CN106706794B - A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas - Google Patents
A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas Download PDFInfo
- Publication number
- CN106706794B CN106706794B CN201710003535.8A CN201710003535A CN106706794B CN 106706794 B CN106706794 B CN 106706794B CN 201710003535 A CN201710003535 A CN 201710003535A CN 106706794 B CN106706794 B CN 106706794B
- Authority
- CN
- China
- Prior art keywords
- solution
- cigarette
- standard
- standard working
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention provides a kind of methods of tongue fur faint scent characteristic chicken flavor substance main in quantitative analysis ramuscule cigarette mainstream flue gas, comprising the following steps: (1) preparation of inner mark solution；(2) preparation of standard working solution；(3) preparation of sample solution；(4) gas chromatography tandem mass spectrometry instrument is analyzed；(5) drafting of standard working curve and the calculating of sample result.The present invention has following excellent results: the method for the present invention creative use gas chromatography tandem mass spectrometry instrument measures 3 kinds of main micro fragrance matter contents such as divaricatic acid ethyl ester, orcin monomethyl ether and β-orcin carboxylate methyl ester of trace in ramuscule cigarette mainstream flue gas, solves the influence for the factors such as flue gas such chemical levels are low and flue gas complex matrices are serious to the Analysis interference of object.The high sensitivity of method, repeatability and the rate of recovery are preferable, are suitable for the quantitative analysis of trace object in ramuscule cigarette smoke complex matrices.
Description
Technical field
The invention discloses a kind of sides of tongue fur faint scent characteristic chicken flavor substance main in quantitative analysis ramuscule cigarette mainstream flue gas
Method, in particular to a kind of main tongue fur based on trace in gas-chromatography-tandem mass spectrometer measurement ramuscule cigarette smoke are clear
The method of fragrant characteristic chicken flavor substance belongs to cigarette physical and chemical index detection technique field.
Background technique
Ramuscule cigarette due to novel appearance, design fashion the features such as, receive trend of following the fashion, highlight self individual character,
The special favor of the consumption family of gracefulness life.Initially received in last century the eighties by United States Consumer, gradually
It is popular in Europe and Korean market, become an important pole for cigarette market.In recent years, specific gravity of the ramuscule cigarette in Chinese-style cigarette
It is stepped up with status.Chinese-style cigarette new category of the ramuscule cigarette as rapid growth, in fields such as lowering harm and decreasing coking, cost efficiency
There is natural advantage, while its fragrance present in aspiration procedure presents and strength satisfaction is also weaker than together to a certain extent
Class conventional cigarette, it is therefore necessary to hold use problem of the flavors and fragrances in ramuscule cigarette tobacco leaf formulation.
At the same time, there is natural plant resource abundant and extensive in view of the development need of Chinese-style cigarette and China
Traditional Chinese medical theory, many cigarette enterprises all put at present a large amount of human and material resources and financial resources exploitation meet respective cigarette style
Chinese herbal medicine, the plant resources class perfume material of feature, achieve gratifying research achievement, as " WUYESHENG " of cigarette development in Guangdong,
" gold holy " brand of Nanchang Cigarette Factory, Shanghai " Double Happiness ", Anhui " pellet is strong ", Changsha Cigarette Factory " white sand ", Shifang Cigarette Factory
The brands such as " national treasure ".It among these, also include " tongue fur faint scent " the style and features cigarette constantly favored by consumer.
Largely it turns out that, " tongue fur faint scent " style and features in cigarette smoke are mainly derived from a kind of outer flavoring source of tree moss
The application of material matter.Tree moss (treemoss), scientific name Evernia furfuraceae, alias Ramalina fastigiata, tree cauliflower are grown nonparasitically upon another plant
Lichens plant is more common on pine, fir, oak, dragon spruce or fir tree, belongs to Song Luoke with oak moss, medicinal extract or absolute oil product are equal
There is supply of commodities, common odor characteristic is a kind of natural green fragrant and strong resin breath of unique liverwort substance, but sets
Tongue fur fragrance is slightly poorer than oak moss, has pine gas, as the substitute of oak moss, adjustable chypre, fragrance surprise, lavender, all sorts of flowers,
The essence such as tongue fur perfume (or spice) have preferable fixation to act on.Currently, major tobacco company and its research institution all use tree moss more and more
Product assigns the unique aromatic style of cigarette product.
