CN105738530A - Method for optioning aroma component in natural moss perfume spice - Google Patents

Method for optioning aroma component in natural moss perfume spice Download PDF

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CN105738530A
CN105738530A CN201610282172.1A CN201610282172A CN105738530A CN 105738530 A CN105738530 A CN 105738530A CN 201610282172 A CN201610282172 A CN 201610282172A CN 105738530 A CN105738530 A CN 105738530A
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spice
natural
delicate fragrance
fraction
aroma component
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CN105738530B (en
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朱怀远
庄亚东
曹毅
张媛
沈晓晨
尤晓娟
朱龙杰
韩开冬
何红梅
刘献军
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China Tobacco Jiangsu Industrial Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0001Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00 by organoleptic means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025Gas chromatography

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Abstract

The invention provides a method for optioning aroma components in natural moss perfume spice. The method comprises the following steps of: pre-separating components in a natural moss perfume raw material by using a wiped film molecular distillation instrument; qualitatively and quantitatively analyzing chemical components of different grades of fraction by using gas chromatography-mass spectrometry; respectively injecting the different grades of fraction into cigarette in an injection mode by using an essence and flavor injector; evaluating the sensory quality of the cigarette by using an aroma outline smoke panel test; by using a data processing method, optioning the aroma components contributing to typical perfume characteristics of the natural moss perfume spice according to respective variable contribution rates. By adopting the method for optioning the aroma components in the natural moss perfume spice, significant aroma components can be accurately optioned, simulation and compounding of natural spice can be improved, and active promotion functions on quality control and standardized production of natural spice can be also achieved.

Description

The selection method of aroma component in natural tongue delicate fragrance spice
Technical field
The present invention relates to a kind of selection method of aroma component in natural tongue delicate fragrance spice.
Background technology
To be grown under cool place, wet environment, grow nonparasitically upon another plant oak, pine, fir, fir trunk on, or Fructus Persicae, Fructus Pruni, Fructus Mali pumilae, Usneaceae Evernia bashfully and on Robinia pseudoacacia L. tree the product for preparing through certain processing technique as raw material of a kind of Lecanorales lichen, it is generally of the natural delicate fragrance of the liverwort material of uniqueness and strong resin breath, is important natural tongue delicate fragrance spice.Conventional goods generally have tree moss concrete, tree moss absolute, oakmoss concrete, oak moss absolute absolute oil etc..
Owing to lichens spice has the tongue delicate fragrance of uniqueness, lasting is relatively more of a specified duration, and can coordinate mutually with multiple spice, is constantly subjected to the concern of spice circle accordingly, with respect to the exploitation of lichens spice, application and chemical composition analysis.As a kind of natural perfume material, its composition is sufficiently complex, and, amino acids contained in thallus, fatty acid, depside, three mushroom acid, flavone, Herba Alii fistulosi wake up, the spell chemical substance of the various secondary metabolite of the type such as body and simple aromatic compound and multiple uniqueness has the biological activitys such as antiviral, antimicrobial, antitumor, antiallergic, plant growing suppression, anti-plant-eating animal and enzyme inhibition, therefore, how exactly its chemical constituent to be carried out qualitative and quantitative analysis and be also always up the study hotspot of organic chemist and medicine scholar.
Dong Sun Han seminar reports that the Asia tree belonging to three sections sends out, ditch tree sends out, the chemical composition of seven kinds of Yunnan product lichens such as tip snowflake clothing is sent out and rolled up to major diameter Usnea, beard Usnea, woods Herba Cladoniae rangiferinae, brick spore, and separation is obtained the compounds such as red star clothing acetoacetic ester, red star clothing acid, rhizonic acid carried out spectroscopic identification, the utilization for these plant resourceses provides scientific basis.The chemical composition of four kinds of lichens such as handle fruit Corii Bovis seu Bubali leaf, multiform tree, Kuan Banshen island clothing bleaching modification and top fruit coral branch has also been analyzed by this seminar, is divided into from identifying 18 kinds of compounds through thin layer chromatography and column chromatography.
