CN106706794A - Quantitative analysis method of main moss fragrance characteristics flavor component in fine cigarette mainstream smoke - Google Patents

Quantitative analysis method of main moss fragrance characteristics flavor component in fine cigarette mainstream smoke Download PDF

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CN106706794A
CN106706794A CN201710003535.8A CN201710003535A CN106706794A CN 106706794 A CN106706794 A CN 106706794A CN 201710003535 A CN201710003535 A CN 201710003535A CN 106706794 A CN106706794 A CN 106706794A
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cigarette
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CN106706794B (en
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廖惠云
庄亚东
张华�
秦艳华
熊晓敏
石怀彬
韩开冬
朱莹
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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
    • 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
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • 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
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/062Preparation extracting sample from raw material

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Abstract

The invention provides a quantitative analysis method of main moss fragrance characteristics flavor components in fine cigarette mainstream smoke. The method comprises the following steps of (1), internal standard solution preparation; (2), standard work solution preparation; (3), sample solution preparation; (4), gas chromatography and tandem mass spectrometer analysis; (5), standard work curve drawing and sample result calculation. The quantitative analysis method of the main moss fragrance characteristics flavor components in fine cigarette mainstream smoke has the advantages that according to the quantitative analysis method, three main micro flavor component contents including soft evernia ethyl acetate, Monomethyl phenol monomethyl ether, beta Monomethyl phenol carboxylic acid methyl ester and the like of trace amount in the fine cigarette mainstream smoke are measured by using the gas chromatography and tandem mass spectrometer, and influence by the low content of the compound in the smoke and severe disturbance for the analysis of the objects of the smoke complex matrix is avoided. The quantitative analysis method of the main moss fragrance characteristics flavor components in fine cigarette mainstream smoke is high in sensitivity, high in repeatability and recovery rate, and suitable for the quantitative analysis of the trace amount objects in the fine cigarette smoke complex matrix.

Description

Main tongue delicate fragrance characteristic chicken flavor material in a kind of quantitative analysis ramuscule cigarette mainstream flue gas Method
Technical field
The invention discloses a kind of side of main tongue delicate fragrance characteristic chicken flavor material in quantitative analysis ramuscule cigarette mainstream flue gas Method, in particular to a kind of main tongue based on trace in gas-chromatography-tandem mass spectrometer measure ramuscule cigarette smoke is clear The method of fragrant characteristic chicken flavor material, belongs to cigarette physical and chemical index detection technique field.
Background technology
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 by United States Consumer in last century the eighties, gradually Popular, the important pole as cigarette market in Europe and Korean market.In recent years, proportion of the ramuscule cigarette in Chinese-style cigarette Stepped up with status.Ramuscule cigarette as rapid growth the new category of Chinese-style cigarette, in fields such as lowering harm and decreasing coking, cost efficiency There is natural advantage, while its fragrance present in aspiration procedure is presented 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 essence and flavoring agent in ramuscule cigarette tobacco leaf formulation.
At the same time, in view of the development need of Chinese-style cigarette, and China has abundant natural plant resource and extensive Traditional Chinese medical theory, many cigarette enterprises all put at present substantial amounts of human and material resources and financial resources exploitation meet respective cigarette style The Chinese herbal medicine of feature, plant resources class perfume material, achieve gratifying achievement in research, such as in Guangdong cigarette develop " WUYESHENG ", " gold is holy " brand of Nanchang Cigarette Factory, Shanghai " Double Happiness ", Anhui " pellet is strong ", " white sand " of Changsha Cigarette Factory, Shifang Cigarette Factory The brand such as " national treasure ".Among these, also comprising " tongue delicate fragrance " the style and features cigarette constantly favored by consumer.
It is substantial amounts of it turns out that, " tongue delicate fragrance " style and features in cigarette smoke are mainly derived from the outer perfuming source of the class of tree moss one 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, and Song Luoke is belonged to together with oak moss, and its medicinal extract or absolute oil product are equal There is supply of commodities, common odor characteristic is a kind of fragrant and strong resin breath of natural green grass or young crops of unique liverwort material, but is set Tongue fragrance is slightly poorer than oak moss, with pine gas, as the substitute of oak moss, adjustable chypre, fragrance are strange, lavender, all sorts of flowers, The essence such as tongue perfume (or spice), have preferable fixation to act on.At present, major tobacco companies and its research institution are all increasingly using tree moss Product assigns cigarette product unique aromatic style.
