CN105738530B - The selection method of aroma component in natural tongue delicate fragrance spices - Google Patents
The selection method of aroma component in natural tongue delicate fragrance spices Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0001—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00 by organoleptic means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The present invention provides a kind of selection method of aroma component in natural tongue delicate fragrance spices, and the component in natural tongue delicate fragrance raw material is carried out into pre-separation using wiped film molecular distillation instrument；Using the chemical constituent of gas chromatography/mass spectrometry qualitative and quantitative analysis cuts at different levels；Cuts at different levels use essence and flavoring agent injection instrument to be injected separately into injection system in cigarette；The aesthetic quality of each cigarette is evaluated using fragrance profile method of smokeing panel test；Using data processing method, according to the contribution rate of each independent variable, selection forms the aroma component of natural tongue delicate fragrance spices exemplary fragrance feature.The selection method of aroma component in this kind of natural tongue delicate fragrance spices, the important aroma component selected out is accurate, and beneficial to the imitative fragrant, compounding of natural perfume material, quality control, standardized production for natural perfume material will also play positive impetus.
Description
Technical field
The present invention relates to a kind of selection method of aroma component in natural tongue delicate fragrance spices.
Background technology
To be grown under shady and cool, wet environment, grow nonparasitically upon another plant oak, pine, fir, fir trunk on, or peach, apricot, apple,
A kind of Lecanorales lichen of Usneaceae Evernia bashfully and on locust tree tree is as raw material through certain processing technology system
The product obtained, generally there is the natural delicate fragrance of unique liverwort material and strong resin breath, be important natural tongue delicate fragrance
Spices.Conventional product typically has tree moss concrete, tree moss absolute, oakmoss concrete, oak moss absolute absolute oil etc..
Because lichens spices has unique tongue delicate fragrance, lasting is more long, and can mutually coordinate with a variety of spices, therefore, closes
The concern of spices circle is constantly subjected in the exploitation, application and chemical composition analysis of lichens spices.As a kind of natural perfume material, its group
Into sufficiently complex, moreover, amino acids contained in thallus, aliphatic acid, depside, three mushroom acid, flavones, green onion are waken up, spelling body with
And the various secondary metabolite of type such as simple aromatic compound and a variety of unique chemical substances have it is antiviral,
The bioactivity such as antimicrobial, antitumor, antiallergy, plant growth suppression, anti-plant-eating animal and enzyme inhibition, therefore, such as
What carries out the study hotspot that qualitative and quantitative analysis is also always organic chemist and medicine scholar to its chemical constituent exactly.
Dong Sun Han seminar reports the Asia tree hair for belonging to three sections, ditch tree hair, major diameter sunglo, beard sunglo, woods
The chemical composition of seven kinds of Yunnan production lichens such as reindeer moss, brick spore hair and volume tip snowflake clothing, and to isolated red star clothing acid
The compounds such as ethyl ester, red star clothing acid, rhizonic acid have carried out Spectral Identification, for these plant resourceses utilization provide science according to
According to.The seminar also bleaches four kinds of lichens such as modification and top fruit coral branch to handle fruit ox-hide leaf, multiform tree hair, Kuan Banshen islands clothing and planted
The chemical composition of thing is analyzed, and 18 kinds of compounds are isolated and identified through thin-layer chromatography and column chromatography.
Natural tongue delicate fragrance spices, especially medicinal extract product, typically all cause to soak containing the composition such as a large amount of pigments, plant be cured
The pure degree of cream is slightly worse, and color depth matter is hard, larger limitation be present during applied to high-grade essence.And also containing causing people's mistake in spices
The compositions such as the A Lan phenol contained in some quick compositions, such as tree moss, oak moss medicinal extract easily cause people's allergy by some external
Scholar is confirmed, in addition, also containing a considerable amount of heavy metal elements in many medicinal extract, has also buried quality for the application of spices
Potential safety hazard.Some mechanisms, association have specific limit standard to the usage amount of tree moss product, oak moss product, 1998, state
Content of border essence association (IFRA) the regulation tree moss concrete in the consumer goods must not exceed 0.1%, European Union cosmetics instruction (the
EU Cosmetic Directive) provide that the content of oak moss product in cosmetics can not be more than 0.1%, corresponding to A Lan phenol
Content with chloro A Lan phenol is no more than 21ppm and 9ppm.