Currently, outer flavoring source material Quality Research a kind of for natural tree moss focus primarily upon chemical composition analysis and its
Two aspect such as effect assessment in perfuming cigarette.For example, Liu Qiang et al. is using solid phase microextraction and gas chromatography-mass spectrography point
The fragrance component of tree moss absolute and medicinal extract has been analysed, and has carried out perfuming cigarette test with tree moss absolute.The result shows that: 1. tree moss is net
The fragrance component of oil and medicinal extract composition is essentially identical, and main aromatic components are orcin double methyl ethers, orcin monomethyl ether, Ah
Blue phenol, methyl β-orcinolcarboxylate, red star clothing acid methyl esters, red star clothing acetoacetic ester, everninic acid ethyl ester, divaricatic acid methyl esters, palm fibre
Ethyl gallate, ethyl linoleate, ethyl oleate, ethyl stearte, rosin acid and methyl abietate etc.；2. tree moss absolute can assign
The fragrant aromatic style of the blueness of cigarette tongue fur sample, obviously increases flue gas concentration, and can improve the comfort of oral cavity and throat.Zhu Huaiyuan etc.
Molecular distillation technique is applied to the deep-processing process of natural plants extract type spice by people, and it is equal successfully to have developed a kind of character clarification
Liquid perfume even, quality is stable.The fragrance has the typical tongue fur faint scent odor characteristic of tree moss concrete, while eliminating tree moss
Most harmful substances in medicinal extract can be used to substitute tree moss concrete used in perfuming cigarette.
But up to the present, not yet discovery to tongue fur faint scent characteristic chicken flavor substance main in ramuscule cigarette mainstream flue gas into
The report of row accurate quantification analysis lacks the quantitative information of crucial tongue fur faint scent characteristic chicken flavor substance in single cigarette flue gas, in turn
The influence of lag is brought to the relationship between analysis of key fragrance matter and cigarette style characteristic.For this purpose, this patent uses GC-
The analysis means of MS/MS have carried out quantitative analysis to tongue fur faint scent characteristic chicken flavor substance main in ramuscule cigarette mainstream flue gas for the first time.
Summary of the invention
The present invention is directed to overcome existing technological deficiency, provide a kind of using gas chromatography tandem mass spectrometry instrument measurement ramuscule
The method of the main tongue fur faint scent characteristic chicken flavor content of material of trace in cigarette mainstream flue gas, this method energy accurate quantification analyze cigarette
The content of the main tongue fur faint scent characteristic chicken flavor substance of trace in main flume, measurement result is accurate, high sensitivity, matrix interference
It is few.
Technical scheme is as follows: main tongue fur faint scent characteristic chicken flavor in a kind of quantitative analysis ramuscule cigarette mainstream flue gas
The method of substance, comprising the following steps:
(1) preparation of inner mark solution: using heptadecane as internal standard compound, the use of methanol is solvent, prepares inner mark solution.
(2) preparation of standard working solution: with divaricatic acid ethyl ester, orcin monomethyl ether and β-orcin carboxylate methyl ester
The standard items of equal substances are object, the use of methanol are solvent, are diluted be prepared into Standard Stock solutions step by step, are then added respectively
Enter a certain amount of inner mark solution, is prepared into standard working solution.
(3) preparation of sample solution: gathering the object in cigarette smoke, be accurately added a certain amount of inner mark solution with
And the extractant of certain volume, mechanical shaking extraction obtain sample solution then to the excessively organic filter membrane of extract liquor.
(4) gas chromatography tandem mass spectrometry instrument is analyzed: being worked with gas chromatography tandem mass spectrometry instrument (GC-MS/MS) standard
Solution and sample solution are tested and analyzed.
