CN114214117B - Method for improving limonene release balance in bergamot oil essence - Google Patents

Method for improving limonene release balance in bergamot oil essence Download PDF

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Publication number
CN114214117B
CN114214117B CN202111521181.9A CN202111521181A CN114214117B CN 114214117 B CN114214117 B CN 114214117B CN 202111521181 A CN202111521181 A CN 202111521181A CN 114214117 B CN114214117 B CN 114214117B
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China
Prior art keywords
bergamot oil
limonene
oil essence
essence
emulsifier
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CN202111521181.9A
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CN114214117A (en
Inventor
唐丽
廖头根
张翼鹏
王猛
王坚
周冰
唐军
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China Tobacco Yunnan Industrial Co Ltd
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China Tobacco Yunnan Industrial Co Ltd
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    • 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
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention discloses a method for improving the release balance of limonene in bergamot oil essence and a method for reducing the limonene loss rate of bergamot oil essence after a high-temperature silk drying process. Compared with the direct addition of bergamot oil essence, the liquid bergamot oil essence added in the cut tobacco can be more suitable for the high-temperature cut tobacco baking process in the cigarette processing process, and the loss rate of limonene is lower than that of the bergamot oil essence, so that the bergamot oil essence can be more reserved in a cigarette product. Meanwhile, after the liquid bergamot oil essence added into the tobacco shreds is combusted in the tobacco shreds, the transfer rate of the limonene in the first half section and the second half section of the tobacco is not obviously different, which indicates that the limonene is released more uniformly. The evaluation result shows that the cigarette sample rolled in the cut tobacco is added, the front and rear sections of the whole sample smoking experience are balanced and stable, and the comfort is obviously improved.

