the oncidium essential oil prepared by the method.
In another aspect, the application also provides an essential oil composition, which comprises the oncidium essential oil.
Preferably, the weight percentage of the oncidium essential oil in the essential oil composition is 50% -90%; more preferably, 80% -85%.
Further, the essential oil composition further comprises any one or more of the following components: linalool, dihydromyrcenol, phenethyl alcohol, terpineol, cinnamyl alcohol, benzyl acetate, jasmonate, eugenol, methyl anthranilate, methyl dihydrojasmonate, methyl ionone, isoeugenol, heliotropin, dihydrojasmone, linalool acetate, benzyl acetate, vanillin, ethyl vanillin, propylene glycol, glycerol, caprylocaprate.
In a preferred embodiment, the composition comprises the following components in percentage by mass:
80% -85% of oncidium essential oil, 0.1% -1.5% of linalool, 0.1% -3.0% of dihydromyrcenol, 0.05% -0.2% of phenethyl alcohol, 0.1% -2.5% of terpineol, 0.05% -0.6% of cinnamyl alcohol, 0.1% -3.5% of benzyl acetate, 0.1% -2.2% of jasmonate, 0.1% -4.5% of eugenol, 0.1% -5.5% of methyl anthranilate, 0.05% -0.4% of methyl dihydrojasmonate, 0.05% -0.5% of methyl ionone, 0.1% -1.5% of isoeugenol, 0.1% -1.5% of heliotropin, 0.1% -1.5% of dihydrojasmone, 0.1% -1.5% of linalool acetate, 0.1% -1.5% of benzyl acetate, 0.01% -0.05% of vanillin, 0.01% -0.05% of ethyl decanoate, 0.1% -10% of glycerol and 0.15% of glycerin.
In another aspect, the application also provides application of the oncidium essential oil or the essential oil composition in cigarettes.
In a preferred embodiment, the obtained oncidium essential oil prepared by the method and/or the composition can be directly added into tobacco shreds, filter sticks, cigarette paper, forming paper and/or tipping gum.
More preferably, the oncidium essential oil and/or the composition are injected into the explosion beads and then added into the filter stick of the cigarette.
The explosive beads, also called flavor drop pills, brittle capsules and the like, refer to a small liquid bead embedded in a cigarette filter tip, liquid with different types of flavors is wrapped in the small liquid bead, and the explosive bead is an emerging material in the cigarette. Before smoking, a smoker can pinch and explode the cigarette to flow out the liquid in the beads, enrich the taste of the cigarette and improve the smoking quality of the cigarette. Although a certain number and variety of bead-blasted cigarettes exist in the market at present, the flavor substances in the bead-blasted cigarettes often lack of targeted design, have poor harmony with smoke and have great influence on the aroma characteristics of the cigarettes, so that the practical application is limited.
According to the application, the oncidium essential oil and various aromatic substances are combined into the essential oil composition for the cigarette bead blasting for the first time, so that the problems of lack of targeted design and poor smoke harmony of the existing bead blasting are solved. When the essential oil composition is applied to cigarettes, the explosive beads containing the essential oil composition show rich and unique flower fragrance and sweet fragrance, and have the advantages of no stimulation, no miscellaneous gases, good harmony, fine smoke, soft and smooth mouth feel, obvious sweet taste, clean aftertaste and the like. Therefore, the application provides a novel essential oil composition with the effects of enhancing aroma and reducing harm, which can be used in high-quality cigarettes.
In another aspect, the present application also provides a pop-up bead comprising the composition described above; preferably, the explosive bead contains 10-30 μl of the composition; more preferably, the diameter of the explosion beads is 2-4 mm, the weight is 10-25 mg/granule, the roundness is less than 0.15 mm, and the crushing pressure value is 1-1.5 kgf.