(5) drafting of standard working curve and the calculating of sample result.
The preparation of the inner mark solution, specifically includes the following steps: (1) internal standard stock solution: accurately weighing 0.2g positive ten
Seven carbon alkane, are accurate to 0.1mg, in the volumetric flask of 100mL, are dissolved with methanol and are settled to scale.(2) inner mark solution: accurate
0.1mL internal standard stock solution is pipetted, in the volumetric flask of 100mL, with methanol dilution and is settled to scale.
The preparation of the standard working solution is specifically includes the following steps: (1) primary standard stock solution: accurately weighing
0.3g divaricatic acid ethyl ester, 0.1g orcin monomethyl ether and 0.25g β-orcin carboxylate methyl ester, are accurate to 0.1mg, in 50mL
Volumetric flask in, dissolved with methanol and be settled to scale.(2) secondary standard stock solution: 0.1mL primary standard deposit is accurately pipetted
Liquid with methanol dilution and is settled to scale in the volumetric flask of 50mL.(3) standard working solution: second level mark is accurately pipetted respectively
Quasi- 50 μ L of stock solution, 100 μ L, 300 μ L, 600 μ L, 1mL and 2mL, until in the volumetric flask of 10mL, then respectively in accurate addition 1mL
Solution is marked, with methanol dilution and scale is settled to, obtains series standard working solution.
The preparation of the sample solution is specifically includes the following steps: (1) cigarette smoking: according to 19609 standard of GB/T
It is required that 20 cigarette of suction, wherein with the granule phase substance in cambridge filter trapping cigarette mainstream flue gas.(2) granule phase substance extracts: will catch
The cambridge filter of collection cigarette mainstream smoke condensate is transferred in 250mL bread bottle, is that solvent carries out oscillation extraction with 40mL methanol
It takes, extraction time 40min, is then filtered using 0.45 μm of organic phase filter membrane to get sample solution is arrived.
The GC-MS/MS analysis, instrumental conditions are as follows: use the HP-INNOWAX (μ of 30m × 0.25mm × 0.25
M) capillary chromatographic column；Carrier gas is helium, and constant current speed is 1.0mL/min；Input mode: sample volume is 1 μ L, and pulse does not shunt
Sample introduction, sample introduction pulse are 25psi, time 1min；Injector temperature is 240 DEG C；Transmission line temperature is 260 DEG C；Heating
Program is that initial temperature is 80 DEG C, is increased to 240 DEG C with the rate of 5 DEG C/min, keeps 18min.Its mass spectral analysis condition are as follows: electricity
It is the source EI, positive ion mode from mode；Ion source temperature: 230 DEG C；Quadrupole rod temperature: being 150 DEG C；Collision gas: nitrogen, stream
Fast 1.5mL/min, carrier gas (helium) flow velocity are 2.25mL/min；Multiple-reaction monitoring (MRM) mode, detail parameters are listed in the table below.
The MRM parameter situation of object
The Specification Curve of Increasing and result calculate as follows: with object in standard working solution and interior target concentration it
Than carrying out linear regression analysis with the ratio between object in chromatogram and interior target peak area for ordinate for abscissa, being marked
Quasi- working curve.By object in the sample solution measured under the same terms and interior target chromatographic peak area ratio, standard work is substituted into
Make curve, the content of object in cigarette sample is acquired according to following equation.
In formula:
W --- the content of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances in ramuscule cigarette mainstream flue gas, unit are nanogram every
(ng/ branch)；
A --- the peak area of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances；
As --- target peak area in corresponding；
The intercept of b --- standard working curve；
Ms --- target quality in adding, unit are nanogram (ng)；
The slope of a --- standard working curve；
The quantity of M --- cigarette, unit are branch.
The utility model has the advantages that sample treatment and chromatograph mass spectrum analysis condition is optimized really in detection method of the invention
Recognize.Compared with prior art, the present invention has following excellent results:
(1) trace in the method for the present invention creative use gas chromatography tandem mass spectrometry instrument measurement ramuscule cigarette mainstream flue gas
3 kinds of divaricatic acid ethyl ester, orcin monomethyl ether and β-orcin carboxylate methyl ester etc. main micro fragrance matter contents, solve
The influence for the factors such as such chemical levels of flue gas are low and flue gas complex matrices are serious to the Analysis interference of object.