Natural tongue delicate fragrance spice, especially extractum goods, generally all contain the compositions such as a large amount of pigment, plant be cured, cause that the pure degree of extractum is slightly worse, color depth matter is hard, there is bigger restriction when being applied to high-grade essence.And possibly together with some compositions causing people's allergy in spice, the compositions such as the A Lan phenol contained in the extractum such as tree moss, oak moss easily cause people's allergy and have been confirmed by some external scholars, in addition, possibly together with a considerable amount of heavy metal elements in a lot of extractum, also security-hidden trouble has been buried in the application for spice.The consumption that makes of tree moss goods, oak moss goods is had concrete limit standard by some mechanism, association, 1998, international essence association (IFRA) regulation tree moss concrete content in consumer goods must not exceed 0.1%, in European Union's cosmetics instruction (theEUCosmeticDirective) regulation cosmetics, the content of oak moss goods can not more than 0.1%, and the content corresponding to A Lan phenol and chloro A Lan phenol not can exceed that 21ppm and 9ppm.
Natural perfume material is carried out further deep processing, restructuring, the composite development trend having become fragrance industry after extracting important aroma component therein.But the research about the important aroma component constituting natural tongue delicate fragrance spice odor characteristic is still rare at present, and mostly some bibliographical informations are to quote external result of study at present, still there is no the research report of important aroma component selection method.Therefore need to seek the new method of a kind of objective, use easy to spread, effective, the important aroma component of selection natural perfume material, for tongue delicate fragrance essence composite, recombinate significant, also will play positive impetus to realizing the criteria for classification production of natural perfume material, quality control.
Summary of the invention
For the problems referred to above that prior art exists, it is an object of the invention to provide a kind of selection method of aroma component in natural tongue delicate fragrance spice, can selecting out the important aroma component of composition natural tongue delicate fragrance spice exemplary fragrance feature, the method is objective, effective, it is easy to promote the use of.
In order to solve above-mentioned technical problem, the present invention adopts following technical proposals:
In a kind of natural tongue delicate fragrance spice, the selection method of aroma component, comprises the steps:
Step 1, raw material fractionated, adopt wiped film molecular distillation instrument by natural tongue delicate fragrance raw material classification, be separated into three grades of fractions;
The fractions at different levels of step 1 are respectively adopted the wherein each chemical constituent of gas chromatography/mass spectrometry qualitative and quantitative analysis by step 2, fractional composition qualitative and quantitative;
Step 3, the fractions at different levels of step 1 adopt essence and flavoring agent injection instrument be injected separately in Medicated cigarette with injection system;
Step 4, the fragrance profile method each Medicated cigarette to step 3 of smokeing panel test is adopted to carry out sensory quality assessment;
Step 5, in step 2, the content of qualitative each composition out is independent variable, each index in step 4 is dependent variable, set up multivariate regression models, calculate the sum of squares of partial regression of regression sum of square and each independent variable, according to the contribution rate of this independent variable, assess the aroma component whether this composition is the odor characteristic constituting natural tongue delicate fragrance spice.
Further, in step 1, the fractionated of raw material is particularly as follows: the natural tongue delicate fragrance raw material that weighs, it is added thereto to ethanol, it is stirred vigorously and disperses, finely dispersed solution is poured in the feed liquid bottle of wiped film molecular distillation instrument, open cooling circulating water, the temperature of the first order and second level condensed water is set to 2 DEG C, the third level adopts liquid nitrogen condensation, feed rate is 1-4ml/min, the parameter of wiped film molecular distillation instrument is: vapo(u)rizing temperature 50 DEG C-90 DEG C, blade applicator rotating speed is 50-250r/min, absolute pressure is 0.1-2.0Pa, orthogonal test designs table is adopted to carry out several times test, collect first order fraction accordingly, second level fraction, third level fraction each several.
Further, natural tongue delicate fragrance spice described in step 1 is the one in tree moss goods, oak moss goods, the medium lichens extract of prunus mume (sieb.) sieb.et zucc. clothing goods or mixture.