Description

Method for improving limonene release balance in bergamot oil essence
Technical Field
The invention belongs to the field of tobacco industry application, and particularly relates to a method for improving limonene release balance in bergamot oil essence.
Background
Limonene, also known as limonene, dipentene and the like, is a natural monoterpene widely existing in Rutaceae plants, such as bergamot, is rich in limonene, has pleasant lemon flavor fragrance, and has great potential and economic value as a natural substance because of the functions of bacteriostasis, corrosion resistance, oxidation resistance, flavoring and the like. The essence rich in limonene is added into the cigarette, so that the product has limonene, and the cigarette product also has the functional characteristic of limonene. At present, most domestic cigarette enterprises hope to increase the content of limonene in cigarette products by adding essence rich in high content of limonene in cigarette production. However, from the practical situation, simply improving the content of the limonene in the cigarette cannot well improve the quality of the final product, because the limonene is not only required to be added in the cigarette, but also the transfer balance of the limonene in the combustion process of the cigarette needs to be considered, if the balance is poor, the suction feeling of the final product also has larger fluctuation, so that the consumption experience is affected, and the transfer balance means the consistency of the limonene in the mouth-by-mouth smoke in the combustion process of the cigarette, the better the balance is, the uniform release of the limonene in different suction stages before, during and after the suction feeling is not generated, and the sensory evaluation is high.
Therefore, if the functional characteristics of the limonene are expected to be well applied to the cigarette products, the problem that the limonene content in the cigarettes is not simply improved is solved, but the important attention is paid to how to uniformly release the limonene in the cigarette combustion process after the limonene content in the cigarettes is improved, and the reason that the limonene transfer balance in the cigarette products is poor is that the tobacco shreds need to be combusted, the limonene is sucked along with the main stream smoke gradually, and the added limonene-rich essence cannot be gradually released at the moment, so that the requirement of the tobacco shred combustion process on the essence release balance cannot be met, the problem that the limonene transfer balance is poor is caused, the functional characteristics of the limonene cannot be well exerted, the quality fluctuation of the cigarette products is large, and the cigarette products cannot be well improved.
In addition, the cigarette processing process has a high-temperature treatment process, and if bergamot oil essence is directly added in the prior art, the bergamot oil essence has higher limonene loss rate after the high-temperature cut tobacco baking process.
Therefore, it is important to develop a method for releasing limonene in bergamot oil essence in a balanced manner in the field of cigarette industry and a method for reducing the limonene loss rate of bergamot oil essence after a high-temperature cut tobacco baking process.
The present invention has been made in view of the above problems.
Disclosure of Invention
The invention provides a method for improving the release balance of limonene in bergamot oil essence, which comprises the following steps of preparing the bergamot oil essence into liquid bergamot oil essence;
the preparation method comprises the following steps:
(1) Adding a certain amount of bergamot oil, an emulsifier and an auxiliary emulsifier into a glass container, stirring at a constant speed, and simultaneously adding deionized water;
(2) And (3) adopting a high-speed centrifuge to centrifuge the mixed solution in the step (1) at a high speed under 3800-4500rmp for 30-50min until the mixed solution is in a transparent state, so as to obtain the liquid bergamot oil essence.
Preferably, in step (1), the emulsifier includes, but is not limited to, tween 20, tween 40, tween 60, and the co-emulsifier includes, but is not limited to, absolute ethanol, n-propanol, n-butanol, n-hexanol, n-octanol.
Preferably, in step (1), the hydrophilic-lipophilic balance (HLB value) of the emulsifier is important for the formation of the liquid bergamot oil flavour, and the emulsifier needs to be selected in combination with the stability of the mixed solution.
Preferably, in the step (1), the ratio of the mass of the emulsifier to the mass of the co-emulsifier (Km value) is also important for the formation of the liquid bergamot oil flavour, the Km value of the present invention should be limited to 2-3:1.
Preferably, in the step (1), the bergamot oil is used in an amount of 13% -15% based on the whole mass ratio.
The second aspect of the invention provides an application of the liquid bergamot oil essence prepared by the method of the first aspect of the invention in cigarettes, wherein the liquid bergamot oil essence is added into cut tobacco of the cigarettes, and the adding proportion is 3% -5% of the mass of the cut tobacco.
According to a third aspect of the present invention there is provided a method of reducing the limonene loss rate of bergamot oil flavour following a high temperature cut tobacco drying process, characterised in that according to the first aspect of the invention there is provided a method of preparing bergamot oil flavour as a liquid and adding it to cut tobacco of cigarettes according to the second aspect of the invention.
Wherein, under the experimental set process parameters of the yarn drying, the loss rate of the limonene is measured.
The peak area of the limonene is detected by adopting GC, and the transfer rate (T) of the limonene in the cut tobacco added with the liquid bergamot oil essence is calculated according to the following formula.
Wherein:
A 1 -peak area of limonene in cut tobacco sample;
A 2 -peak area of limonene in the mouth-by-mouth smoke total particulate matter sample;
B 1 -peak area of internal standard in cut tobacco sample;
B 2 -peak area of internal standard in total particulate matter sample of mouth-by-mouth flue gas.
The tobacco shreds added with the liquid bergamot oil essence are rolled, and cigarette samples are subjected to smoking evaluation, so that three aspects of aroma, smoke and taste characteristics are mainly examined.
The emulsion state stability referred to in the present invention means the stability of the product to maintain the emulsion in this state.
Compared with the prior art, the invention has the following beneficial effects:
1. compared with the liquid bergamot oil essence added directly in the tobacco shreds, the bergamot oil essence has the advantages that the loss rate of limonene of the bergamot oil essence is 68.82% under the experimentally set process parameters, and the loss rate of limonene of the liquid bergamot oil essence is 34.31%, so that the liquid bergamot oil essence can be more suitable for high-temperature treatment in the cigarette processing process, the loss rate of limonene is lower than that of the bergamot oil essence, and the functional characteristics of limonene can be more effectively exerted in cigarette products.