(2) for object content in fume sample, low, serious interference feature, innovation use " extraction to the method for the present invention
Solution direct injected+pulse does not shunt " analytical model, not only simplify sample pretreatment process, and improve the sound of object
Answer sensitivity.
(3) the method for the present invention utilizes inner mark method ration, can not have to accurate constant volume, and can reduce by pre-treating method weight
Existing property and instrument precision problem bring error.
Detailed description of the invention
Fig. 1 is the flow chart of measuring method of the present invention；
Fig. 2 is the ion pair of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances and internal standard heptadecane in standard working solution
Chromatogram；
Fig. 3 is the ion pair of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances and internal standard heptadecane in cigarette mainstream flue gas
Chromatogram.
Specific embodiment
Embodiment 1
The present embodiment is as follows to the detection method of the main tongue fur faint scent characteristic chicken flavor substance of trace in ramuscule cigarette mainstream flue gas
(flow chart of the detection method is as shown in Figure 1):
(1) preparation of inner mark solution
1. internal standard stock solution: accurately weighing 0.2020g heptadecane, in the volumetric flask of 100mL, simultaneously with methanol dissolution
It is settled to scale.
2. inner mark solution: accurately 0.1mL internal standard stock solution is pipetted, in the volumetric flask of 100mL, with methanol dilution and constant volume
To scale.Wherein the concentration of heptadecane is 2.02 μ g/mL.
(2) preparation of standard working solution
1. primary standard stock solution: accurately weigh 0.2986g divaricatic acid ethyl ester, 0.1169g orcin monomethyl ether and
0.2499g β-orcin carboxylate methyl ester, is accurate to 0.1mg, in the volumetric flask of 50mL, is dissolved with methanol and is settled to scale.
2. secondary standard stock solution: accurately pipetting 0.1mL primary standard stock solution uses methanol in the volumetric flask of 50mL
It dilutes and is settled to scale.
3. standard working solution: accurately pipette respectively 50 μ L of secondary standard stock solution, 100 μ L, 300 μ L, 600 μ L, 1mL and
2mL, until in the volumetric flask of 10mL, then accurate addition 1mL inner mark solution respectively, with methanol dilution and it is settled to scale, is obtained serial
Standard working solution.Wherein the concentration range of divaricatic acid ethyl ester is 0.0597~2.389 μ g/mL, orcin monomethyl ether
Concentration range is 0.02338~0.9352 μ g/mL, β-orcin carboxylate methyl ester concentration range is 0.04995~1.998 μ g/
ML, wherein the concentration of internal standard compound is 0.202 μ g/mL.
(3) preparation of sample solution
1. cigarette smoking: it is object that ramuscule cigarette is sold in the city Yi Yi, aspirates 20 volumes according to the requirement of 19609 standard of GB/T
Cigarette, wherein with the granule phase substance in cambridge filter trapping cigarette mainstream flue gas.
2. granule phase substance extracts: the cambridge filter for trapping cigarette mainstream smoke condensate being transferred in 250mL bread bottle, is added
Enter 1mL inner mark solution, is that solvent carries out oscillation extraction with 40mL methanol, extraction time 40min is then organic using 0.45 μm
Phase filter membrane is filtered to arrive sample solution.
(4) gas chromatography tandem mass spectrometry is analyzed
The standard working solution and sample solution to be measured for taking 6 various concentrations respectively carry out gas chromatography tandem mass spectrometry analysis
(chromatogram of object and internal standard compound is as shown in Figure 2 to 3 in the standard working solution, typical sample solution).