In a preferred embodiment, the composition is present in the explosive beads in an amount of 10 to 25. Mu.L/particle; the diameter of the explosive beads is 2.5-3.5 mm, more preferably 2.5 mm, 2.6 mm, 3.0 mm, 3.45 mm, 3.5 mm, preferably 10.5-24.2 mg per particle, and the crushing pressure value is preferably 1.3 kgf.
In actual production operation, specific parameters such as the shape, the size, the specification, the crushing pressure value and the like of the explosion beads can be adjusted according to the specification and the size of the cigarette filter stick to which the explosion beads are added, and the explosion beads can be prepared by using tools, equipment or machines for producing corresponding specifications and the like.
In another aspect, the application also provides a cigarette, which contains the oncidium essential oil or the essential oil composition.
Preferably, the oncidium essential oil and/or the essential oil composition is/are applied to cut tobacco, filter sticks and/or cigarette paper of the cigarettes; or, the filter stick of the cigarette contains at least one explosion bead containing the oncidium essential oil and/or the essential oil composition.
In a preferred embodiment, the bead may be added to a plain cigarette, a binary composite cigarette, and/or a ternary composite cigarette; the location of the bursting beads in the cigarette filter rod is not limited, and is preferably 12-16 mm, more preferably 15 mm, from the lip end; one or more explosion beads can be added into each cigarette.
Preferably, the cigarette has a specification of not limited, and can be a thin, medium or conventional cigarette, or a common cigarette, a binary composite cigarette and/or a ternary composite cigarette, wherein the circumference of the cigarette is preferably 15-30 mm, more preferably 17 mm, 20 mm, 24 mm, 24.3 mm and 27 mm.
The application has the following beneficial effects:
1. according to the preparation method of the oncidium essential oil, the oncidium is subjected to enzymolysis treatment by using a compound enzyme preparation with a proper proportion for the first time, and then a flash extraction technology and a supercritical fluid extraction technology are combined to obtain the high-quality oncidium essential oil suitable for cigarettes;
2. the oncidium essential oil composition provided by the application effectively improves the stability of oncidium essential oil, can effectively improve the fragrance of cigarettes and reduce the harmful components in smoke when being applied to cigarette bursting beads, and is suitable for high-quality cigarettes.
Detailed Description
In order to more clearly illustrate the general concept of the present application, the following detailed description is given by way of example. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present application. It will be apparent, however, to one skilled in the art that the application may be practiced without one or more of these details. In other instances, well-known features have not been described in detail in order to avoid obscuring the application.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer.
Wherein: cellulase, pectinase, ficin, xylanase and beta-glucanase in the enzyme preparation are all purchased from novelin (china) biotechnology limited; preparing explosive beads by using a capsule dripping pill machine for cigarettes, which is provided by the Kataibo Xin pharmaceutical machinery Co-Ltd and has the model of DWJJ; the method comprises the steps of (1) putting explosive beads into a cigarette filter stick by adopting a JK-S1 flavor capsule input device provided by Korean positive light practical company; a cigarette was prepared using a cigarette rolling machine model ZJ17 from Changde tobacco machinery Co.Ltd.
In the following embodiments, unless specified otherwise, the reagents or apparatus used are conventional products available commercially without reference to the manufacturer.
In the following embodiments, the cigarette bursting beads are preferably prepared by a split-liquid dropping method, which includes the steps of dropping after cutting off the glue column by using the shearing force of the opposite impact of cooling oil, and specifically may be: the wall material and core liquid in the dropping process are cut off by utilizing the shearing force formed by two cooling oil with different incidence angles in the solenoid, and are condensed into balls by the action of surface tension in the cooling oil, and then the balls are manufactured into the explosion ball finished product after the procedures of deoiling, drying, screening and the like.
The sensory quality of the cigarette disclosed by the application is referred to in GB 5606.4-2005 part 4: the cigarette sensory quality judgment standard in the sensory technology requirements comprises the following steps: gloss, aroma, harmony, miscellaneous gases, irritation and aftertaste.