2. Compared with the direct addition of bergamot oil essence, the liquid bergamot oil essence added in the cut tobacco disclosed by the invention is more suitable for the requirement of the burning process of the cut tobacco on the release balance of limonene, after the burning process of the cut tobacco, the accumulated release rate of the first half section of limonene of a rolled sample of the cut tobacco with the bergamot oil essence is higher than that of the second half section of limonene, the transfer rates of the first half section and the second half section of limonene of the cut tobacco with the liquid bergamot oil essence are obviously different, and the release rate of the limonene of the sample of the liquid bergamot oil essence is more balanced than that of the sample with the bergamot oil essence.
3. Compared with the cigarette sample prepared by directly adding the bergamot oil essence, the cigarette sample prepared by the liquid bergamot oil essence added in the cut tobacco has the advantages that the aroma is sufficient, the comfort is obviously improved, and the whole sample is balanced and stable in smoking feeling front and back.
Drawings
Without any means for
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
(1) Adding bergamot oil 15%, tween 60 and absolute ethanol into a glass container, stirring at constant speed, and simultaneously adding deionized water.
Tween 60 was selected as the emulsifier taking into account both the hydrophilic-lipophilic balance (HLB value) of the emulsifier and the stability of the emulsion (see table 1).
The ratio km=2:1 of tween 60 mass to absolute ethanol mass.
The method for measuring the state stability of the emulsion comprises the following steps: and (3) centrifuging, namely respectively carrying out centrifugal test on various emulsion, taking a certain amount of various finished products in a centrifuge tube, centrifuging at 4000r/min for 10min to measure the heights occupied by the oil and emulsion layers, dividing the number of the occupied emulsion layers by the total number of the emulsion layers, and obtaining the actual emulsion degree of the emulsion, wherein the ratio is in the range of 0-1, and the higher the ratio is, the better the emulsion state stability is.
(2) And (3) adopting a high-speed centrifuge, and centrifuging the mixed solution in the step (1) at a high speed under 4200rmp for 40min until the mixed solution is in a transparent state, so as to obtain the liquid bergamot oil essence.
The liquid bergamot oil essence prepared by the steps is added into cut tobacco according to the proportion of 4%, and the loss rate of limonene is measured under the experimentally set cut tobacco baking process parameters. And secondly, calculating the mouth-by-mouth smoke transfer rate of the limonene in the cut tobacco added with the liquid bergamot oil essence. And finally, evaluating the cigarette samples. The results are shown in tables 2, 3, 4 and 5.
Comparative example
The bergamot oil essence is directly added into the tobacco shreds according to the proportion of 4 percent.
Example 2
As in the example procedure, T20 was chosen as the emulsifier.
Example 3
The ratio Km of the mass of the emulsifier to the mass of the co-emulsifier was set to 1:1 as in the example procedure.
Example 4
The ratio Km of the mass of the emulsifier to the mass of the co-emulsifier was set to 3:2 as in the example procedure.
TABLE 1 influence of different emulsifier HLB values on emulsion State stability
Table 2 loss rate of limonene during silk drying in examples and comparative examples
TABLE 3 transfer rate of limonene from mouth to mouth smoke in tobacco shred (%)
Table 4 analysis of variance of the limonene transfer rates in the first half and the second half of the examples and comparative examples
F Critical value F
Example 1 5.136 7.709
Example 2 7.179 7.709
Example 3 7.593 7.709
Example 4 6.559 7.709
Comparative example 9.239 7.709
Table 5 sensory evaluation of suction results comparison
As can be seen from Table 1, the HLB value and emulsion state stability of T60 are significantly higher than T20.
As can be seen from table 2, the loss rate of limonene in the process of drying the shreds in example 1 is significantly lower than that in other examples and comparative examples, which shows that the bergamot oil essence is made into liquid bergamot oil essence according to the method of the present invention, which can indeed reduce the limonene loss rate of bergamot oil essence after the high temperature shred drying process. In addition, the selection of the emulsifier, the ratio of the mass of the emulsifier to the mass of the auxiliary emulsifier is critical to the limonene loss rate of the bergamot oil essence after the high-temperature tobacco shred baking process, and the invention can meet the requirements of high-temperature treatment in cigarette processing.
As can be seen from tables 3 and 4, according to the transfer condition of the limonene in the total particulate matters of the smoke from 1 to 7 mouths, in order to further analyze the release balance of the limonene in the smoke of cigarettes, the 2 nd to 4 th mouths are taken as the first half section and the 5 th to 7 th mouths are taken as the second half section, single-factor analysis of variance is carried out on the transfer rate data of the limonene in the smoke of the first half section and the second half section, the variance of the embodiment 1 is 5.14 and is smaller than a critical value, which indicates that the transfer rates of the first half section and the second half section of the limonene of the embodiment 1 have no significant difference, the release of the limonene is more balanced than that of the comparative example in the burning process of cut tobacco, and although the variances of other embodiments are smaller than the critical value, the loss rate of other embodiments is higher in the high-temperature treatment process. Considering the emulsifier used in example 1 of the present invention, the ratio of the mass of the emulsifier to the mass of the co-emulsifier is more suitable.
As can be seen from table 5, the scores of the cigarette samples prepared in example 1 in the aroma characteristics, the smoke characteristics and the taste characteristics are better than those of the other examples and the comparative examples, which further illustrates that the cigarette samples prepared in example 1 are combusted to release limonene uniformly, and the limonene is sucked along with the main stream smoke gradually, so that the functional characteristics of the limonene are well exerted, the quality of the cigarette products is stable, and the overall sensory quality of the cigarette samples is improved better.

Claims (1)

1. A method for reducing the limonene loss rate of bergamot oil essence after a high-temperature cut tobacco baking process is characterized in that the bergamot oil essence is prepared into liquid bergamot oil essence according to the following method, and the liquid bergamot oil essence is added into tobacco shreds of cigarettes in a proportion of 3% -5% of the mass of the tobacco shreds;
the preparation method for preparing the bergamot oil essence into the liquid bergamot oil essence comprises the following steps:
(1) Adding a certain amount of bergamot oil, an emulsifier and an auxiliary emulsifier into a glass container, stirring at a constant speed, and simultaneously adding deionized water;
(2) Centrifuging the mixed solution in step (1) at 3800-4500rmp for 30-50min until the mixed solution is transparent to obtain liquid bergamot oil essence;
in the step (1), the emulsifier is Tween 60, and the auxiliary emulsifier is absolute ethyl alcohol;
the Km value of the ratio of the mass of the emulsifier to the mass of the auxiliary emulsifier is 2:1;
in the step (1), the amount of bergamot oil is 13% -15% based on the whole mass ratio.
CN202111521181.9A 2021-12-13 2021-12-13 Method for improving limonene release balance in bergamot oil essence Active CN114214117B (en)

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