At present, for the outer perfuming source material Quality Research of the natural class of tree moss one focus primarily upon chemical composition analysis and its The aspect of effect assessment in perfuming cigarette etc. two.Such as, Liu Qiang et al. is using SPME and gas chromatography-mass spectrography point The fragrance component of tree moss absolute and medicinal extract is analysed, and perfuming cigarette experiment has been carried out with tree moss absolute.Result shows:1. tree moss is net The fragrance component composition of oil and medicinal extract is essentially identical, its main aromatic components be the double methyl ethers of orcin, 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 be assigned The green grass or young crops perfume aromatic style of cigarette tongue sample, substantially increases flue gas concentration, and can improve the comfort of oral cavity and throat.Zhu Huaiyuan etc. Molecular distillation technique is applied to people the deep-processing process of natural plants extract type spice, successfully have developed a kind of proterties clarification equal Even, steady quality liquid perfume.The spices has the typical tongue delicate fragrance odor characteristic of tree moss concrete, while eliminating tree moss Most harmful substances in medicinal extract, can be used to substitute the tree moss concrete used in perfuming cigarette.
But, up to the present, not yet find to enter main tongue delicate fragrance characteristic chicken flavor material in ramuscule cigarette mainstream flue gas The report of row accurate quantification analysis, lacks the quantitative information of crucial tongue delicate fragrance characteristic chicken flavor material in single cigarette flue gas, and then Delayed influence is brought to the relation between analysis of key fragrance matter and cigarette style characteristic.Therefore, this patent uses GC- The analysis means of MS/MS, have carried out quantitative analysis to main tongue delicate fragrance characteristic chicken flavor material in ramuscule cigarette mainstream flue gas first.
The content of the invention
It is contemplated that overcoming existing technological deficiency, there is provided one kind determines ramuscule using gas chromatography tandem mass spectrometry instrument The method of the main tongue delicate fragrance characteristic chicken flavor content of material of trace in cigarette mainstream flue gas, the method energy accurate quantification analysis cigarette The content of the main tongue delicate fragrance characteristic chicken flavor material of trace in main flume, measurement result is accurate, sensitivity is high, matrix interference It is few.
Technical scheme is as follows:Main tongue delicate fragrance characteristic chicken flavor in a kind of quantitative analysis ramuscule cigarette mainstream flue gas The method of material, comprises the following steps:
(1) preparation of inner mark solution:The use of methyl alcohol is solvent with heptadecane as internal standard compound, prepares inner mark solution.
(2) preparation of standard working solution:With divaricatic acid ethyl ester, orcin monomethyl ether and β-orcin carboxylate methyl ester Standard items Deng material are object, the use of methyl alcohol are solvent, and Standard Stock solutions are prepared into through stepwise dilution, are then added respectively Enter a certain amount of inner mark solution, be prepared into standard working solution.
(3) preparation of sample solution:Gather the object in cigarette smoke, accurately add a certain amount of inner mark solution with And the extractant of certain volume, mechanical shaking extraction, then to the excessively organic filter membrane of extract, obtain sample solution.
(4) gas chromatography tandem mass spectrometry instrument analysis:Standard is worked with gas chromatography tandem mass spectrometry instrument (GC-MS/MS) Solution and sample solution are tested and analyzed.
(5) drafting of standard working curve and the calculating of sample result.
The preparation of described inner mark solution, specifically includes following steps:(1) internal standard storing solution:Accurately weigh 0.2g positive ten Seven carbon alkane, are accurate to 0.1mg, in the volumetric flask of 100mL, scale are dissolved and be settled to methyl alcohol.(2) inner mark solution:Accurately 0.1mL internal standard storing solutions are pipetted, in the volumetric flask of 100mL, with methanol dilution and scale is settled to.
