CN109187777A - A kind of quick-fried pearl cigarette smoking of aroma is gone with wine category feature fragrance ingredient measuring method - Google Patents
A kind of quick-fried pearl cigarette smoking of aroma is gone with wine category feature fragrance ingredient measuring method Download PDFInfo
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- CN109187777A CN109187777A CN201810928775.3A CN201810928775A CN109187777A CN 109187777 A CN109187777 A CN 109187777A CN 201810928775 A CN201810928775 A CN 201810928775A CN 109187777 A CN109187777 A CN 109187777A
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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
- 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
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7206—Mass spectrometers interfaced to gas chromatograph
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
It goes with wine category feature fragrance ingredient measuring method the invention discloses a kind of quick-fried pearl cigarette smoking of aroma, main flume is trapped, extract, measure flavor component-ethyl acetate, ethyl lactate, ethyl hexanoate and cognac oil in quick-fried pearl class flue gas using GC-MS/MS.A kind of method for being suitable for measuring bouquet components in quick-fried pearl cigarette mainstream flue gas is established, the method for foundation is simple and reliable, can be applied to the detection of bouquet components in quick-fried pearl cigarette mainstream flue gas；This method is simple and convenient to sample analysis, and detection limit is low, high sensitivity, repeatability and the rate of recovery are good, has enlightenment and directive function to the later period production of cigarette.
Description
Technical field
The invention belongs to cigarette making techniques fields, and in particular to a kind of quick-fried pearl cigarette smoking of aroma is gone with wine category feature fragrance
Determination of composition method.
Background technique
" quick-fried pearl cigarette " is exactly that will be wrapped in the capsule with semi-permeable membrane or sealing of liquid flavor and fragrance, embedding by filter stick
Pearl technology is implanted into cigarette filter, causes its rupture by pinching the capsule when use, the liquid flavor and fragrance built in it is made to incorporate filter stick
Fiber, to have the function that increase smoke moisture, improve filter stick retention aroma effect.Meanwhile fragrance component volatilizees in capsule, it can
To realize the function of cigarette flavouring, abundant mouthfeel level.
In the 1960s, American Tobacco company starts to provide quick-fried pearl cigarette to market, there is large development in the world.Closely
The quick-fried pearl cigarette cultivation effect of Nian Lai, China is obvious, is especially pushed away with the quick-fried pearl cigarette of aroma that " state's aroma " is representative
Out, state's implosion pearl cigarette market has been ignited.
During quick-fried pearl cigarette real consumption, there are the feelings that the impression of rear several mouthfuls of characteristic chicken flavors and former mouths have larger difference
Condition.After this illustrates that quick-fried pearl is broken, the release of flavors and fragrances is simultaneously unstable, to directly affect the aesthetic quality of product.Aroma is quick-fried
Pearl is the quick-fried pearl of one kind using white wine characteristic chicken flavor ingredient as core material, can increase cigarette aroma after pinching brokenly.It is general " help wine and enter cigarette "
It reads and introduces after cigarette consumption, concern of the quick-fried pearl of aroma increasingly by consumer and tobacco enterprise, therefore establish the quick-fried pearl of aroma
Cigarette aspirates the measuring method for category feature flavor component of going with wine by mouth to evaluate the quick-fried pearl cigarette front and back suction stability of aroma very
It is necessary.
Drinks characteristic chicken flavor method for measuring components has lot of documents report in wine.Chemical substance in cigarette smoke is
More than 8000 kinds, matrix complexity is far more than common white spirit matrix, using the drinks characteristic chicken flavor of common white spirit at sorting
Survey method cannot be satisfied with the detection of drinks characteristic chicken flavor ingredient in flue gas, therefore propose in the detection flue gas of qualitative, quantitative a kind of
The method of bouquet components substance is particularly significant.
Summary of the invention
It goes with wine category feature fragrance ingredient measuring method the present invention provides a kind of quick-fried pearl cigarette smoking of aroma, this method is benefit
Measured simultaneously with gas chromatography tandem mass spectrometry method the quick-fried pearl cigarette of aroma by mouth aspirate in lower main flume drinks characteristic chicken flavor at
Point, the wine feature perfume (or spice) ingredient in flue gas can be effectively detected.