Its instrumental conditions are as follows: use HP-INNOWAX (30m × 0.25mm × 0.25 μm) capillary chromatographic column；Carrier gas
For helium, constant current speed is 1.0mL/min；Input mode: sample volume is 1 μ L, and pulse Splitless injecting samples, sample introduction pulse is
25psi, time 1min；Injector temperature is 240 DEG C；Transmission line temperature is 260 DEG C；Temperature program is that initial temperature is 80
DEG C, 240 DEG C are increased to the rate of 5 DEG C/min, keeps 18min.Its mass spectral analysis condition are as follows: ionization mode be the source EI, just from
Subpattern；Ion source temperature: 230 DEG C；Quadrupole rod temperature: being 150 DEG C；Collision gas: nitrogen, flow velocity 1.5mL/min, carrier gas
(helium) flow velocity is 2.25mL/min；Multiple-reaction monitoring (MRM) mode, detail parameters are listed in the table below.
The MRM parameter situation of object
(5) Specification Curve of Increasing and result calculate
Firstly, with the ratio between object in standard working solution and interior target concentration for abscissa, with object in chromatogram
It is ordinate with the ratio between interior target peak area, carries out linear regression analysis, obtain standard working curve.Take the standard of minimum concentration
Working solution does 9 Parallel testing analyses, calculates its standard deviation, with the corresponding concentration of 3 times of standard deviation, conversion is obtained
The detection limit of method.The data such as regression equation corresponding with standard working curve, related coefficient, detection limit see the table below.
The working curve and detection limit of analysis method
By object in the sample solution measured under the same terms and interior target chromatographic peak area ratio, it is bent to substitute into standard work
Line acquires the content of object in cigarette sample according to following equation.
In formula:
W --- the content of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances in ramuscule cigarette mainstream flue gas, unit are nanogram every
(ng/ branch)；
A --- the peak area of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances；
As --- target peak area in corresponding；
The intercept of b --- standard working curve；
Ms --- target quality in adding, unit are nanogram (ng)；
The slope of a --- standard working curve；
The quantity of M --- cigarette, unit are branch.
3 kinds of main tongue fur faint scent characteristic chicken flavor substance testing results are seen below in ramuscule cigarette sample main flume in the present embodiment
Table:
Embodiment 2
The present embodiment is as follows to the detection method of precision and recovery of standard addition of the invention:
It is analysis object with ramuscule cigarette sample used in embodiment 1, has carried out withinday precision experiment respectively, in a few days
Precision Experiment is that same sample is measured in parallel 6 times (same batch processed) under identical conditions, calculates separately 6 parallel determinations
As a result relative standard deviation (RSD), measurement result see the table below.In table the results show that this experimental method it is in a few days repeated
RSD < 10% shows that method has good precision for the quantitative analysis of trace materials.
It is analysis object with ramuscule cigarette sample used in repetitive test, at above-mentioned sample-pretreating method
The standard specimen of the comparable content of its burst size is added in reason, carries out the test of matrix mark-on, as a result see the table below.As can be seen from the table, sample
For the recovery of standard addition of product between 87.39%~113.75%, illustration method has preferable accuracy.
What standard solution used in the present embodiment was only illustrated by taking one of concentration as an example, other concentration value institutes
The standard solution of preparation analyzes standard curve and regression equation and above-described embodiment obtained through gas chromatography tandem mass spectrometry instrument
It is identical, it is not enumerating herein.Illustrated embodiment is intended merely to better understand the method for the present invention, and does not have any restrictions
Effect, the i.e. method of the above method or equivalent above situation are all contained in the protection scope of technical solution of the present invention.