The preparation of described standard working solution specifically includes following steps:(1) primary standard storing solution:Accurately weigh 0.3g divaricatic acids ethyl ester, 0.1g orcins monomethyl ether and 0.25g β-orcin carboxylate methyl ester, are accurate to 0.1mg, in 50mL Volumetric flask in, scale is dissolved and is settled to methyl alcohol.(2) secondary standard storing solution:Accurately pipette 0.1mL primary standard deposits Liquid, in the volumetric flask of 50mL, with methanol dilution and is settled to scale.(3) standard working solution:Two grades of marks are accurately pipetted respectively The μ L of quasi- storing solution 50,100 μ L, 300 μ L, 600 μ L, 1mL and 2mL, into the volumetric flask of 10mL, then respectively in accurate addition 1mL Mark solution, with methanol dilution and is settled to scale, obtains series standard working solution.
The preparation of described sample solution specifically includes following steps:(1) cigarette smoking:According to the standards of GB/T 19609 It is required that 20 cigarette of suction, wherein trapping the granule phase substance in cigarette mainstream flue gas with cambridge filter.(2) granule phase substance extraction:To catch The cambridge filter for collecting cigarette mainstream smoke condensate is transferred in 250mL bread bottle, is that solvent carries out vibration extraction with 40mL methyl alcohol Take, extraction time is 40min, then filtered using 0.45 μm of organic phase filter membrane, that is, obtain sample solution.
Described GC-MS/MS is analyzed, and its instrumental conditions is:Using HP-INNOWAX (30m × 0.25mm × 0.25 μ M) capillary chromatographic column;Carrier gas is helium, and constant current speed is 1.0mL/min;Input mode:Sample size is 1 μ L, and pulse is not shunted Sample introduction, sample introduction pulse is 25psi, and the time is 1min;Injector temperature is 240 DEG C;Transmission line temperature is 260 DEG C;Heat up Program is that initial temperature is 80 DEG C, and 240 DEG C are increased to the speed of 5 DEG C/min, keeps 18min.Its mass spectral analysis condition is:Electricity It is EI sources, positive ion mode from mode;Ion source temperature:230℃;Quadrupole rod temperature:It is 150 DEG C;Collision gas:Nitrogen, stream Fast 1.5mL/min, carrier gas (helium) flow velocity is 2.25mL/min;Multiple-reaction monitoring (MRM) pattern, detail parameters are listed in the table below.
The MRM parameter situations of object
Described Specification Curve of Increasing and result is calculated as follows:With object in standard working solution and interior target concentration it Than being abscissa, with the ratio between object in chromatogram and interior target peak area as ordinate, linear regression analysis is carried out, marked Quasi- working curve.Object and interior target chromatographic peak area ratio in the sample solution that will be measured under the same terms, substitute into standard work Make curve, the content of object in cigarette sample is tried to achieve according to following equation.
In formula:
W --- 3 kinds of contents of main tongue delicate fragrance characteristic chicken flavor material in ramuscule cigarette mainstream flue gas, unit is nanogram every (ng/ branch);
A --- 3 kinds of peak areas of main tongue delicate fragrance characteristic chicken flavor material;
As --- target peak area in correspondence;
The intercept of b --- standard working curve;
Ms --- target quality in addition, unit is nanogram (ng);
The slope of a --- standard working curve;
The quantity of M --- cigarette, unit is branch.
Beneficial effect:Detection method of the invention is optimized really to sample treatment and chromatograph mass spectrum analysis condition Recognize.Compared with prior art, the present invention has following excellent results:
(1) trace in the inventive method creative use gas chromatography tandem mass spectrometry instrument measure ramuscule cigarette mainstream flue gas The main micro fragrance matter content of 3 kinds of divaricatic acid ethyl ester, orcin monomethyl ether and β-orcin carboxylate methyl ester etc., solves Such chemical levels of flue gas are low, and the factor such as flue gas complex matrices are serious to the Analysis interference of object influence.