Further deep processing is carried out to natural perfume material, restructuring, compounding are as perfume after extracting important aroma component therein
Expect a development trend of industry.But ground at present on forming the important aroma component of natural tongue delicate fragrance spices odor characteristic
It is still rare to study carefully, and some document reports are to quote external result of study mostly at present, still without important aroma component selection method
Research report.Therefore a kind of objective, easy to spread new method used need to be sought, selects the effective, important of natural perfume material
Aroma component, compounding for tongue delicate fragrance essence, recombinate significant, the criteria for classification metaplasia to realizing natural perfume material
Quality control will also play positive impetus.
The content of the invention
In view of the above-mentioned problems existing in the prior art, it is an object of the invention to provide caused in a kind of natural tongue delicate fragrance spices
The selection method of fragrant composition, the important aroma component of the natural tongue delicate fragrance spices exemplary fragrance feature of composition, the party can be selected out
Method is objective, effective, use easy to spread.
In order to solve the above-mentioned technical problem, the present invention uses following technical proposals：
The selection method of aroma component, comprises the following steps in a kind of natural tongue delicate fragrance spices：
Natural tongue delicate fragrance raw material, is classified, separated by the classification separation of step 1, raw material using wiped film molecular distillation instrument
For three-level cut；
Step 2, fractional composition qualitative and quantitative, gas chromatography/mass spectrometry is respectively adopted in the cuts at different levels of step 1 and is determined
Property, the wherein each chemical constituent of quantitative analysis；
Step 3, essence and flavoring agent injection instrument is used to be injected separately into injection system in cigarette the cuts at different levels of step 1；
Step 4, each cigarette progress sensory quality assessment of the method to step 3 of being smoked panel test using fragrance profile；
Step 5, using the content of qualitative each composition out in step 2 as independent variable, each index in step 4 is because becoming
Amount, multivariate regression models is established, calculate the sum of squares of partial regression of regression sum of square and each independent variable, the tribute according to the independent variable
Offer rate, assess the composition whether be the odor characteristic for forming natural tongue delicate fragrance spices aroma component.
Further, in step 1, the classification separation of raw material is specially：The natural tongue delicate fragrance raw material weighed, is added thereto
Ethanol, it is stirred vigorously and is disperseed, finely dispersed solution is poured into the feed liquid bottle of wiped film molecular distillation instrument, is opened cold
But recirculated water, the temperature of the first order and second level condensed water is set to 2 DEG C, the third level uses liquid nitrogen condensation, feed rate 1-
4ml/min, the parameter of wiped film molecular distillation instrument are：50 DEG C -90 DEG C of vapo(u)rizing temperature, blade applicator rotating speed are 50-250r/min,
Absolute pressure is 0.1-2.0Pa, is carried out using orthogonal test designs table and tested several times, is accordingly collected into first order cut, the
Two level cut, third level cut it is each several.
Further, natural tongue delicate fragrance spices described in step 1 be tree moss product, oak moss product, plum clothing product mediumly
One kind or mixture in clothing extract.
Further, it is necessary to carry out decentralized processing, raw material using ethanol when the natural tongue delicate fragrance spices is medicinal extract sample
With the mass ratio 1 of ethanol:2~7.
Further, in step 2, fractional composition is qualitative to be specially：The analysis condition of gas chromatography/mass spectrometry is：Adopt
It is 30m × 0.25mm × 0.25 μm high-resolution capillary column with specification, temperature programming：40 DEG C of holding 2min, with 3 DEG C/min liters
To 230 DEG C of holding 5min, then to run 5min after 280 DEG C；Carrier gas He flow velocity 1.0mL/min, injector temperature are 250 DEG C, are entered
The μ L of sample amount 1, split ratio 10:1；Mass Spectrometry Conditions：Using electron impact ion source EI ionization mode, ionization energy is
70eV, ion source temperature are 230 DEG C, and chromatogram and mass spectrographic transmission line temperature are 280 DEG C, 150 DEG C of quadrupole rod temperature, using scanning
Mode and scanning mass range be 30~500amu, it is qualitative to each chemical composition in cut with reference to database retrieval.