Further, when described natural tongue delicate fragrance spice is extractum sample, it is necessary to adopt ethanol to carry out mass ratio 1:2~7 of dispersion process, raw material and ethanol.
Further, in step 2, fractional composition is qualitative particularly as follows: the analysis condition of gas chromatography/mass spectrometry is: adopting specification is 30m × 0.25mm × 0.25 μm high-resolution capillary column, temperature programming: 40 DEG C keep 2min, rise to 230 DEG C with 3 DEG C/min and keep 5min, then run 5min after 280 DEG C;Carrier gas He flow velocity 1.0mL/min, injector temperature is 250 DEG C, sample size 1 μ L, and split ratio is 10:1;Mass Spectrometry Conditions: adopt the ionization mode of electron impact ion source EI, ionizing energy is 70eV, ion source temperature is 230 DEG C, chromatograph and mass spectrographic transmission line temperature are 280 DEG C, quadrupole rod temperature 150 DEG C, the mass range adopting scan mode and scanning is 30~500amu, in conjunction with database retrieval, each chemical composition in fraction is qualitative.
Further, step 2 adopts internal standard method each composition is carried out quantitative analysis, in adopting, be designated as benzyl benzoate.
Further, in step 2, fractional composition quantitatively particularly as follows: the molecular distillation fraction at different levels accurately weighing 0.5g, adds and marks storing solution in the benzyl benzoate that 0.05~0.2ml concentration is 1.5~3mg/ml, more accurately adds the acetonitrile of 0.8ml, to be measured after shaking up;
Accurately weigh the β-orcin carboxylate methyl ester of 0.0025~2.5g, ethyl oleate, Ethyl linoleate, ethyl linolenate, ethyl palmitate standard substance, add acetonitrile to dissolve, it is settled to 50mL with acetonitrile, obtain the standard reserving solution of each material, then stepwise dilution becomes standard working solution, the interior mark contained in interior mark quality contained in standard working solution at different levels and fraction sample is identical in quality, is respectively adopted respective standard working curve and composition is carried out quantitative analysis.
Further, Medicated cigarette described in step 3 is the blank Medicated cigarette of non-flavoring and casing, and the addition of fractions at different levels is the 0.005%~5% of tobacco quality.
The invention has the beneficial effects as follows: the selection method of aroma component in this kind of natural tongue delicate fragrance spice, the important aroma component selected out is accurate, be beneficial to the imitative perfume (or spice) of natural perfume material, composite, also will play positive impetus for the quality control of natural perfume material, standardized production.The technological synthesiss such as molecular distillation, Medicated cigarette perfumery, data process are applied to the selection of natural perfume material aroma component by the method, first by the heavy component of natural perfume material and light components pre-separation, fractional composition is comparatively single, is beneficial to fraction objective evaluation of function in perfuming cigarette;Have chosen the aromatic style that can represent tongue delicate fragrance spice odor characteristic first, adopt many person-times of sensory evaluations, in conjunction with data processing technique, method is easy and simple to handle, processed by the test of substantial amounts of perfuming, sensory evaluation and data, specify that the selection method constituting natural perfume material exemplary fragrance feature important component first;Method use easy to spread, also can be used for the selection of other day spice active component.
Detailed description of the invention
The following detailed description of the preferred embodiments of the present invention.
The selection method of aroma component in the natural tongue delicate fragrance spice of embodiment, the important aroma component selected out is accurate, is beneficial to the imitative perfume (or spice) of natural perfume material, composite, also will play positive impetus for the quality control of natural perfume material, standardized production.
The selection method of aroma component in this kind of natural tongue delicate fragrance spice, adopts wiped film molecular distillation instrument that the component in natural tongue delicate fragrance raw material is carried out pre-separation;Adopt the chemical constituent of gas chromatography/mass spectrometry qualitative and quantitative analysis fraction at different levels;Fractions at different levels adopt essence and flavoring agent injection instrument to be injected separately in Medicated cigarette with injection system;Adopt fragrance profile smoke panel test method evaluate each Medicated cigarette aesthetic quality;Adopting data processing method, according to the contribution rate of each independent variable, selection constitutes the aroma component of natural tongue delicate fragrance spice exemplary fragrance feature.