Example 1 extraction experiment of essential oil from oncidium
In the embodiment, the extraction method of the oncidium essential oil by combining enzymolysis with supercritical fluid extraction is adopted. The specific extraction method comprises the following steps:
drying and crushing petals of the oncidium in a full bloom stage to 80 meshes to obtain oncidium powder; mixing the oncidium powder and water according to a mass ratio of 1:1, stirring to slurry, adding an enzyme preparation for enzymolysis, and carrying out enzymolysis reaction 2 h under the conditions that the temperature is 45 ℃ and the pH is 5 to obtain an enzymolysis product; placing the zymolyte in a supercritical fluid extraction kettle, extracting with carbon dioxide flow of 15-25 kg/h, separating by a separation kettle, extracting 2 h to obtain extract, concentrating, inactivating at 100deg.C for 5 min to obtain the oncidium essential oil, and the rest conditions are shown in Table 1.
The extraction rate of the oncidium essential oil is calculated as shown in the following table 1.
Wherein: y is the extraction rate of the oncidium essential oil,%; m is the mass of dried oncidium, g; m is m 1 G, for receiving the mass of the dish; m is m 2 G for receiving the quality of the dish and the oncidium essential oil.
TABLE 1
Note that: the enzyme preparation proportion is the enzyme activity ratio; the enzyme preparation is added in the mass percent based on the oncidium.
As can be seen from the results in Table 1, the type, proportion and addition amount of the enzyme preparation in the extraction process of the oncidium essential oil have an influence on the extraction efficiency of the oncidium essential oil. In the supercritical fluid extraction process, the extraction temperature, the extraction pressure, the separation temperature and the separation pressure are also related to the extraction efficiency of the oncidium essential oil.
Preferably, the enzyme activity ratio is selected to be 5:4:4:2:3, cellulase, pectase, ficin, xylanase and beta-glucanase are taken as enzyme preparation components, the addition amount of the cellulase, pectase, ficin, xylanase and beta-glucanase is 1.2 percent of the mass of the oncidium powder, the extraction temperature is selected to be 45 ℃, the extraction pressure is 30 MPa, the pressure of a separation kettle is 6 MPa, and the extraction rate of the oncidium essential oil obtained at the separation temperature of 55 ℃ is highest.
Example 2 method for extracting essential oil of oncidium
The extraction of the oncidium essential oil is carried out under the condition that the preferred extraction rate of the embodiment 1 is highest, and the fact that the oncidium essential oil extracted by the method shows unique floral and sweet fragrance is found in the actual operation process, but the fragrance of the oncidium essential oil is slightly light after being heated at high temperature when the oncidium essential oil is applied to cigarettes, and the fragrance is not obvious when the oncidium essential oil is sucked.
Therefore, in order to increase aroma components in the oncidium essential oil and improve aroma thereof, the present example uses flash extraction to treat oncidium enzymatic hydrolysate in addition to the preferred conditions of example 1.
The specific treatment method comprises the following steps: and (3) placing the zymolyte in a flash extractor for flash extraction to obtain an extracting solution, and performing supercritical fluid extraction on the extracting solution according to the preferred conditions of the embodiment 1 to obtain the oncidium essential oil.
The fragrance of the oncidium essential oil is evaluated by 10 evaluators at the detection port of the sniffer, the fragrance intensity is recorded, the intensity is specifically classified into four grades of 0-3, the final score is obtained by comprehensive scoring of the evaluators, the specific intensity grade is shown in table 2, and the test result is shown in table 3.
TABLE 2
TABLE 3 Table 3
Note that: the multiple is extractant: the mass of the zymolyte is 70% ethanol aqueous solution with the concentration of 70%.