Claims (4)
1. a kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas, including following step
It is rapid:
(1) preparation of inner mark solution: using heptadecane as internal standard compound, the use of methanol is solvent, prepares inner mark solution；
(2) preparation of standard working solution: with divaricatic acid ethyl ester, orcin monomethyl ether and β-orcin carboxylate methyl ester mark
Quasi- product are object, the use of methanol are solvent, are prepared into Standard Stock solutions through diluting step by step, are then respectively adding a certain amount of
Inner mark solution is prepared into standard working solution；
(3) preparation of sample solution: gathering the object in cigarette smoke, and inner mark solution and extractant, oscillation is added
It extracts, then to the excessively organic filter membrane of extract liquor, obtains sample solution；
(4) gas chromatography tandem mass spectrometry instrument is analyzed:
Standard working solution and sample solution are tested and analyzed with gas chromatography tandem mass spectrometry instrument GC-MS/MS；
The GC-MS/MS analysis, instrumental conditions are as follows: use 30m × 0.25mm × 0.25 μm HP-INNOWAX hair
Capillary chromatographic column；Carrier gas is helium, and constant current speed is 1.0mL/min；Input mode: sample volume is 1 μ L, and pulse is not diverted into
Sample, sample introduction pulse are 25psi, time 1min；Injector temperature is 240 DEG C；Transmission line temperature is 260 DEG C；Heat up journey
Sequence is that initial temperature is 80 DEG C, is increased to 240 DEG C with the rate of 5 DEG C/min, keeps 18min；
The mass spectral analysis condition are as follows: ionization mode is the source EI, positive ion mode；Ion source temperature: 230 DEG C；Quadrupole rod temperature
Degree: 150 DEG C；Collision gas: nitrogen, flow velocity 1.5mL/min, carrier gas helium flow velocity are 2.25mL/min；Multiple-reaction monitoring MRM mould
Formula, detail parameters are listed in the table below:
The MRM parameter situation of object
(5) drafting of standard working curve and the calculating of sample result, the standard working curve is drawn and result calculates such as
Under: with the ratio between object in standard working solution and interior target concentration for abscissa, with object in chromatogram and interior target peak
Area ratio is ordinate, carries out linear regression analysis, obtains standard working curve；The sample solution that will be measured under the same terms
Middle object and interior target chromatographic peak area ratio substitute into standard working curve, acquire target in cigarette sample according to following equation
The content of object:
In formula:
W --- the content of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances in ramuscule cigarette mainstream flue gas, unit are every ng/ of nanogram
Branch；
A --- the peak area of 3 kinds of main tongue fur faint scent characteristic chicken flavor substances；
As --- target peak area in corresponding；
The intercept of b --- standard working curve；
Ms --- target quality in adding, unit are nanogram ng；
The slope of a --- standard working curve；
The quantity of M --- cigarette, unit are branch.
2. measuring method according to claim 1, it is characterised in that: the preparation of the inner mark solution, specifically include with
Lower step:
(1) internal standard stock solution: weighing 0.2g heptadecane, be accurate to 0.1mg, in the volumetric flask of 100mL, is dissolved with methanol
And it is settled to scale；
(2) inner mark solution: 0.1mL internal standard stock solution accurately is pipetted, in the volumetric flask of 100mL, with methanol dilution and is settled to
Scale.
3. measuring method according to claim 1, it is characterised in that: the preparation of the standard working solution specifically includes
Following steps:
(1) 0.3g divaricatic acid ethyl ester, 0.1g orcin monomethyl ether and 0.25g β-tongue fur primary standard stock solution: are accurately weighed
Black phenol carboxylate methyl ester, is accurate to 0.1mg, in the volumetric flask of 50mL, is dissolved with methanol and is settled to scale；
(2) secondary standard stock solution: accurately pipetting 0.1mL primary standard stock solution uses methanol dilution in the volumetric flask of 50mL
And it is settled to scale；
(3) standard working solution: accurately pipette respectively 50 μ L of secondary standard stock solution, 100 μ L, 300 μ L, 600 μ L, 1mL and
2mL, until in the volumetric flask of 10mL, then accurate addition 1mL inner mark solution respectively, with methanol dilution and it is settled to scale, is obtained serial
Standard working solution.