Further, in step 2 using internal standard method to each composition carry out quantitative analysis, it is used in be designated as phenylamino benzoic acid
Methyl esters.
Further, in step 2, fractional composition is specially quantitatively：The accurate molecular distillation cuts at different levels for weighing 0.5g, add
Enter the benzyl benzoate internal standard storing solution that 0.05~0.2ml concentration is 1.5~3mg/ml, then the accurate acetonitrile for adding 0.8ml,
Shake up rear to be measured；
Accurate β-orcin the carboxylate methyl ester for weighing 0.0025~2.5g, ethyl oleate, ethyl linoleate, leukotrienes second
Ester, ethyl palmitate standard items, acetonitrile dissolving is added, 50mL is settled to acetonitrile, obtains the standard reserving solution of each material, then
It is diluted to standard working solution step by step, contained internal standard quality and the internal standard contained in fraction sample in standard working solutions at different levels
It is identical in quality, respective standard working curve is respectively adopted quantitative analysis is carried out to composition.
Further, cigarette described in step 3 is the blank cigarette of non-flavoring and casing, and the addition of cuts at different levels is pipe tobacco
The 0.005%~5% of quality.
The beneficial effects of the invention are as follows：The selection method of aroma component, the weight selected out in this kind of natural tongue delicate fragrance spices
Want aroma component accurate, beneficial to the imitative fragrant, compounding of natural perfume material, quality control, standardized production for natural perfume material also will
Play positive impetus.The technological synthesis such as molecular distillation, cigarette blending, data processing are applied to natural perfume material by this method
The selection of aroma component, first by the heavy component of natural perfume material and light components pre-separation, fractional composition is more single, beneficial to evaporating
Divide the objective evaluation of the function in perfuming cigarette；Have chosen first can represent the aromatic style of tongue delicate fragrance spices odor characteristic,
Using more person-times of sensory evaluations, with reference to data processing technique, method is easy to operate, is tested by substantial amounts of perfuming, sensory evaluation
And data processing, the selection method for forming natural perfume material exemplary fragrance feature important component is specify that first；Method is easy to spread
Use, the also selection available for other day spices active principle.
Embodiment
The following detailed description of the preferred embodiments of the present invention.
The selection method of aroma component in the natural tongue delicate fragrance spices of embodiment, the important aroma component selected out is accurate,
Beneficial to the imitative fragrant, compounding of natural perfume material, quality control, standardized production for natural perfume material will also be played positive promotion and made
With.
The selection method of aroma component in this kind of natural tongue delicate fragrance spices, using wiped film molecular distillation instrument by natural tongue
Component in delicate fragrance raw material carries out pre-separation；Using the chemical group of gas chromatography/mass spectrometry qualitative and quantitative analysis cuts at different levels
Point；Cuts at different levels use essence and flavoring agent injection instrument to be injected separately into injection system in cigarette；Using fragrance profile smoke panel test method evaluation
The aesthetic quality of each cigarette；Using data processing method, according to the contribution rate of each independent variable, selection forms natural tongue delicate fragrance spices
The aroma component of exemplary fragrance feature.
Embodiment 1
The selection method of important aroma component, comprises the following steps in a kind of natural tongue delicate fragrance spices：
The classification separation of raw material：15g oakmoss concrete is weighed, 75g ethanol is added thereto, is stirred vigorously point
Dissipate, finely dispersed solution poured into the feed liquid bottle of wiped film molecular distillation instrument, open cooling circulating water, by the first order and
The temperature of second level condensed water is set to 2 DEG C, and the third level uses liquid nitrogen condensation, feed rate 2ml/min, remaining parameter of instrument
For：50 DEG C of vapo(u)rizing temperature, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, blade applicator rotating speed be 50r/min, 100r/min, 150r/min,
200r/min, 250r/min, absolute pressure 0.1Pa, 0.5Pa, 1Pa, 1.5Pa, 2.0Pa, using L25(56) orthogonal experiment plan
Count table and carry out 25 experiments, be accordingly collected into the first order, the second level, each 25 of third level cut.