(2), for object content in fume sample is low, serious interference feature, innovation is using " extraction for the inventive method Solution direct injected+pulse is not shunted " analytical model, both simplify sample pretreatment process, the sound of object is improve again Answer sensitivity.
(3) the inventive method utilizes inner mark method ration, without accurate constant volume, and be able to can reduce by pre-treating method weight The error that existing property and instrument precision problem are brought.
Brief description of the drawings
Fig. 1 is the flow chart of assay method of the present invention;
Fig. 2 is the ion pair of 3 kinds of main tongue delicate fragrance characteristic chicken flavor materials and internal standard heptadecane in standard working solution Chromatogram;
Fig. 3 is the ion pair of 3 kinds of main tongue delicate fragrance characteristic chicken flavor materials 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 delicate fragrance characteristic chicken flavor material 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 storing solution:0.2020g heptadecanes accurately are weighed, in the volumetric flask of 100mL, is dissolved simultaneously with methyl alcohol It is settled to scale.
2. inner mark solution:0.1mL internal standard storing solutions accurately are 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 storing solution:It is accurate weigh 0.2986g divaricatic acids ethyl ester, 0.1169g orcins monomethyl ether and 0.2499g β-orcin carboxylate methyl ester, are accurate to 0.1mg, in the volumetric flask of 50mL, scale are dissolved and be settled to methyl alcohol.
2. secondary standard storing solution:0.1mL primary standard storing solutions accurately are pipetted, in the volumetric flask of 50mL, methyl alcohol is used Dilute and be settled to scale.
3. standard working solution:Accurately pipette respectively the μ L of secondary standard storing solution 50,100 μ L, 300 μ L, 600 μ L, 1mL and 2mL, into the volumetric flask of 10mL, then it is accurate respectively add 1mL inner mark solutions, with methanol dilution and be settled to scale, obtain serial Standard working solution.The concentration range of wherein divaricatic acid ethyl ester is 0.0597~2.389 μ g/mL, orcin monomethyl ether Concentration range is that the concentration range of 0.02338~0.9352 μ g/mL, β-orcin carboxylate methyl ester is 0.04995~1.998 μ g/ The concentration of mL, wherein internal standard compound is 0.202 μ g/mL.
(3) preparation of sample solution
1. cigarette smoking:Yi Yi cities pin ramuscule cigarette is object, and 20 volumes are aspirated according to the requirement of the standards of GB/T 19609 Cigarette, wherein trapping the granule phase substance in cigarette mainstream flue gas with cambridge filter.
2. granule phase substance extraction:The cambridge filter for trapping cigarette mainstream smoke condensate is transferred in 250mL bread bottle, plus Enter 1mL inner mark solutions, be that solvent carries out oscillation extraction with 40mL methyl alcohol, extraction time is 40min, then organic using 0.45 μm Phase filter membrane is filtered, that is, obtain sample solution.
(4) gas chromatography tandem mass spectrometry analysis
Standard working solution and the sample solution to be measured for taking 6 various concentrations respectively carry out gas chromatography tandem mass spectrometry analysis (in the standard working solution, typical sample solution the chromatogram of object and internal standard compound as shown in Figure 2 to 3).
Its instrumental conditions is:Using HP-INNOWAX (30m × 0.25mm × 0.25 μm) capillary chromatographic column;Carrier gas It is helium, constant current speed is 1.0mL/min;Input mode:Sample size is 1 μ L, pulse Splitless injecting samples, and sample introduction pulse is 25psi, the time is 1min;Injector temperature is 240 DEG C;Transmission line temperature is 260 DEG C;Heating schedule is that initial temperature is 80 DEG C, 240 DEG C are increased to the speed of 5 DEG C/min, keep 18min.Its mass spectral analysis condition is:Ionization mode be EI sources, just from Subpattern;Ion source temperature:230℃;Quadrupole rod temperature:It is 150 DEG C;Collision gas:Nitrogen, flow velocity 1.5mL/min, carrier gas (helium) flow velocity is 2.25mL/min;Multiple-reaction monitoring (MRM) pattern, detail parameters are listed in the table below.