To achieve the goals above, the technical solution adopted by the present invention is as follows:
A kind of quick-fried pearl cigarette smoking of aroma is gone with wine category feature fragrance ingredient measuring method, comprising the following steps:
1) fragrance ingredient extracts: choosing several cigarettes to be tested, the quick-fried pearl in cigarette of crumbing lights cigarette to be tested, and trap
Cigarette mainstream flue gas total particulate；The cigarette mainstream flue gas total particulate of trapping is dissolved in 25-35mL 1ug/mL D3Enanthic acid
It in the methanol solution of ethyl ester and is extracted, obtains extract liquor；
2) standard working solution configures: preparing has concentration gradient and contains internal standard D3The series standard working solution of cognac oil；
3) GC-MS/MS measure: by step 1) extract liquor and step 2 obtained in standard working solution under the same conditions into
Row GC-MS/MS measurement；
4) result calculates: being quantified by the ratio between target analytes peak area and internal standard peak area using internal standard method.
The choosing method of cigarette is tested in the step 1): cigarette sample being placed in (22 ± 1) DEG C, relative humidity is
48h is balanced in the environment of (60 ± 2) %, then selects its average weight in ± 0.02g range and average resistance to suction in ± 49Pa/ branch model
Cigarette in enclosing is as test cigarette.
The concrete mode of cigarette mainstream flue gas total particulate is trapped in the step 1) are as follows: use rotating disc type smoking machine, use
The cambridge filter of diameter 92mm traps cigarette mainstream smoke total particulate matter；Flatly according to suction in every 60 ± 5 seconds, every mouthful of pumping volume
35 ± 5ml, puff duration 1-3s, cigarette first to be tested exhaust, and pop up filter disc, are packed into next filter disc, carry out the
Two mouthfuls suction, and so on aspirated.
The concrete mode extracted in step 1): 30mL 1ug/ is added in the filter disc for trapping cigarette mainstream flue gas total particulate
mL D3In the methanol solution of cognac oil, ultrasonic extraction 25-35 minutes, extract liquor is obtained.
Series standard working solution is prepared in the step 2, and detailed process is as follows: compound concentration gradient is 0.1,0.2,
The hybrid standard working solution of 0.5,1,2,5 μ g/mL, the internal standard D of the hybrid standard working solution of each concentration3Cognac oil
Concentration be 1 μ g/mL；Concentration gradient is acetic acid second in the hybrid standard working solution of 0.1,0.2,0.5,1,2,5 μ g/mL
Ester, ethyl lactate, ethyl hexanoate and cognac oil concentration be respectively 0.1,0.2,0.5,1,2,5 μ g/mL.
GC conditions in the determination condition of GC-MS/MS in the step 3) are as follows:
280 DEG C of injector temperature；Temperature programming: 50 DEG C of column compartment initial temperature, 1min is kept, with the heating rate liter of 10 DEG C/min
To 130 DEG C, 1min is kept；280 DEG C finally are warming up to 40 DEG C/min, keeps 8min；Split sampling, split ratio 18:1, into
Sample amount 1.0uL.Carrier gas is helium, and pressure is 98kpa, flow velocity 1.58mL/min before column；Total run time is 20min.
Chromatographic column is fused-silica capillary column, specification 30m*0.25mm*0.25um in the step 3).
Mass Spectrometry Conditions in the determination condition of GC-MS/MS in the step 3) are as follows:
Ion source be the source EI, ionization voltage 70eV, 280 DEG C of ion source temperature, 280 DEG C of interface temperature, scanning speed 1111s/
Dec, solvent delay 3min；Scanning mode: multiple-reaction monitoring.
Beneficial effects of the present invention:
The present invention traps main flume with cambridge filter, extraction, measures fragrance in quick-fried pearl class flue gas using GC-MS/MS
Ingredient-ethyl acetate, ethyl lactate, ethyl hexanoate and cognac oil.One kind is established to be suitable for measuring quick-fried pearl cigarette main flue
The method of bouquet components in gas, the method for foundation is simple and reliable, can be applied to bouquet components in quick-fried pearl cigarette mainstream flue gas
Detection；This method is simple and convenient to sample analysis, and detection limit is low, high sensitivity, repeatability and the rate of recovery are good, to the later period of cigarette
Production has certain enlightenment effect.
Detailed description of the invention
Fig. 1 is the MRM figure of ethyl acetate in standard specimen；
Fig. 2 is the MRM figure of ethyl lactate in standard specimen；
Fig. 3 is the MRM figure of ethyl hexanoate in standard specimen；
Fig. 4 is the MRM figure of cognac oil in standard specimen；
Fig. 5 is internal standard D in standard specimen3The MRM of cognac oil schemes；
Fig. 6 is four kinds of characteristic chicken flavor composition analysis results of the quick-fried pearl cigarette sample of certain trade mark aroma.