Fractional composition is qualitative：The analysis condition of gas chromatography/mass spectrometry is：HP-17MS(30m×0.25mm×0.25μ
M) high-resolution capillary column, temperature programming：40 DEG C of holding 2min, 230 DEG C of holding 5min are risen to 3 DEG C/min, then with 280 DEG C
After run 5min；Carrier gas He flow velocity 1.0mL/min, injector temperature are 250 DEG C, the μ L of sample size 1, split ratio 10:1；Mass spectrum
Condition：Using electron impact ion source EI ionization mode, ionization energy is 70eV, and ion source temperature is 230 DEG C, chromatogram and
Mass spectrographic transmission line temperature is 280 DEG C, 150 DEG C of quadrupole rod temperature, using SCAN scan modes, the mass range of scanning is 30~
500amu.It is qualitative to each chemical composition in cut with reference to database retrieval (Nist08, Wily7.0).
Fractional composition quantifies：The accurate molecular distillation cuts at different levels for weighing 0.5g or so, adding 0.1ml concentration is
2.38mg/ml benzyl benzoate internal standard storing solution, then the accurate acetonitrile for adding 0.8ml, shake up rear to be measured.
Accurate β-orcin the carboxylate methyl ester for weighing 0.0025~2.5g, ethyl oleate, ethyl linoleate, leukotrienes second
Ester, ethyl palmitate standard items, acetonitrile dissolving is added, 50mL is settled to acetonitrile, obtains the standard reserving solution of each material, then
It is diluted to standard working solution step by step, contained internal standard quality and the internal standard contained in fraction sample in standard working solutions at different levels
It is identical in quality, respective standard working curve is respectively adopted quantitative analysis is carried out to composition.
By the first order cut under each separation condition relative to the 0.005% of tobacco quality, to be injected using flavoring and casing
Machine is uniformly injected into cigarette, and cigarette used is the unprinted leaf group of no flavoring and casing.
Judging panel's progress fragrance profile that 15, tissue has industry qualification is smoked panel test, and the average value of 15 people is as this index
Final assignment.After this grade of cut adds, compared with compareing cigarette, the oak moss fragrance of flue gas is more obvious, has oakmoss concrete pair
The partial action of flue gas, add the tension force of flue gas, skeleton sense, dynamics.Show after using molecular distillation pre-separation, in cut
Composition species is more concentrated, and good basis has been established for the selection of the important aroma component of oakmoss concrete.Table 1 is given in distillation temperature
50 DEG C of degree, blade applicator rotating speed is 50r/min, the smoking result of first order cut when absolute pressure is 0.1Pa.
The smoking result of the cut of table 1
Using the content of each composition in all first order cuts as independent variable, each index in table 1 is dependent variable, is established more
First regression model, the sum of squares of partial regression of regression sum of square and each independent variable is calculated, table 2 gives to be divided into the middle part of this grade of cut
Divide the contribution rate result of calculation to each index.
Contribution rate of the fractions of table 2 to index
As can be seen that the composition such as n-decane, 1,2,5- trimethylbenzenes does not have tribute for the odor characteristic of oakmoss concrete in table 2
Offer, to form the invalid component of oakmoss concrete odor characteristic, divaricatic acid ethyl ester and difference Evernia element monomethyl ether are to oak moss
The odor characteristic of medicinal extract has certain contribution.Contribution rate according to each composition to fragrance index, comprehensive all analysis results are final true
Recognize in first order cut, orcin monomethyl ether, difference Evernia element monomethyl ether, everninic acid ethyl ester, rhizonic acid ethyl ester, β-Tai Hei
Phenol carboxylate methyl ester, red star clothing acetoacetic ester, orcin carboxylic acid, ethyl ester, divaricatic acid ethyl ester, 2- hydroxyl -4- methoxyl groups -6- positive penta
Yl benzoic acid ethyl ester is the important aroma component for forming the natural tongue delicate fragrance spices exemplary fragrance feature of oakmoss concrete.