The MRM parameter situations of object
(5) Specification Curve of Increasing and result are calculated
First, with the ratio between object in standard working solution and interior target concentration as abscissa, with object in chromatogram It is ordinate with the ratio between interior target peak area, carries out linear regression analysis, obtains standard working curve.Take the standard of least concentration Working solution, does 9 Parallel testing analyses, calculates its standard deviation, and with the corresponding concentration of 3 times of standard deviation, conversion draws The detection limit of method.The data such as regression equation, coefficient correlation, the detection limit corresponding with standard working curve see the table below.
The working curve and detection limit of analysis method
Object and interior target chromatographic peak area ratio in the sample solution that will be measured under the same terms, substitute into standard work bent Line, the content of object in cigarette sample is tried to achieve according to following equation.
In formula:
W --- 3 kinds of contents of main tongue delicate fragrance characteristic chicken flavor material in ramuscule cigarette mainstream flue gas, unit is nanogram every (ng/ branch);
A --- 3 kinds of peak areas of main tongue delicate fragrance characteristic chicken flavor material;
As --- target peak area in correspondence;
The intercept of b --- standard working curve;
Ms --- target quality in addition, unit is nanogram (ng);
The slope of a --- standard working curve;
The quantity of M --- cigarette, unit is branch.
3 kinds of main tongue delicate fragrance characteristic chicken flavor material testing results see 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 of the invention and recovery of standard addition:
Ramuscule cigarette sample used is analysis object with embodiment 1, withinday precision experiment has been carried out respectively, in a few days Precision Experiment is same sample parallel determination 6 times (same batch processed) under identical conditions, and 6 parallel determinations are calculated respectively The relative standard deviation (RSD) of result, measurement result see the table below.Result shows in table, the in a few days repeatability of this experimental technique RSD<10%, for the quantitative analysis of trace materials, show that method has good precision.
It is analysis object with ramuscule cigarette sample used by replica test, at above-mentioned sample-pretreating method Reason, adds the standard specimen of the suitable content of its burst size, carries out matrix mark-on experiment, as a result see the table below.As can be seen from the table, sample Between 87.39%~113.75%, illustration method has preferable accuracy to the recovery of standard addition of product.
What the standard liquid used in the present embodiment was only illustrated by taking one of concentration as an example, other concentration value institutes The standard liquid of preparation analyzes obtained standard curve and regression equation and above-described embodiment through gas chromatography tandem mass spectrometry instrument It is identical, do not enumerating herein.Illustrated embodiment is intended merely to be better understood from the inventive method, and without any limitation The method of effect, the i.e. above method or equivalent above-mentioned situation is all contained in the protection domain of technical scheme.

Claims (4)

1. in a kind of quantitative analysis ramuscule cigarette mainstream flue gas main tongue delicate fragrance characteristic chicken flavor material method, including following step Suddenly:
(1) preparation of inner mark solution:The use of methyl alcohol is solvent with heptadecane as internal standard compound, prepares inner mark solution;
(2) preparation of standard working solution:With the mark of divaricatic acid ethyl ester, orcin monomethyl ether and β-orcin carboxylate methyl ester Quasi- product are object, the use of methyl alcohol are solvent, and Standard Stock solutions are prepared into through stepwise dilution, are then respectively adding a certain amount of Inner mark solution, is prepared into standard working solution;
(3) preparation of sample solution:The object in cigarette smoke is gathered, inner mark solution and extractant, vibration is added Extract, then to the excessively organic filter membrane of extract, obtain sample solution;
(4) gas chromatography tandem mass spectrometry instrument analysis:
Standard working solution and sample solution are tested and analyzed with gas chromatography tandem mass spectrometry instrument GC-MS/MS;