Embodiment 1
In a kind of natural tongue delicate fragrance spice, the selection method of important aroma component, comprises the steps:
The fractionated of raw material: weigh the oakmoss concrete of 15g, it is added thereto to the ethanol of 75g, it is stirred vigorously and disperses, finely dispersed solution is poured in the feed liquid bottle of wiped film molecular distillation instrument, open cooling circulating water, the temperature of the first order and second level condensed water is set to 2 DEG C, the third level adopts liquid nitrogen condensation, feed rate is 2ml/min, all the other parameters of instrument are: vapo(u)rizing temperature 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, blade applicator rotating speed is 50r/min, 100r/min, 150r/min, 200r/min, 250r/min, absolute pressure is 0.1Pa, 0.5Pa, 1Pa, 1.5Pa, 2.0Pa, adopt L25(56) orthogonal test designs table carries out 25 tests, collects the first order, the second level, each 25 of third level fraction accordingly.
Fractional composition is qualitative: the analysis condition of gas chromatography/mass spectrometry is: HP-17MS (30m × 0.25mm × 0.25 μm) high-resolution capillary column, temperature programming: 40 DEG C keep 2min, rise to 230 DEG C with 3 DEG C/min and keep 5min, then run 5min after 280 DEG C;Carrier gas He flow velocity 1.0mL/min, injector temperature is 250 DEG C, sample size 1 μ L, and split ratio is 10:1;Mass Spectrometry Conditions: adopting the ionization mode of electron impact ion source EI, ionizing energy is 70eV, and ion source temperature is 230 DEG C, chromatograph and mass spectrographic transmission line temperature are 280 DEG C, quadrupole rod temperature 150 DEG C, adopts SCAN scan mode, and the mass range of scanning is 30~500amu.In conjunction with database retrieval (Nist08, Wily7.0), each chemical composition in fraction is qualitative.
Fractional composition is quantitative: accurately weigh the molecular distillation fraction at different levels of about 0.5g, adds and marks storing solution in the benzyl benzoate that 0.1ml concentration is 2.38mg/ml, more accurately adds the acetonitrile of 0.8ml, to be measured after shaking up.
Accurately weigh the β-orcin carboxylate methyl ester of 0.0025~2.5g, ethyl oleate, Ethyl linoleate, ethyl linolenate, ethyl palmitate standard substance, add acetonitrile to dissolve, it is settled to 50mL with acetonitrile, obtain the standard reserving solution of each material, then stepwise dilution becomes standard working solution, the interior mark contained in interior mark quality contained in standard working solution at different levels and fraction sample is identical in quality, is respectively adopted respective standard working curve and composition is carried out quantitative analysis.
By the first order fraction under each separation condition relative to the 0.005% of tobacco quality, to adopt flavoring and casing injector to be uniformly injected in cigarette, Medicated cigarette used is the unprinted leaf group not having flavoring and casing.
Organizing 15 judging panels with industry qualification to carry out fragrance profile to smoke panel test, the meansigma methods of 15 people is as the final assignment of this index.After this grade of fraction adds, compared with comparison Medicated cigarette, the oak moss fragrance of flue gas is comparatively obvious, has the oakmoss concrete partial action to flue gas, adds the tension force of flue gas, skeleton sense, dynamics.After showing employing molecular distillation pre-separation, the composition kind in fraction is comparatively concentrated, and good basis has been established in the selection for the important aroma component of oakmoss concrete.Table 1 gives vapo(u)rizing temperature 50 DEG C, and blade applicator rotating speed is 50r/min, the smoking result of first order fraction when absolute pressure is 0.1Pa.