4. measuring method according to claim 1, it is characterised in that: the preparation of the sample solution specifically includes following
Step:
(1) cigarette smoking: 20 cigarette are aspirated according to the requirement of 19609 standard of GB/T, wherein trapping cigarette master with cambridge filter
Flow the granule phase substance in flue gas；
(2) granule phase substance extracts: the cambridge filter for trapping cigarette mainstream smoke condensate being transferred in 250mL bread bottle, is added
1mL inner mark solution is that solvent carries out oscillation extraction with 40mL methanol, then extraction time 40min uses 0.45 μm of organic phase
Filter membrane is filtered to arrive sample solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003535.8A CN106706794B (en) | 2017-01-04 | 2017-01-04 | A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003535.8A CN106706794B (en) | 2017-01-04 | 2017-01-04 | A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106706794A CN106706794A (en) | 2017-05-24 |
| CN106706794B true CN106706794B (en) | 2018-12-11 |
Family
ID=58906648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710003535.8A Active CN106706794B (en) | 2017-01-04 | 2017-01-04 | A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106706794B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107510092A (en) * | 2017-09-12 | 2017-12-26 | 云南中烟工业有限责任公司 | A kind of cigarette shreds additive of tree moss note and its preparation method and application |
| CN107354007A (en) * | 2017-09-12 | 2017-11-17 | 云南中烟工业有限责任公司 | A kind of cigarette bobbin paper additive of tree moss note and its preparation method and application |
| CN108267523A (en) * | 2018-01-24 | 2018-07-10 | 江苏中烟工业有限责任公司 | A kind of ramuscule cigarette mainstream is by the computational methods of aldoketones substance in mouth flue gas |
| CN109212106A (en) * | 2018-11-20 | 2019-01-15 | 东营市海科新源化工有限责任公司 | Be heated easy decomposed substance or the gas chromatography analysis method containing micro target substance |
| CN110018248B (en) * | 2019-03-22 | 2022-05-24 | 河南中烟工业有限责任公司 | Tree moss absolute oil selection method for cigarettes |
| CN110568106B (en) * | 2019-10-17 | 2021-08-03 | 云南中烟工业有限责任公司 | Quantitative detection method for turpentine substances in turpentine 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 |
| 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 |
| 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 |
| CN111289677B (en) * | 2020-03-31 | 2023-04-14 | 中国烟草总公司郑州烟草研究院 | Method for measuring spicy components in main stream smoke of cigarette |
| CN113567608A (en) * | 2021-07-26 | 2021-10-29 | 福建中烟工业有限责任公司 | Method for measuring characteristic components of strokes in flavored cut tobacco and absorption rate and equipment evaluation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041174A (en) * | 2011-01-07 | 2011-05-04 | 江苏中烟工业有限责任公司 | Preparation method of moss-scented tobacco flavor and application of moss-scented cigarette flavor in cigarette flavoring |
| CN103333743A (en) * | 2013-07-10 | 2013-10-02 | 江苏中烟工业有限责任公司 | Essence with moss faint scent and applications thereof |
| CN104178348A (en) * | 2014-08-15 | 2014-12-03 | 江苏中烟工业有限责任公司 | Separation method of main aroma components in tree moss concrete and application of main aroma components in cigarette perfuming |
| CN105738530A (en) * | 2016-04-29 | 2016-07-06 | 江苏中烟工业有限责任公司 | Method for optioning aroma component in natural moss perfume spice |
| CN105768198A (en) * | 2016-04-29 | 2016-07-20 | 江苏中烟工业有限责任公司 | Electronic cigarette juice with moss faint scent feature and preparation method thereof |
| CN105837442A (en) * | 2016-04-29 | 2016-08-10 | 江苏中烟工业有限责任公司 | Separation method for aromatic component divaicatic acid ethyl ester in moss fen-flavor spice |
-
2017
- 2017-01-04 CN CN201710003535.8A patent/CN106706794B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041174A (en) * | 2011-01-07 | 2011-05-04 | 江苏中烟工业有限责任公司 | Preparation method of moss-scented tobacco flavor and application of moss-scented cigarette flavor in cigarette flavoring |