Described GC-MS/MS is analyzed, and its instrumental conditions is:Using HP-INNOWAX 30m × 0.25mm × 0.25 μm hair Capillary chromatographic column;Carrier gas is helium, and constant current speed is 1.0mL/min;Input mode:Sample size is 1 μ L, and pulse is not diverted into Sample, sample introduction pulse is 25psi, and the time is 1min;Injector temperature is 240 DEG C;Transmission line temperature is 260 DEG C;Intensification journey Sequence is that initial temperature is 80 DEG C, and 240 DEG C are increased to the speed of 5 DEG C/min, keeps 18min;
Described mass spectral analysis condition is:Ionization mode is EI sources, positive ion mode;Ion source temperature:230℃;Quadrupole rod temperature Degree:It is 150 DEG C;Collision gas:Nitrogen, flow velocity 1.5mL/min, carrier gas helium flow velocity is 2.25mL/min;Multiple-reaction monitoring MRM Pattern, detail parameters are listed in the table below:
The MRM parameter situations of object
(5) drafting of standard working curve and the calculating of sample result, described Specification Curve of Increasing and result are calculated as follows:With The ratio between object and interior target concentration are abscissa in standard working solution, with object in chromatogram and interior target peak area it Than being ordinate, linear regression analysis is carried out, obtain standard working curve.Target in the sample solution that will be measured under the same terms Thing and interior target chromatographic peak area ratio, substitute into standard working curve, and containing for object in cigarette sample is tried to achieve according to following equation Amount:
W = ( A A s - b ) &times; M s a &times; M
In formula:
W --- 3 kinds of contents of main tongue delicate fragrance characteristic chicken flavor material in ramuscule cigarette mainstream flue gas, unit is every ng/ of nanogram Branch;
A --- 3 kinds of peak areas of main tongue delicate fragrance characteristic chicken flavor material;
As --- target peak area in correspondence;
The intercept of b --- standard working curve;
Ms --- target quality in addition, unit is nanogram ng;
The slope of a --- standard working curve;
The quantity of M --- cigarette, unit is branch.
2. assay method according to claim 1, it is characterised in that:The preparation of described inner mark solution, specifically include with Lower step:
(1) internal standard storing solution:0.2g heptadecanes are weighed, 0.1mg is accurate to, in the volumetric flask of 100mL, is dissolved with methyl alcohol And it is settled to scale;
(2) inner mark solution:0.1mL internal standard storing solutions accurately are pipetted, in the volumetric flask of 100mL, with methanol dilution and is settled to Scale.
3. assay method according to claim 1, it is characterised in that:The preparation of described standard working solution is specifically included Following steps:
(1) primary standard storing solution:Accurately weigh 0.3g divaricatic acids ethyl ester, 0.1g orcins monomethyl ether and 0.25g β-tongue Black phenol carboxylate methyl ester, is accurate to 0.1mg, in the volumetric flask of 50mL, scale is dissolved and be settled to methyl alcohol;
(2) secondary standard storing solution:0.1mL primary standard storing solutions accurately are pipetted, in the volumetric flask of 50mL, methanol dilution is used And it is settled to scale;
(3) standard working solution:Accurately pipette respectively the μ L of secondary standard storing solution 50,100 μ L, 300 μ L, 600 μ L, 1mL and 2mL, into the volumetric flask of 10mL, then it is accurate respectively add 1mL inner mark solutions, with methanol dilution and be settled to scale, obtain serial Standard working solution.
4. assay method according to claim 1, it is characterised in that:The preparation of described sample solution specifically includes following Step:
(1) cigarette smoking:20 cigarette are aspirated in requirement according to the standards of GB/T 19609, wherein trapping cigarette master with cambridge filter Granule phase substance in stream flue gas;
(2) granule phase substance extraction:The cambridge filter for trapping cigarette mainstream smoke condensate is transferred in 250mL bread bottle, is added 1mL inner mark solutions, are that solvent carries out oscillation extraction with 40mL methyl alcohol, and extraction time is 40min, then uses 0.45 μm of organic phase Filter membrane is filtered, that is, obtain sample solution.
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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
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
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
CN110018248A (en) * 2019-03-22 2019-07-16 河南中烟工业有限责任公司 A kind of cigarette tree moss absolute selection method
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
CN110568106A (en) * 2019-10-17 2019-12-13 云南中烟工业有限责任公司 Quantitative detection method for turpentine substances in turpentine plants or extracts
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
CN111289677A (en) * 2020-03-31 2020-06-16 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
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