The smoking result of table 1 fraction
With the content of each composition in all first order fractions for independent variable, each index in table 1 is dependent variable, setting up multivariate regression models, calculate the sum of squares of partial regression of regression sum of square and each independent variable, table 2 gives the fractions contribution rate result of calculation to each index in this grade of fraction.
Table 2 fractions contribution rate to index
Table 2 can be seen that, the compositions such as n-decane, 1,2,5-trimethylbenzene are not contributed for the odor characteristic of oakmoss concrete, for constituting the invalid component of oakmoss concrete odor characteristic, the odor characteristic of oakmoss concrete is had certain contribution by divaricatic acid ethyl ester and difference Evernia element monomethyl ether.According to each composition contribution rate to fragrance index, comprehensive all analysis results, in final confirmation first order fraction, orcin monomethyl ether, difference Evernia element monomethyl ether, everninic acid ethyl ester, rhizonic acid ethyl ester, β-orcin carboxylate methyl ester, red star clothing acetoacetic ester, orcin carboxylic acid, ethyl ester, divaricatic acid ethyl ester, 2-hydroxyl-4-methoxyl group-6-n-amylbenzene Ethyl formate are the important aroma components constituting oakmoss concrete natural tongue delicate fragrance spice exemplary fragrance feature.
Embodiment 2
The condition of embodiment 2 is substantially the same manner as Example 1 with step, and embodiment 2 and embodiment 1 are distinctive in that, oakmoss concrete raw material is replaced by tree moss absolute.Tree moss absolute directly adopts molecular distillation instrument to carry out classification, separation.
By the third level fraction under each separation condition relative to the 1% of tobacco quality, to adopt flavoring and casing injector to be uniformly injected in cigarette, Medicated cigarette used is the unprinted leaf group not having flavoring and casing.
Organize 20 judging panels with industry qualification to carry out fragrance profile to smoke panel test.After this grade of fraction adds, compared with comparison Medicated cigarette, flue gas concentration promotes to some extent, with the fragrance harmony of Medicated cigarette, mouthfeel zero defect.Flue gas leading portion, fresh and sweet fragrant sense has lifting, and flue gas becomes exquisite, compacts, has the fresh and sweet of tree moss.
With the content of each composition in all third level fractions for independent variable, each index in table 1 is dependent variable, setting up multivariate regression models, calculate the sum of squares of partial regression of regression sum of square and each independent variable, table 3 gives the fractions contribution rate result of calculation to each index in this grade of fraction.
Table 3 fractions contribution rate to index
According to each composition contribution rate to fragrance index, 1,2, the hydrocarbon component such as 3-trimethylbenzene are not contributed for the odor characteristic of tree moss absolute, for constituting the invalid component of oakmoss concrete odor characteristic, comprehensive all analysis results, in final confirmation third level fraction, ethyl hexanoate, 10-Pinen-3-ol, alpha-terpineol, carvone, phellandral, alloaromadendrene, cuparene, aromadendrene, ledene, bisabolene, δ-cadinene are the important aroma components of the exemplary fragrance feature constituting tree moss absolute natural tongue delicate fragrance spice.
Embodiment 3
The condition of embodiment 2 is substantially the same manner as Example 1 with step, and embodiment 2 and embodiment 1 are distinctive in that, oakmoss concrete raw material is replaced by tree moss concrete.Molecular distillation instrument parameter is: vapo(u)rizing temperature 60 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, 1200 DEG C, blade applicator rotating speed is 100r/min, 150r/min, 200r/min, 250r/min, 300r/min, absolute pressure is 5Pa, 10Pa, 20Pa, 30Pa, 50Pa, adopts L25(56) orthogonal test designs table carries out 25 tests.
By the second level fraction under each separation condition relative to the 0.5% of tobacco quality, to adopt flavoring and casing injector to be uniformly injected in cigarette, Medicated cigarette used is the unprinted leaf group not having flavoring and casing.
Organize 20 judging panels with industry qualification to carry out fragrance profile to smoke panel test.After this grade of fraction adds, compared with comparison Medicated cigarette, the soft exquisiteness of flue gas, flue gas concentration is promoted substantially, pleasant impression is comfortable.The fragrance of tree moss is carried throughout, has skeleton sense, and dispersion ratio is more uniform, and flue gas is fine and smooth, abundant, and the dry sensation of control sample is stronger.