Embodiment 2
The condition of embodiment 2 and step are substantially the same manner as Example 1, and the difference of embodiment 2 and embodiment 1 is, by rubber
Tongue medicinal extract raw material is replaced by tree moss absolute.Tree moss absolute is directly classified, separated using molecular distillation instrument.
, will using flavoring and casing injector by the third level cut under each separation condition with relative to the 1% of tobacco quality
It is uniformly injected into cigarette, and cigarette used is the unprinted leaf group of no flavoring and casing.
Judging panel's progress fragrance profile that 20, tissue has industry qualification is smoked panel test.After this grade of cut adds, with compareing cigarette
Compare, flue gas concentration has been lifted, the fragrance harmony with cigarette, mouthfeel zero defect.Flue gas leading portion, fresh and sweet fragrant sense have lifting, cigarette
Gas becomes the exquisite, sweetness for the tree moss that compacts, has.
Using the content of each composition in all third level cuts as independent variable, each index in table 1 is dependent variable, is established more
First regression model, the sum of squares of partial regression of regression sum of square and each independent variable is calculated, table 3 gives to be divided into the middle part of this grade of cut
Divide the contribution rate result of calculation to each index.
Contribution rate of the fractions of table 3 to index
The perfume (or spice) of the hydrocarbon component such as contribution rate, 1,2,3- trimethylbenzene according to each composition to fragrance index for tree moss absolute
Gas feature is not contributed, and to form the invalid component of oakmoss concrete odor characteristic, comprehensive all analysis results are final to confirm the 3rd
In level cut, ethyl hexanoate, pinocarveol, alpha-terpineol, carvol, phellandral, alloaromadendrene, cuparene, aromadendrene, loudspeaker
Alkene, bisabolene, δ-cadinene are that the important cause for the exemplary fragrance feature for forming the natural tongue delicate fragrance spices of tree moss absolute is fragrant
Composition.
Embodiment 3
The condition of embodiment 2 and step are substantially the same manner as Example 1, and the difference of embodiment 2 and embodiment 1 is, by rubber
Tongue medicinal extract raw material is replaced by tree moss concrete.Molecular distillation instrument parameter is：60 DEG C of vapo(u)rizing temperature, 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 5Pa,
10Pa, 20Pa, 30Pa, 50Pa, using L25(56) 25 experiments of orthogonal test designs table development.
By the second level cut under each separation condition with relative to the 0.5% of tobacco quality, using flavoring and casing injector
It is uniformly injected into cigarette, cigarette used is the unprinted leaf group of no flavoring and casing.
Judging panel's progress fragrance profile that 20, tissue has industry qualification is smoked panel test.After this grade of cut adds, with compareing cigarette
Compare, the soft exquisiteness of flue gas, flue gas concentration is lifted substantially, pleasant impression is comfortable.The fragrance of tree moss is carried throughout, there is skeleton sense, point
Dissipate than more uniform, flue gas is fine and smooth, abundant, and the dry sensation of control sample is stronger.
Using the content of each composition in all second level cuts as independent variable, each index in table 1 is dependent variable, is established more
First regression model, the sum of squares of partial regression of regression sum of square and each independent variable is calculated, table 4 gives to be divided into the middle part of this grade of cut
Divide the contribution rate result of calculation to each index.
Contribution rate of the fractions of table 4 to index
As can be seen that the composition such as n-decane, 1,2,5- trimethylbenzenes does not have tribute for the odor characteristic of tree moss concrete in table 4
Offer, to form the invalid component of tree moss concrete odor characteristic, rhizonic acid ethyl ester, everninic acid ethyl ester, red star clothing acetoacetic ester are to tree
The odor characteristic of tongue medicinal extract has certain contribution.Contribution rate according to each composition to fragrance index, comprehensive all analysis results, finally
Confirm in the cut of the second level, orcin monomethyl ether, difference Evernia element monomethyl ether, everninic acid ethyl ester, rhizonic acid ethyl ester, β-tongue
Black phenol carboxylate methyl ester, red star clothing acetoacetic ester, orcin carboxylic acid, ethyl ester, divaricatic acid ethyl ester, 2- hydroxyl -4- methoxyl groups -6- are just
Amyl group ethyl benzoate is the important aroma component for forming the natural tongue delicate fragrance spices exemplary fragrance feature of oakmoss concrete.
The above embodiment of the present invention is only intended to clearly illustrate example of the present invention, not to the reality of the present invention
Apply the restriction of mode.For those of ordinary skill in the field, can also make on the basis of the above description other
Various forms of changes or variation.Here all embodiments can not be exhaustive.Every technical side for belonging to the present invention
Row of the obvious changes or variations that case is extended out still in protection scope of the present invention.
Claims (5)
1. a kind of selection method of aroma component in natural tongue delicate fragrance spices, it is characterised in that comprise the following steps：
Natural tongue delicate fragrance raw material, is classified, is separated into three by the classification separation of step 1, raw material using wiped film molecular distillation instrument
Level cut；
Step 2, fractional composition qualitative and quantitative, by the cuts at different levels of step 1 be respectively adopted gas chromatography/mass spectrometry it is qualitative,
The wherein each chemical constituent of quantitative analysis；In step 2 using internal standard method to each composition carry out quantitative analysis, it is used in be designated as
Benzyl benzoate, fractional composition are specially quantitatively：The accurate molecular distillation cuts at different levels for weighing 0.5 g, addition 0.05~
0.2ml concentration is 1.5~3mg/ml benzyl benzoate internal standard storing solution, then accurately adds 0.8 ml acetonitrile, after shaking up
It is to be measured；
Accurate β-orcin the carboxylate methyl ester for weighing 0.0025~2.5g, ethyl oleate, ethyl linoleate, ethyl linolenate, palm fibre
Ethyl gallate standard items, acetonitrile dissolving is added, 50 mL are settled to acetonitrile, obtain the standard reserving solution of each material, then step by step
It is diluted to standard working solution, contained internal standard quality and the internal standard quality contained in fraction sample in standard working solutions at different levels
It is identical, respective standard working curve is respectively adopted quantitative analysis is carried out to composition；
Step 3, essence and flavoring agent injection instrument is used to be injected separately into injection system in cigarette the cuts at different levels of step 1；In step 3
The cigarette is the blank cigarette of non-flavoring and casing, and the addition of cuts at different levels is the 0.005%~5% of tobacco quality；
Step 4, each cigarette progress sensory quality assessment of the method to step 3 of being smoked panel test using fragrance profile；
Step 5, using in step 2 it is qualitative out each composition content as independent variable, each index in step 4 is dependent variable, is built
Vertical multivariate regression models, the sum of squares of partial regression of regression sum of square and each independent variable is calculated, according to the contribution rate of the independent variable,
Assess the composition whether be the odor characteristic for forming natural tongue delicate fragrance spices aroma component.
2. the selection method of aroma component in natural tongue delicate fragrance spices as claimed in claim 1, it is characterised in that former in step 1
The classification of material separates：The natural tongue delicate fragrance raw material weighed, adds ethanol, is stirred vigorously and is disperseed thereto, will divide
Dissipate uniform solution to pour into the feed liquid bottle of wiped film molecular distillation instrument, cooling circulating water is opened, by the first order and the second level
The temperature of condensed water is set to 2 DEG C, and the third level uses liquid nitrogen condensation, feed rate 1-4ml/min, wiped film molecular distillation instrument
Parameter be：50 DEG C -90 DEG C of vapo(u)rizing temperature, blade applicator rotating speed are 50-250 r/min, absolute pressure 0.1-2.0Pa, are used
Orthogonal test designs table is carried out to be tested several times, and it is each some to be accordingly collected into first order cut, second level cut, third level cut
It is individual.
3. the selection method of aroma component in natural tongue delicate fragrance spices as claimed in claim 1, it is characterised in that：Institute in step 1
Natural tongue delicate fragrance spices is stated as one kind or mixture in lichens extract.
4. the selection method of aroma component in natural tongue delicate fragrance spices as claimed in claim 1, it is characterised in that：The natural tongue
, it is necessary to carry out the mass ratio 1 of decentralized processing, raw material and ethanol using ethanol when delicate fragrance spices is medicinal extract sample:2~7.
5. the selection method of aroma component in the natural tongue delicate fragrance spices as described in claim any one of 1-4, it is characterised in that step
In rapid 2, fractional composition is qualitative to be specially：The analysis condition of gas chromatography/mass spectrometry is：Specification is used as 30m × 0.25mm
× 0.25 μm of high-resolution capillary column, temperature programming：40 DEG C of 2 min of holding, 230 DEG C of holding 5min are risen to 3 DEG C/min,
Again to run 5 min after 280 DEG C；The mL/min of carrier gas He flow velocitys 1.0, injector temperature are 250 DEG C, the μ L of sample size 1, split ratio
For 10:1；Mass Spectrometry Conditions：Using electron impact ion source EI ionization mode, ionization energy is 70eV, and ion source temperature is
230 DEG C, chromatogram and mass spectrographic transmission line temperature are 280 DEG C, 150 DEG C of quadrupole rod temperature, using scan mode and the quality of scanning
Scope is 30~500amu, qualitative to each chemical composition in cut with reference to database retrieval.
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Families Citing this family (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 |
| CN106706794B (en) * | 2017-01-04 | 2018-12-11 | 江苏中烟工业有限责任公司 | A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas |
| CN106908550B (en) * | 2017-04-06 | 2019-09-03 | 福建中烟工业有限责任公司 | A kind of method of Usneaceae plant characteristics ingredient in detection tobacco sample |
| CN109932436B (en) * | 2017-12-19 | 2022-04-12 | 湖南中烟工业有限责任公司 | Digital fragrance distinguishing method based on characteristic mass spectrum |
| CN110554120B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Detection method of tree moss fragrant ester substance |
| CN110568107B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Detection method of moss phenolic substances in moss plants or extracts |
| CN110554119B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Quantitative detection method for tree moss aroma phenolic substances |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| BG65650B1 (en) * | 2004-09-01 | 2009-04-30 | Солея ДАНЬО | Method for the evaluation of the aroma of tobacco smoke and classification by aroma of types and varieties of tobaccos |
| CN101393182B (en) * | 2008-10-23 | 2011-07-27 | 红云红河烟草(集团)有限责任公司 | Method for measuring fragrance quality of tobacco and products thereof |
| CN102495163B (en) * | 2011-11-17 | 2013-12-25 | 云南省烟草烟叶公司 | Establishing method and use of flue-cured tobacco GC/MS fingerprint |
| CN102654493A (en) * | 2012-05-08 | 2012-09-05 | 红云红河烟草(集团)有限责任公司 | Method of evaluating contribution rate of tobacco leaf raw material in cigarette formulation |
| CN102759588B (en) * | 2012-07-16 | 2014-05-07 | 上海烟草集团有限责任公司 | Method for separating and preparing key acid flavor components in cigarette mainstream smoke and application of key acid volatile components |
| CN104155395B (en) * | 2014-08-15 | 2016-04-27 | 江苏中烟工业有限责任公司 | A kind of high speed adverse current chromatogram method for separating of terpenes component in tree moss concrete |
| CN104178348B (en) * | 2014-08-15 | 2016-05-11 | 江苏中烟工业有限责任公司 | The separation method of main aroma component and the application in perfuming cigarette thereof in a kind of tree moss concrete |
| CN104745303A (en) * | 2015-04-10 | 2015-07-01 | 云南中烟工业有限责任公司 | Spice for cigarettes and application thereof |
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