As can be seen from the results in Table 3, the enzymolysis combined flash extraction technology and the supercritical fluid extraction technology can obtain the aromatic flavor while ensuring the high extraction rate, and are suitable for the oncidium essential oil of cigarettes. Wherein, the variety of the extractant, the addition amount of the extractant, the extraction temperature, the extraction time, the rotation speed and the like in the flash extraction process have influence on the aroma quality of the obtained oncidium essential oil. Specifically, in the flash extraction process, the extractant is 70% ethanol which is 5 times of the enzymolysis product in mass, the extraction temperature is 25 ℃, the rotation speed is 6000 r/min, and when the extraction is carried out for 2 min, the aromatic flavor of the oncidium essential oil is rich and the extraction rate is highest and can reach 8.26% at most.
Example 3 essential oil composition
In this example, an essential oil composition comprising the essential oil of oncidium prepared by the preferred post-procedure of example 2 was provided, the specific components of the composition were as follows, and the system stability was observed after the composition was left to stand for 1 week, and the specific observations are shown in table 4.
Composition 1:
85% of oncidium essential oil, 0.5% of linalool, 0.5% of dihydromyrcenol, 0.1% of phenethyl alcohol, 0.5% of terpineol, 0.1% of cinnamyl alcohol, 0.5% of benzyl acetate, 0.5% of jasmonate, 0.5% of eugenol, 0.5% of methyl anthranilate, 0.1% of methyl dihydrojasmonate, 0.1% of methyl ionone, 0.1% of isoeugenol, 0.1% of heliotropin, 0.1% of dihydrojasmone, 0.1% of linalool acetate, 0.1% of benzyl acetate, 0.05% of vanillin, 0.01% of ethyl vanillin, 0.2% of propylene glycol, 5.17% of glycerol and 5.17% of caprylic and capric glyceride.
Composition 2:
84% of oncidium essential oil, 0.5% of linalool, 0.5% of dihydromyrcenol, 0.1% of phenethyl alcohol, 0.5% of terpineol, 0.1% of cinnamyl alcohol, 0.5% of benzyl acetate, 0.5% of jasmonate, 0.5% of eugenol, 0.5% of methyl anthranilate, 0.1% of methyl dihydrojasmonate, 0.1% of methyl ionone, 0.1% of isoeugenol, 0.1% of heliotropin, 0.1% of dihydrojasmone, 0.1% of linalool acetate, 0.1% of benzyl acetate, 0.05% of vanillin, 0.01% of ethyl vanillin, 1.2% of propylene glycol, 5.17% of glycerol and 5.17% of caprylic and capric glyceride.
Composition 3:
85.2% of oncidium essential oil, 0.5% of linalool, 0.5% of dihydromyrcenol, 0.1% of phenethyl alcohol, 0.5% of terpineol, 0.1% of cinnamyl alcohol, 0.5% of benzyl acetate, 0.5% of jasmonate, 0.5% of eugenol, 0.5% of methyl anthranilate, 0.1% of methyl dihydrojasmonate, 0.1% of methyl ionone, 0.1% of isoeugenol, 0.1% of heliotropin, 0.1% of dihydrojasmone, 0.1% of linalool acetate, 0.1% of benzyl acetate, 0.05% of vanillin, 0.01% of ethyl vanillin, 5.17% of glycerol and 5.17% of glyceryl octadecanoate.
Composition 4:
85% of oncidium essential oil, 0.5% of linalool, 0.5% of dihydromyrcenol, 0.1% of phenethyl alcohol, 0.5% of terpineol, 0.1% of cinnamyl alcohol, 0.5% of benzyl acetate, 0.5% of jasmonate, 0.5% of eugenol, 0.5% of methyl anthranilate, 0.1% of methyl dihydrojasmonate, 0.1% of methyl ionone, 0.1% of isoeugenol, 0.1% of heliotropin, 0.1% of dihydrojasmone, 0.1% of linalool acetate, 0.1% of benzyl acetate, 0.05% of vanillin, 0.01% of ethyl vanillin, 0.2% of propylene glycol, 5.17% of glycerol and 5.17% of beta-damascenone.
Blank control group: only the oncidium essential oil is contained.
TABLE 4 Table 4
As can be seen from the results in Table 4, composition 1 has better stability.
Example 4 sensory evaluation and quality evaluation
Test example 1
The embodiment provides a preparation method of the oncidium essential oil, which comprises the following steps:
step one, washing petals of the oncidium in a full bloom stage, removing impurities, airing and drying, and crushing the petals to 80 meshes to obtain oncidium powder;
step two, mixing the oncidium powder and water according to a mass ratio of 1:1, stirring to form slurry, and adding 1.2 g enzyme preparation into each 100. 100 g oncidium powder, wherein the enzyme preparation contains enzyme with an enzyme activity ratio of 5:4:4:2:3, carrying out enzymolysis reaction on the cellulase, pectase, ficin, xylanase and beta-glucanase at the temperature of 45 ℃ and the pH value of 5 to obtain an enzymolysis product 2 h;
step three, placing the zymolyte in a flash extractor, adding 70% ethanol with the mass 5 times of that of the zymolyte for flash extraction, wherein the extraction temperature is 25 ℃, the rotation speed is 6000 r/min, and the extraction is carried out for 2 min to obtain an extracting solution;
and fourthly, placing the extract in a supercritical fluid extraction kettle, extracting at the extraction temperature of 45 ℃ and the extraction pressure of 30 MPa at the carbon dioxide flow rate of 20 kg/h, separating by a separation kettle at the separation temperature of 55 ℃ at the separation pressure of 6 MPa, extracting 2 h to obtain an extract, concentrating at 50 ℃ and inactivating at 100 ℃ for 5 minutes to obtain the oncidium essential oil.
The composition containing the oncidium essential oil comprises the following components in percentage by mass:
85% of oncidium essential oil, 0.5% of linalool, 0.5% of dihydromyrcenol, 0.1% of phenethyl alcohol, 0.5% of terpineol, 0.1% of cinnamyl alcohol, 0.5% of benzyl acetate, 0.5% of jasmonate, 0.5% of eugenol, 0.5% of methyl anthranilate, 0.1% of methyl dihydrojasmonate, 0.1% of methyl ionone, 0.1% of isoeugenol, 0.1% of heliotropin, 0.1% of dihydrojasmone, 0.1% of linalool acetate, 0.1% of benzyl acetate, 0.05% of vanillin, 0.01% of ethyl vanillin, 0.2% of propylene glycol, 5.17% of glycerol and 5.17% of caprylic and capric glyceride.
A bursting bead comprising the composition, prepared by using the split-liquid drop method. Wherein the content of the composition in the explosive beads is 15 mu L/grain, the diameter of the explosive beads is 3 mm, the weight of the explosive beads is 20 mg/grain, the roundness is less than 0.15 mm, and the crushing pressure value is 1.3 kgf.
The cigarette containing the explosion beads is prepared according to the existing cigarette production process. The cigarette is a common cigarette, a circumference 17, mm, a burst bead is placed in a cigarette filter stick, and the burst bead is placed in the middle section of the cigarette filter stick, specifically 15.0 mm away from a lip end.
Test example 2
The test example differs from test example 1 only in that no enzymatic treatment was performed.
Test example 3
The experimental example differs from experimental example 1 only in that the flash extraction technique is replaced by ultrasonic extraction.
Test example 4
The experimental example differs from experimental example 1 only in that the supercritical fluid extraction technique is replaced by a molecular distillation method.
Test example 5
The test example differs from test example 1 only in that the composition was not prepared as a pop-up bead.
Comparative example 1
This comparative example differs from test example 1 only in that the composition does not include the oncidium essential oil.
Cigarette physicochemical property detection experiment
The cigarettes of test examples 1 to 5 and comparative example 1 were measured for the content of harmful components in mainstream smoke before and after burst beads were not broken, respectively, and the cigarette hazard evaluation index, i.e., H value (two decimal places) was calculated, and specific results obtained are shown in table 5.
The calculation method of the cigarette hazard evaluation index (H value) is shown in the following formula.
Wherein: h is a cigarette hazard evaluation index; x is X CO The measured value of the release amount of CO in the main stream smoke of the cigarette; x is X HCN The measured value of the HCN release amount in the main stream smoke of the cigarettes; x is X NH3 Is NH in main stream smoke of cigarette 3 A measured value of the release amount; x is X B[a]P Benzo [ a ] in main stream smoke of cigarette]Actual measurement of pyrene release amount; x is X Phenol (P) Is the actual measurement value of the release amount of phenol in the main stream smoke of the cigarettes; x is X Crotonaldehyde Is the measured value of the release amount of crotonaldehyde in the main stream smoke of cigarettes; x is X NNK Is the actual measurement value of NNK release amount in main stream smoke of cigarettes.
Table 5 evaluation of cigarette hazard in each example
From the data in Table 5, the cigarettes of test example 1 were reduced in the presence of seven harmful components before and after the bursting of the beads.
The conclusion shows that the cigarette containing the composition taking the oncidium essential oil as the main component can effectively reduce the harmful components of main stream smoke generated by burning tobacco during smoking, improve the quality of the cigarette and reduce the harm to human health.
Sensory quality evaluation experiment
33 professional sensory evaluators were randomly drawn to perform sensory quality evaluation on cigarettes obtained in each example. The sensory quality of the cigarette disclosed by the application is referred to in GB 5606.4-2005 part 4: the cigarette sensory quality judgment standard in the sensory technology requirements comprises the following steps: the gloss, fragrance, harmony, miscellaneous odor, irritation and aftertaste, and specific evaluation criteria are shown in Table 6.
Table 6 criteria for judging the sensory quality of cigarettes
The sensory quality of each example cigarette was scored by a professional sensory evaluator according to the sensory quality evaluation criteria of the cigarettes in table 6, and the average value was taken as the final score, and the sensory quality evaluation scoring results of each example cigarette are shown in table 7.
Table 7 sensory quality evaluation of cigarettes obtained by examples
As can be seen from the data in table 7, the cigarettes obtained in test example 1 have a higher multiple score in sensory quality evaluation than those of comparative example 1, indicating that the sensory quality of the cigarettes according to the embodiment of the application is significantly improved. As can be seen from the specific feedback description of the professional sensory evaluator, the sensory feel of the cigarette obtained in test example 1 during smoking is mainly represented by: the richness, fineness and thickness of the smoke are obviously improved, the smoke is more intense and is thoroughly emitted, the fusion degree is better, the fragrance of flower fragrance, sweet fragrance and fruit fragrance is prominent, no stimulation and impurity gas are generated, the harmony is good, the smoke fineness is high, the mouth is soft, the sweet taste is obviously enhanced, and the aftertaste is still clean.
The conclusion shows that when the pop beads prepared from the composition taking the oncidium essential oil as the main component provided by the application are applied to cigarettes, the sensory quality of the cigarettes can be obviously improved, the fragrance is improved, the aftertaste is improved, the irritation and miscellaneous gases of the cigarettes are obviously reduced, and the strong and unique oncidium fragrance and sweetness are shown, which are not possessed by the cigarettes containing other additives.
In summary, according to the preparation method of the oncidium essential oil provided by the application, the oncidium essential oil with high quality suitable for cigarettes can be obtained by adopting the composite enzyme preparation with proper proportion to carry out enzymolysis treatment on the oncidium, and combining the flash extraction technology and the supercritical fluid extraction technology.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are to be included in the scope of the claims of the present application.

Claims (7)

1. A method for preparing a oncidium essential oil, comprising the steps of:
step one, drying and crushing the petals of the oncidium into 40-100 meshes to obtain oncidium powder;
step two, mixing the oncidium powder and water according to a mass ratio of 1:1-5, stirring to slurry, adding an enzyme preparation, wherein the enzyme preparation comprises cellulase, pectase, ficin, xylanase and beta-glucanase with an enzyme activity ratio of 1-9:2-6:2-5:2-5:1-5, and carrying out enzymolysis reaction on the mixture 1-5 h under the conditions that the temperature is 30-60 ℃ and the pH is 4-7 to obtain an enzymolysis product;
step three, performing flash extraction on the zymolyte at the temperature of 10-40 ℃ and the rotating speed of 1000-10000 r/min for 1-5 min to obtain an extracting solution; the flash extraction extractant is 50% -75% ethanol, and the mass ratio of the extractant to the enzymolysis product is 1-10:1, a step of;
step four, extracting the extracting solution by supercritical fluid to obtain extracting solution, concentrating and inactivating to obtain the oncidium essential oil; the supercritical fluid extraction temperature is 30-60 ℃, the extraction pressure is 20-35 MPa, the carbon dioxide flow is 15-25 kg/h, and the extraction is 1-5 h; the supercritical fluid extraction also comprises a separation step of a separation kettle, wherein the pressure of the separation kettle is 5-10 MPa, and the separation temperature is 50-60 ℃.
2. The preparation method according to claim 1, wherein the enzyme preparation is added in an amount of 1-1.5% by mass of the vetiver powder.
3. The oncidium essential oil prepared by the method as claimed in claim 1 or 2.
4. An essential oil composition, characterized in that it comprises the oncidium essential oil of claim 3.
5. The essential oil composition of claim 4, further comprising any one or more of the following ingredients: linalool, dihydromyrcenol, phenethyl alcohol, terpineol, cinnamyl alcohol, benzyl acetate, jasmonate, eugenol, methyl anthranilate, methyl dihydrojasmonate, methyl ionone, isoeugenol, heliotropin, dihydrojasmone, linalool acetate, benzyl acetate, vanillin, ethyl vanillin, propylene glycol, glycerol, caprylocaprate.
6. Use of the oncidium essential oil of claim 3 or the essential oil composition of claim 4 or 5 in cigarettes.
7. A cigarette comprising the oncidium essential oil of claim 3 or the essential oil composition of claim 4 or 5.
CN202310906053.9A 2023-07-24 2023-07-24 Preparation method, composition and application of oncidium essential oil Active CN116622445B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106040118A (en) * 2016-05-11 2016-10-26 南京泽朗医药科技有限公司 A preparing method of a white michelia essence oil microcapsule and applications of the microcapsule in tobacco
CN107760057A (en) * 2017-10-30 2018-03-06 潍坊友容实业有限公司 A kind of Suaeda salsa Betacyanins extracting method
CN111084416A (en) * 2019-11-22 2020-05-01 云南中烟工业有限责任公司 Bitter inhibitor-containing blasting bead for Yunnan gentian-flavored cigarette and preparation method and application thereof
CN115948197A (en) * 2023-03-13 2023-04-11 内蒙古昆明卷烟有限责任公司 Preparation method and application of hemp flower oil
CN115948202A (en) * 2023-03-13 2023-04-11 内蒙古昆明卷烟有限责任公司 Fried dough twist oil, and preparation method, composition and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106040118A (en) * 2016-05-11 2016-10-26 南京泽朗医药科技有限公司 A preparing method of a white michelia essence oil microcapsule and applications of the microcapsule in tobacco
CN107760057A (en) * 2017-10-30 2018-03-06 潍坊友容实业有限公司 A kind of Suaeda salsa Betacyanins extracting method
CN111084416A (en) * 2019-11-22 2020-05-01 云南中烟工业有限责任公司 Bitter inhibitor-containing blasting bead for Yunnan gentian-flavored cigarette and preparation method and application thereof
CN115948197A (en) * 2023-03-13 2023-04-11 内蒙古昆明卷烟有限责任公司 Preparation method and application of hemp flower oil
CN115948202A (en) * 2023-03-13 2023-04-11 内蒙古昆明卷烟有限责任公司 Fried dough twist oil, and preparation method, composition and application thereof

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