With the content of each composition in the fraction of all second level for independent variable, each index in table 1 is dependent variable, setting up multivariate regression models, calculate the sum of squares of partial regression of regression sum of square and each independent variable, table 4 gives the fractions contribution rate result of calculation to each index in this grade of fraction.
Table 4 fractions contribution rate to index
Table 4 can be seen that, the compositions such as n-decane, 1,2,5-trimethylbenzene are not contributed for the odor characteristic of tree moss concrete, for constituting the invalid component of tree moss concrete odor characteristic, the odor characteristic of tree moss concrete is had certain contribution by rhizonic acid ethyl ester, everninic acid ethyl ester, red star clothing acetoacetic ester.According to each composition contribution rate to fragrance index, comprehensive all analysis results, in the fraction of the final confirmation second level, orcin monomethyl ether, difference Evernia element monomethyl ether, everninic acid ethyl ester, rhizonic acid ethyl ester, β-orcin carboxylate methyl ester, red star clothing acetoacetic ester, orcin carboxylic acid, ethyl ester, divaricatic acid ethyl ester, 2-hydroxyl-4-methoxyl group-6-n-amylbenzene Ethyl formate are the important aroma components constituting oakmoss concrete natural tongue delicate fragrance spice exemplary fragrance feature.
The above embodiment of the present invention is only for clearly demonstrating example of the present invention, not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot all of embodiment be given exhaustive.Every belong to apparent change that technical scheme extended out or the variation row still in protection scope of the present invention.

Claims (8)

1. the selection method of aroma component in a natural tongue delicate fragrance spice, it is characterised in that comprise the steps:
Step 1, raw material fractionated, adopt wiped film molecular distillation instrument by natural tongue delicate fragrance raw material classification, be separated into three grades of fractions;
The fractions at different levels of step 1 are respectively adopted the wherein each chemical constituent of gas chromatography/mass spectrometry qualitative and quantitative analysis by step 2, fractional composition qualitative and quantitative;
Step 3, the fractions at different levels of step 1 adopt essence and flavoring agent injection instrument be injected separately in Medicated cigarette with injection system;
Step 4, the fragrance profile method each Medicated cigarette to step 3 of smokeing panel test is adopted to carry out sensory quality assessment;
Step 5, in step 2, the content of qualitative each composition out is independent variable, each index in step 4 is dependent variable, set up multivariate regression models, calculate the sum of squares of partial regression of regression sum of square and each independent variable, according to the contribution rate of this independent variable, assess the aroma component whether this composition is the odor characteristic constituting natural tongue delicate fragrance spice.
null2. the selection method of aroma component in natural tongue delicate fragrance spice as claimed in claim 1,It is characterized in that,In step 1,The fractionated of raw material is particularly as follows: the natural tongue delicate fragrance raw material that weighs,It is added thereto to ethanol,It is stirred vigorously and disperses,Finely dispersed solution is poured in the feed liquid bottle of wiped film molecular distillation instrument,Open cooling circulating water,The temperature of the first order and second level condensed water is set to 2 DEG C,The third level adopts liquid nitrogen condensation,Feed rate is 1-4ml/min,The parameter of wiped film molecular distillation instrument is: vapo(u)rizing temperature 50 DEG C-90 DEG C,Blade applicator rotating speed is 50-250r/min,Absolute pressure is 0.1-2.0Pa,Orthogonal test designs table is adopted to carry out several times test,Collect first order fraction accordingly、Second level fraction、Third level fraction each several.
3. the selection method of aroma component in natural tongue delicate fragrance spice as claimed in claim 1, it is characterised in that: natural tongue delicate fragrance spice described in step 1 is the one in the lichens extracts such as tree moss goods, oak moss goods, prunus mume (sieb.) sieb.et zucc. clothing goods or mixture.