| CN103333743A (en) * | 2013-07-10 | 2013-10-02 | 江苏中烟工业有限责任公司 | Essence with moss faint scent and applications thereof |
| CN104178348A (en) * | 2014-08-15 | 2014-12-03 | 江苏中烟工业有限责任公司 | Separation method of main aroma components in tree moss concrete and application of main aroma components in cigarette perfuming |
| CN105738530A (en) * | 2016-04-29 | 2016-07-06 | 江苏中烟工业有限责任公司 | Method for optioning aroma component in natural moss perfume spice |
| CN105768198A (en) * | 2016-04-29 | 2016-07-20 | 江苏中烟工业有限责任公司 | Electronic cigarette juice with moss faint scent feature and preparation method thereof |
| CN105837442A (en) * | 2016-04-29 | 2016-08-10 | 江苏中烟工业有限责任公司 | Separation method for aromatic component divaicatic acid ethyl ester in moss fen-flavor spice |
Non-Patent Citations (3)
| Title |
|---|
| 分子蒸馏和同时蒸馏萃取法分析树苔浸膏的化学成分;朱怀远 等;《食品科学》;20121231;第33卷(第10期);第212-217页 * |
| 树苔浸膏、净油香味成分分析及其在卷烟中的应用;刘强 等;《烟草科技》;20051231(第3期);第18-21页 * |
| 气相色谱－质谱法分析树苔浸膏的成分;朱怀远 等;《理化检验（化学分册）》;20121231;第48卷(第11期);第1326-1330页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106706794A (en) | 2017-05-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106706794B (en) | A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas | |
| CN106053628B (en) | A kind of method that fast qualitative quantifies fragrance component in tealeaves | |
| CN104316634B (en) | The measuring method of volatile organic acids in a kind of cigarette mainstream flue gas | |
| CN105784912B (en) | A kind of method of lactone fragrance matter in quantitative analysis ramuscule cigarette mainstream flue gas | |
| CN106053653A (en) | Analytical method for identifying flavor characteristic index compound of chilli oil | |
| CN104931605A (en) | Method for detecting quality of pepper powder based on component analysis | |
| CN104792895B (en) | The assay method of menthol in a kind of essence spice for cigarette | |
| CN106226417B (en) | The detection method of polyol ethers and its ester type compound in a kind of tobacco juice for electronic smoke | |
| CN106442753B (en) | A kind of method of TSNAs content in measurement cigarette mainstream flue gas | |
| CN104914184A (en) | Cold trap capturing-gas chromatography/mass spectrum combined detection method for furan in cigarette mainstream smoke | |
| CN106841444A (en) | A kind of method of quantitative analysis ramuscule cigarette main flow by main Alkaloid in mouth flue gas | |
| CN108267523A (en) | A kind of ramuscule cigarette mainstream is by the computational methods of aldoketones substance in mouth flue gas | |
| CN114235981A (en) | Method for identifying perilla leaf essential oil by combining gas-mass spectrometry-sniffing instrument and gas chromatography-ion mobility spectrometry | |
| CN107064364A (en) | The assay method of Performance Liquid Chromatography Analysis for Nicotine in Tobacco optical isomer | |
| CN109521123B (en) | Application of PMP-HPLC method in identification of garden ginseng and forest ginseng | |
| CN107037151A (en) | A kind of assay method of transfer volume of epoxy chloropropane in food contact material | |
| CN106442750B (en) | A kind of method of free gossypol detoxification situation in evaluation cottonseed oil | |
| CN105954434A (en) | Method for detecting phenols spice | |
| CN108088932B (en) | Method for calculating furan substances in mainstream smoke of fine cigarettes | |
| CN110514757A (en) | A kind of method of Volatile flavor components in fast resolving white wine | |
| CN107589204B (en) | Method for determining anthranilate grape essence in wine by gas chromatography-mass spectrometry | |
| CN114217002B (en) | Method for detecting contents of chamomile azulene and sabinene in chamomile essential oil | |
| CN103399111B (en) | Method for selectively measuring ethylene glycol monoethyl ether acetate in dry food packaging paper based on headspace-gas chromatography/mass spectrometry | |
| CN101936970B (en) | Method for determining acrylate compounds in polypropylene fiber adhesive for cigarettes | |
| CN115950979A (en) | Method for tracing origin of complex matrix tobacco extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |