CN116676138A - Oncidium essential oil for cigarettes and preparation method and application thereof - Google Patents

Oncidium essential oil for cigarettes and preparation method and application thereof Download PDF

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Publication number
CN116676138A
CN116676138A CN202310911864.8A CN202310911864A CN116676138A CN 116676138 A CN116676138 A CN 116676138A CN 202310911864 A CN202310911864 A CN 202310911864A CN 116676138 A CN116676138 A CN 116676138A
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China
Prior art keywords
oncidium
essential oil
distillation
cigarettes
preparation
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Chinese (zh)
Inventor
田数
董露
赵怡凡
王智
刘永新
李志翔
范大为
王笙
杜赫
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Inner Mongolia Kunming Cigarettes Co ltd
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Inner Mongolia Kunming Cigarettes Co ltd
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Priority to CN202310911864.8A priority Critical patent/CN116676138A/en
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    • 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
    • A24D3/02Manufacture of tobacco smoke filters
    • A24D3/0204Preliminary operations before the filter rod forming process, e.g. crimping, blooming
    • A24D3/0212Applying additives to filter materials
    • A24D3/0216Applying additives to filter materials the additive being in the form of capsules, beads or the like
    • 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
    • C11B9/027Recovery of volatiles by distillation or stripping

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Abstract

The application provides a oncidium essential oil for cigarettes, a preparation method and application thereof, and relates to the technical field of tobacco essence. According to the application, the enzyme-bacterium composite treatment is combined with microwave-assisted steam distillation and molecular distillation for the first time, so that the high-quality oncidium essential oil suitable for cigarettes is obtained. In addition, the oncidium essential oil provided by the application has good stability and can be stored for a long time, and the oncidium essential oil prepared into the explosion beads can be used in cigarettes to effectively improve the fragrance of the cigarettes, reduce the irritation of smoke, enrich and improve the smoking feeling, obviously improve the sensory quality of the cigarettes and reduce the harm of the cigarettes, and is suitable for high-quality cigarettes.

Description

Oncidium essential oil for cigarettes and preparation method and application thereof
Technical Field
The application relates to the field of tobacco essence, in particular to a oncidium essential oil for cigarettes, and a preparation method and application thereof.
Background
With the increasing attention of people to the relationship between smoking and health, a series of tar reduction measures have been adopted at home and abroad, so that the health risk of consumers can be reduced, but new problems such as light smoke, lack of fragrance and the like are brought.
The aragonite belongs to the multiple stem aerial orchids, has unique flower shape and higher ornamental value, the flower color is pure yellow, magenta and pink, or has brown patterns and spots, and the inflorescence is more varied, and is provided with one or two, ten or hundreds of flowers which are upright. At present, most of researches on the oncidium at home and abroad are the volatile component identification and tissue culture researches. The method has little research on the extraction of the oncidium essence, and no report on the extraction method of the oncidium essential oil suitable for cigarettes exists at present.
Disclosure of Invention
The application aims to provide a oncidium essential oil for cigarettes, and a preparation method and application thereof. The preparation process of the oncidium essential oil provided by the application not only can improve the extraction rate of the oncidium essential oil, but also can effectively reduce the content of harmful substances in smoke, and can obviously reduce the irritation of the smoke and improve the sensory quality and quality of the cigarette when the oncidium essential oil is applied to the cigarette in a bead-bursting mode after proper flavoring.
In one aspect, the application provides a method for preparing a oncidium essential oil, which comprises the following steps:
crushing the oncidium petals to 40-100 meshes to obtain oncidium powder;
step two, mixing the oncidium powder with water, adding an enzyme preparation and bacillus subtilis bacterial liquid, and treating 2-8 h at the temperature of 30-60 ℃ and the pH value of 4-7 to obtain oncidium treatment liquid; the enzyme preparation is selected from one or more of hemicellulase, pectinase, trypsin, acid xylanase and beta-glucanase;
performing microwave-assisted steam distillation on the oncidium treatment liquid, heating to 80-100 ℃ with microwave extraction power of 250W, distilling and extracting for 30-90 min, collecting distillate for separating liquid, and reserving upper-layer fractions to obtain a oncidium crude extract;
and step four, carrying out primary and secondary molecular distillation on the crude extract of the oncidium, and merging the primary molecular distillation light component and the secondary molecular distillation light component to obtain the oncidium essential oil.
Preferably, the microwave-assisted steam distillation is carried out, the temperature is heated to 100 ℃, and the distillation and extraction are carried out for 70 min.
Preferably, the fourth step further comprises a step of inactivation, wherein the inactivation is performed at 100 ℃ for 5 minutes.
Furthermore, the enzyme preparation is hemicellulase, pectase, trypsin, acid xylanase and beta-glucanase with the enzyme activity ratio of (1-9) (2-6) (2-5) (1-5).
Preferably, the enzyme preparation is hemicellulase, pectinase, trypsin, acid xylanase and beta-glucanase with the enzyme activity ratio of 5:3:3:2:4.
More preferably, the enzyme preparation is a food grade liquid enzyme preparation having an enzyme activity of 5-20 mu/g.
Further, the addition amount of the enzyme preparation is 1-1.5% of the mass of the powder of the oncidium, and the addition amount of the bacillus subtilis strain liquid is 0.1-0.5% of the mass of the powder of the oncidium.
Preferably, the addition amount of the enzyme preparation is 1% of the mass of the vetiver powder, and the addition amount of the bacillus subtilis strain liquid is 0.1% of the mass of the vetiver powder.
Further, the bacillus subtilis in the bacillus subtilis liquid is bacillus subtilis CICC24406, and the bacillus subtilis liquid OD 600 The value is 3-4.
Preferably, the bacillus subtilis in the bacillus subtilis liquid is bacillus subtilis CICC24406 and bacillus subtilis liquid OD 600 The value is 3.
The bacillus subtilis is bacillus subtilis [ (]Bacillus subtilis subsp. Subtilis) CICC24406, which is purchased from China center for type culture Collection of microorganisms.
Further, the mass ratio of the oncidium powder to the water is 1 (8-20).
Preferably, the mass ratio of the oncidium powder to the water is 1:10.
Further, the distillation pressure of the primary molecular distillation is 0.1-10 Pa, the sample injection temperature is 60-70 ℃, the distillation temperature is 100-130 ℃, the condensation temperature is 20-40 ℃, the distillation pressure of the secondary molecular distillation is 0.1-10 Pa, the sample injection temperature is 50-70 ℃, the distillation temperature is 150-170 ℃, and the condensation temperature is 60-70 ℃.
Preferably, the distillation pressure of the primary molecular distillation is 5 Pa, the sample introduction temperature is 60 ℃, the distillation temperature is 130 ℃, the condensation temperature is 25 ℃, the distillation pressure of the secondary molecular distillation is 5 Pa, the sample introduction temperature is 50 ℃, the distillation temperature is 160 ℃, and the condensation temperature is 60 ℃.
According to the application, the method of combining the enzyme-bacteria composite preparation with microwave-assisted steam distillation is adopted for the first time to extract the oncidium essential oil, so that the extraction efficiency of the oncidium essential oil is effectively improved, and the problem of overlong microwave-assisted steam distillation extraction time is solved by firstly adopting the enzyme bacteria to treat the oncidium powder. Moreover, the obtained oil has special creamy fragrance, and has good fragrance. The application further adopts molecular distillation to further process and obtain the high-quality oncidium essential oil. The high-quality oncidium essential oil has the characteristics of good stability and rich fragrance, is suitable for the manufacturing process of cigarette bursting beads, and can reduce the content of harmful substances in smoke while improving the smoking experience of a user.
In a preferred embodiment, the preparation method of the Chinese magnolia essential oil comprises the following steps:
crushing the oncidium petals to 40-100 meshes to obtain oncidium powder;
mixing the oncidium powder with water according to a mass ratio of 1 (8-20), adding an enzyme preparation with a mass ratio of 1% -1.5% of the oncidium powder and 0.1% -0.5% of bacillus subtilis liquid, wherein the enzyme preparation comprises hemicellulase, pectase, trypsin, acid xylanase and beta-glucanase with an enzyme activity ratio of (1-9) (2-6) (2-5) (1-5), and treating 2-8 h under the conditions that the temperature is 30-60 ℃ and the pH is 4-7 to obtain the oncidium treatment liquid;
step three, carrying out microwave-assisted steam distillation on the oncidium treatment liquid under normal pressure, heating to 80-100 ℃ with microwave extraction power of 250W, distilling and extracting for 30-90 min, collecting distillate for liquid separation, and reserving upper-layer fractions to obtain a oncidium crude extract;
and fourthly, carrying out primary and secondary molecular distillation on the crude extract of the oncidium, wherein the distillation pressure of the primary molecular distillation is 0.1-10 Pa, the sample injection temperature is 60-70 ℃, the distillation temperature is 100-130 ℃, the condensation temperature is 20-40 ℃, the distillation pressure of the secondary molecular distillation is 0.1-10 Pa, the sample injection temperature is 50-70 ℃, the distillation temperature is 150-170 ℃, the condensation temperature is 60-70 ℃, and the high-quality oncidium essential oil is obtained by inactivating the primary molecular distillation light component and the secondary molecular distillation light component at 100 ℃ for 5 min after the primary molecular distillation light component and the secondary molecular distillation light component are combined.
The preparation method of the bacillus subtilis bacterial liquid comprises the following steps: inoculating Bacillus subtilis CICC24406 into 50 mL LB liquid medium, culturing at 20-40deg.C and 100-200 r/min for 24-72 hr, and OD 600 The value is 3-4.
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 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.
On the other hand, the application also provides the application of the oncidium essential oil or the essential oil composition in preparing 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.
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. the application provides a preparation method of oncidium essential oil suitable for cigarettes, which combines enzyme and fungus compound treatment with microwave-assisted steam distillation and molecular distillation for the first time, and can extract oncidium essential oil with high efficiency and obtain high-quality oncidium essential oil suitable for cigarettes;
2. the oncidium essential oil provided by the application can be stored for a long time, has excellent stability, can be prepared into burst beads for use in cigarettes, can effectively improve the fragrance of the cigarettes, reduce the irritation of smoke, enrich and improve the smoking feeling, obviously improve the sensory quality of the cigarettes, reduce the harm of the cigarettes, 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, hemicellulase, pectase, trypsin, acid xylanase and beta-glucanase in the enzyme preparation are all purchased from Norwestine (China) biotechnology Co., ltd; bacillus subtilis @Bacillus subtilis subsp. Subtilis) CICC24406 is purchased from China center for type culture Collection of Industrial microorganisms; 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 Single factor experiment for extracting essential oil from Vanilla by enzyme-bacteria Complex formulation
In the embodiment, the combination of enzyme and fungus compound preparation treatment and microwave-assisted steam distillation is adopted for the first time to extract the oncidium essential oil. The specific extraction method comprises the following steps:
washing the oncidium flower petals, removing impurities, airing, and crushing to 60 meshes in liquid nitrogen to obtain oncidium powder; mixing the oncidium powder with distilled water, adding an enzyme preparation and bacillus subtilis zymotic fluid, and treating 5 h at 35 ℃ and pH of 4 to obtain oncidium treatment fluid; placing the oncidium treatment liquid in a round bottom flask, connecting a condensing device and a collecting device, performing microwave-assisted steam distillation under normal pressure, setting the microwave extraction power to be 250W, collecting distillate after distillation and extraction for 70 min, separating the distillate in a separating funnel, and reserving the upper layer fraction to obtain oncidium essential oil, wherein the extraction time is calculated according to the time that the content of the oncidium essential oil is not increased, and the rest conditions are shown in Table 2.
The preparation method of the bacillus subtilis bacterial liquid comprises the following steps: inoculating Bacillus subtilis CICC24406 into 50 mL LB liquid medium, culturing at 37deg.C and 150 r/min to OD 600 When the value is 3-4 (about 48 h), the biological activity of the bacillus subtilis in the bacterial liquid is higher.
The extraction rate of the oncidium essential oil is calculated as shown in the following table 2.
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.
And, 10 evaluators evaluate the fragrance of the obtained oncidium essential oil 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 score of the evaluators, the specific intensity grade is shown in table 1, and the test result is shown in table 2.
TABLE 1
TABLE 2
Note that: the enzyme preparation proportion is the enzyme activity ratio; the addition amount of the enzyme preparation and the addition amount of the bacterial liquid are the addition amount of the oncidium per 100 g.
From the results in table 2, it is demonstrated in this example that the combination of enzyme and bacterial complex treatment and microwave assisted steam distillation can be used to extract the essential oil of oncidium.
Preferably, hemicellulase, pectase, trypsin, acid xylanase and beta-glucanase with the enzyme activity ratio of 5:3:3:2:4 are selected as enzyme preparations, the addition amount of the hemicellulase, pectase, trypsin, acid xylanase and beta-glucanase is 1% of the mass of the powder of the oncidium, the addition amount of the bacillus subtilis zymotic bacteria liquid is 0.1% of the mass of the powder of the oncidium, and when the microwave-assisted steam distillation collection temperature is 100 ℃, the extraction rate of the oncidium essential oil is highest, the extraction time is relatively short, and the odor intensity is high.
Example 2 Single factor experiment for extracting essential oil of oncidium by molecular distillation
However, in the actual operation process, the essential oil aroma prepared in the embodiment 1 is still difficult to mask smoke when being applied to cigarettes, and the aroma is not strong enough. In addition, the oncidium essential oil has the problem of poor stability during long-term storage, and a method for preparing a bead explosion product stably stored in a growth period is unavailable.
The molecular distillation method was selected in this example to solve the above-mentioned problems. The molecular distillation treatment is continued on the basis of the preferred conditions of the example 1 to obtain the high-quality oncidium essential oil, and the specific operation comprises the following steps:
the product under the preferred conditions of the embodiment 1 is added into molecular distillation equipment for primary molecular distillation and secondary molecular distillation, wherein the primary molecular distillation is carried out under the conditions of different distillation pressures and distillation temperatures, the sample injection temperature is 60 ℃, the condensation temperature is 25 ℃, the secondary molecular distillation is carried out under the conditions of different distillation pressures and distillation temperatures, the sample injection temperature is 50 ℃, the condensation temperature is 60 ℃, and the primary molecular distillation light component and the secondary molecular distillation light component are combined, so that the high-quality oncidium essential oil is obtained. The odor intensity was determined as described in example 1. The stability of the oncidium was measured by allowing the oncidium essential oil to stand at normal temperature and pressure for 1 month, and the system stability was observed, and the observation results are shown in table 3.
TABLE 3 Table 3
As can be seen from the results in table 3, in this example, it is demonstrated that in the process of extracting the essential oil from the oncidium by using the enzyme-bacteria complex preparation in combination with the microwave-assisted steam distillation method and the molecular distillation method, the optimal preparation condition in the molecular distillation method is that the first-order molecular distillation is performed under the conditions of a distillation pressure of 5 Pa, a sample injection temperature of 60 ℃, a distillation temperature of 130 ℃, a condensation temperature of 25 ℃, and a second-order molecular distillation is performed under the conditions of a distillation pressure of 5 Pa, a sample injection temperature of 50 ℃, a distillation temperature of 160 ℃, and a condensation temperature of 60 ℃. The obtained oncidium essential oil has good stability, strong fragrance, obvious cream sweet fragrance and suitability for preparing cigarette pop beads.
Example 3 experiment for physical and chemical Properties detection and sensory quality evaluation of cigarette
Test example 1
The experimental example provides a preparation method of the oncidium essential oil, which comprises the following steps:
washing the oncidium petals, removing impurities, airing, and crushing in liquid nitrogen to 60 meshes to obtain oncidium powder;
mixing the oncidium powder and distilled water according to a mass ratio of 1:10, stirring to form slurry, adding 1 g enzyme preparation and 100 mu L of bacillus subtilis bacterial liquid into each 100g oncidium powder, wherein the enzyme preparation is a compound enzyme containing hemicellulase, pectase, trypsin, acid xylanase and beta-glucanase with an enzyme activity ratio of 5:3:3:2:4, and treating 5 h under the conditions that the temperature is 35 ℃ and the pH value is 4 to obtain oncidium treatment liquid;
placing the oncidium treatment liquid in a round bottom flask, connecting a condensing device and a collecting device, performing microwave-assisted steam distillation under normal pressure, setting the microwave extraction power to be 250W, observing that oily fractions are distilled when the oncidium treatment liquid is heated to 100 ℃, collecting distillate after distillation and extraction for 70 min, separating the distillate in a separating funnel, and reserving the upper fraction to obtain the oncidium crude extract;
and step four, adding the crude extract of the oncidium into molecular distillation equipment to carry out primary and secondary molecular distillation, wherein the primary molecular distillation is carried out under the conditions of a distillation pressure of 5 Pa, a sample injection temperature of 60 ℃, a distillation temperature of 130 ℃ and a condensation temperature of 25 ℃, the secondary molecular distillation is carried out under the conditions of a distillation pressure of 5 Pa, a sample injection temperature of 50 ℃, a distillation temperature of 160 ℃ and a condensation temperature of 60 ℃, and the primary molecular distillation light component and the secondary molecular distillation light component are combined and inactivated at 100 ℃ for 5 min to obtain the high-quality oncidium essential oil.
The bacillus subtilis is bacillus subtilis [ (]Bacillus subtilis subsp. Subtilis) CICC24406, which is purchased from China center for type culture Collection of microorganisms.
The preparation method of the bacillus subtilis bacterial liquid comprises the following steps: inoculating bacillus subtilis CICC24406 into50 mL LB liquid medium, 37 ℃,150 r/min, 48 h of culture, OD 600 The value is 3.
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 test example differs from test example 1 only in that no bacterial liquid was added.
Test example 4
The test example differs from test example 1 only in that the microwave-assisted steam distillation was replaced by molecular ultrasound-assisted steam distillation.
Test example 5
The test example differs from test example 1 only in that molecular petroleum ether leaching is used instead of molecular distillation.
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 the specific results obtained are shown in table 4.
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 4 evaluation of cigarette hazard in each example
From the data in Table 4, the cigarettes of test example 1 were significantly reduced in the presence of seven harmful components before and after bead bursting.
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 5.
Table 5 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 5, 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 6.
Table 6 sensory quality evaluation of cigarettes obtained in each example
As can be seen from the data in table 6, 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.
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 (10)

1. A method for preparing a oncidium essential oil, comprising the steps of:
crushing the oncidium petals to 40-100 meshes to obtain oncidium powder;
step two, mixing the oncidium powder with water, adding an enzyme preparation and bacillus subtilis bacterial liquid, and treating 2-8 h at the temperature of 30-60 ℃ and the pH value of 4-7 to obtain oncidium treatment liquid; the enzyme preparation is selected from one or more of hemicellulase, pectinase, trypsin, acid xylanase and beta-glucanase;
performing microwave-assisted steam distillation on the oncidium treatment liquid, heating to 80-100 ℃ with microwave extraction power of 250W, distilling and extracting for 30-90 min, collecting distillate for separating liquid, and reserving upper-layer fractions to obtain a oncidium crude extract;
and step four, carrying out primary and secondary molecular distillation on the crude extract of the oncidium, and merging the primary molecular distillation light component and the secondary molecular distillation light component to obtain the oncidium essential oil.
2. The preparation method according to claim 1, wherein the enzyme preparation is hemicellulase, pectase, trypsin, acid xylanase and beta-glucanase with an enzyme activity ratio of (1-9): (2-6): (2-5): (2-5): (1-5).
3. The preparation method of claim 1, wherein the enzyme preparation is added in an amount of 1-1.5% of the mass of the powder of the vetiver, and the bacillus subtilis liquid is added in an amount of 0.1-0.5% of the mass of the powder of the vetiver.
4. The preparation method of claim 1, wherein the bacillus subtilis in the bacillus subtilis liquid is bacillus subtilis CICC24406 and bacillus subtilis liquid OD 600 The value is 3-4.
5. The preparation method according to claim 1, wherein the mass ratio of the oncidium powder to the water is 1 (8-20).
6. The process of claim 1, wherein the primary molecular distillation is carried out at a distillation pressure of 0.1 to 10 Pa, a sample introduction temperature of 60 ℃ to 70 ℃, a distillation temperature of 100 ℃ to 130 ℃, a condensation temperature of 20 ℃ to 40 ℃, a distillation pressure of 0.1 to 10 Pa, a sample introduction temperature of 50 ℃ to 70 ℃, a distillation temperature of 150 ℃ to 170 ℃, and a condensation temperature of 60 ℃ to 70 ℃.
7. The oncidium essential oil prepared by the method as claimed in any one of claims 1-6.
8. An essential oil composition, wherein the essential oil composition comprises the oncidium essential oil of claim 7.
9. Use of the oncidium essential oil of claim 7 or the essential oil composition of claim 8 in the preparation of cigarettes.
10. A cigarette comprising the oncidium essential oil of claim 7 or the essential oil composition of claim 8.
CN202310911864.8A 2023-07-25 2023-07-25 Oncidium essential oil for cigarettes and preparation method and application thereof Pending CN116676138A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106262654A (en) * 2016-08-11 2017-01-04 广州市名花香料有限公司 Cheese powdered flavor and preparation method thereof
CN107227204A (en) * 2017-08-04 2017-10-03 云南中烟新材料科技有限公司 A kind of cichory root tobacco aromaticss and its preparation method and application
CN109953367A (en) * 2019-03-22 2019-07-02 内蒙古昆明卷烟有限责任公司 A kind of Herba Cistanches extracting solution and preparation method thereof, composition and application
CN113974205A (en) * 2021-10-26 2022-01-28 河南中烟工业有限责任公司 Blueberry essence, blueberry extract, and preparation methods and applications thereof
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
CN106262654A (en) * 2016-08-11 2017-01-04 广州市名花香料有限公司 Cheese powdered flavor and preparation method thereof
CN107227204A (en) * 2017-08-04 2017-10-03 云南中烟新材料科技有限公司 A kind of cichory root tobacco aromaticss and its preparation method and application
CN109953367A (en) * 2019-03-22 2019-07-02 内蒙古昆明卷烟有限责任公司 A kind of Herba Cistanches extracting solution and preparation method thereof, composition and application
CN113974205A (en) * 2021-10-26 2022-01-28 河南中烟工业有限责任公司 Blueberry essence, blueberry extract, and preparation methods and applications thereof
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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