4. the selection method of aroma component in natural tongue delicate fragrance spice as claimed in claim 1, it is characterised in that: when described natural tongue delicate fragrance spice is extractum sample, it is necessary to adopt ethanol to carry out mass ratio 1:2~7 of dispersion process, raw material and ethanol.
5. the selection method of aroma component in natural tongue delicate fragrance spice as described in any one of claim 1-4, it is characterized in that, in step 2, fractional composition is qualitative particularly as follows: the analysis condition of gas chromatography/mass spectrometry is: adopting specification is 30m × 0.25mm × 0.25 μm high-resolution capillary column, temperature programming: 40 DEG C keep 2min, rise to 230 DEG C with 3 DEG C/min and keep 5min, then run 5min after 280 DEG C;Carrier gas He flow velocity 1.0mL/min, injector temperature is 250 DEG C, sample size 1 μ L, and split ratio is 10:1;Mass Spectrometry Conditions: adopt the ionization mode of electron impact ion source EI, ionizing energy is 70eV, ion source temperature is 230 DEG C, chromatograph and mass spectrographic transmission line temperature are 280 DEG C, quadrupole rod temperature 150 DEG C, the mass range adopting scan mode and scanning is 30~500amu, in conjunction with database retrieval, each chemical composition in fraction is qualitative.
6. the selection method of aroma component in natural tongue delicate fragrance spice as described in any one of claim 1-4, it is characterised in that: step 2 adopts internal standard method each composition is carried out quantitative analysis, in adopting, be designated as benzyl benzoate.
7. the selection method of aroma component in natural tongue delicate fragrance spice as described in any one of claim 1-4, it is characterized in that, in step 2, fractional composition is quantitatively particularly as follows: the molecular distillation fraction at different levels accurately weighing 0.5g, add mark storing solution in the benzyl benzoate that 0.05~0.2ml concentration is 1.5~3mg/ml, accurately add the acetonitrile of 0.8ml again, to be measured after shaking up;
Accurately weigh the β-orcin carboxylate methyl ester of 0.0025~2.5g, ethyl oleate, Ethyl linoleate, ethyl linolenate, ethyl palmitate standard substance, add acetonitrile to dissolve, it is settled to 50mL with acetonitrile, obtain the standard reserving solution of each material, then stepwise dilution becomes standard working solution, the interior mark contained in interior mark quality contained in standard working solution at different levels and fraction sample is identical in quality, is respectively adopted respective standard working curve and composition is carried out quantitative analysis.
8. the selection method of aroma component in natural tongue delicate fragrance spice as described in any one of claim 1-4, it is characterised in that: Medicated cigarette described in step 3 is the blank Medicated cigarette of non-flavoring and casing, and the addition of fractions at different levels is the 0.005%~5% of tobacco quality.
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Cited By (7)

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CN106290641A (en) * 2016-08-11 2017-01-04 云南中烟工业有限责任公司 A kind of quantitative forecasting technique of Medicated cigarette delicate fragrance type
CN106706794A (en) * 2017-01-04 2017-05-24 江苏中烟工业有限责任公司 Quantitative analysis method of main moss fragrance characteristics flavor component in fine cigarette mainstream smoke
CN106908550A (en) * 2017-04-06 2017-06-30 福建中烟工业有限责任公司 A kind of method of Usneaceae plant characteristics composition in detection tobacco sample
CN109932436A (en) * 2017-12-19 2019-06-25 湖南中烟工业有限责任公司 Fragrant method is distinguished in a kind of digitlization based on characterising mass spectrometry map
CN110554120A (en) * 2019-10-17 2019-12-10 云南中烟工业有限责任公司 Detection method of tree moss aroma phenolic substances
CN110554119A (en) * 2019-10-17 2019-12-10 云南中烟工业有限责任公司 Quantitative detection method for tree moss aroma phenolic substances
CN110568107A (en) * 2019-10-17 2019-12-13 云南中烟工业有限责任公司 Detection method of moss phenolic substances in moss plants or extracts

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