Specific embodiment
Under embodiment of the present invention will be described in detail in conjunction with the embodiments, but those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Specific item is not specified in embodiment
Part person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer, being can
With the conventional products obtained by commercially available purchase.
Embodiment 1
A kind of quick-fried pearl cigarette smoking of aroma is gone with wine category feature fragrance ingredient measuring method, comprising the following steps:
1) cigarette sample pre-processes: cigarette sample being placed in (22 ± 1) DEG C, is balanced in the environment that relative humidity is (60 ± 2) %
Then 48h selects its average weight to be used as test cigarette in the cigarette of ± 0.02g range and average resistance to suction within the scope of ± 49Pa/ branch
Branch.Using rotating disc type smoking machine, cigarette mainstream smoke total particulate matter is trapped with the cambridge filter of diameter 92mm.Lighting cigarette it
Before, it is crumbed quick-fried pearl with hand, flatly according to suction in every 60 seconds, every mouthful of pumping volume 35ml, puff duration 2s, to 20 cigarettes the
It exhausting flatly, pops up filter disc, be packed into next filter disc, this process control is completed within 10s, second mouthful of suction is carried out, other
Mouthful number and so on aspirated, aspirate six mouthfuls altogether, trap six filter discs.Above-mentioned six filter discs are respectively placed in 250mL taper
It is accurate that 30mL 1ug/mL D is added in bottle3The methanol solution of cognac oil ultrasonic extraction 30 minutes, obtains sample purification liquid；
2) standard working solution configures: preparing has concentration gradient and contains internal standard D3The mixing series standard of cognac oil works
Solution；
Compound concentration gradient is the hybrid standard working solution of 0.1,0.2,0.5,1,2,5 μ g/mL, the hybrid standard of each concentration
The internal standard D of working solution3The concentration of cognac oil is 1 μ g/mL；Concentration gradient is 0.1,0.2,0.5,1,2,5 μ g/mL
In hybrid standard working solution, ethyl acetate, ethyl lactate, ethyl hexanoate and cognac oil concentration be respectively 0.1,0.2,
When 0.5,1,2,5 μ g/mL(such as hybrid standard working solution gradient is 0.5 μ g/mL, 0.5 μ g in hybrid standard working solution
The concentration difference of/mL ethyl acetate, 0.5 μ g/mL ethyl lactate, 0.5 μ g/mL ethyl hexanoate and 0.5 μ g/mL cognac oil
For 0.5 μ g/mL)；
3) GC-MS/MS is measured: GC conditions:
Chromatographic column DB-35(30m*0.25mm*0.25um) fused-silica capillary column, 280 DEG C of injector temperature.Temperature programming:
50 DEG C of column compartment initial temperature (keeps 1min), rises to 130 DEG C (keeping 1min) with the heating rate of 10 DEG C/min；Finally with 40
DEG C/min is warming up to 280 DEG C (keep 8min).Split sampling, split ratio 18:1, sample volume 1.0uL.Carrier gas is helium, before column
Pressure is 98kpa, flow velocity 1.58mL/min.Total run time is 20min.
Mass Spectrometry Conditions:
Ion source be the source EI, ionization voltage 70eV, 280 DEG C of ion source temperature, 280 DEG C of interface temperature, scanning speed 1111s/
Dec, solvent delay 3min.Scanning mode: multiple-reaction monitoring (MRM)；
Fig. 1-5 is 4 kinds of feature perfume (or spice) ethyl acetate, ethyl lactate, ethyl hexanoate and cognac oil and internal standard D3Cognac oil
MRM figure.
4) result calculates: being quantified by the ratio between target analytes peak area and internal standard peak area using internal standard method.
It is quantified by the ratio between target analytes peak area and internal standard peak area using internal standard method；It is specific as follows: to contain
The ratio between target analytes peak area and internal standard peak area are ordinate, target analysis in interior target mixed stocker column standard working solution
The concentration of object is abscissa, draws working curve, obtains the standard curve regression equation and related coefficient of object；According to sample
The ratio between target analytes peak area and internal standard peak area in scavenging solution substitute into working curve, obtain the content of sample purification liquid.
Drinks characteristic chicken flavor ingredient burst size is calculated by following formula in main flume under aspirating by mouth:
In formula: m ----every cigarette aspirates drinks characteristic chicken flavor ingredient burst size in lower main flume by mouth, and unit is nanogram
Every (ng/cig).
A --- the concentration of heterocyclic amine compound in-sample purification liquid, unit are nanograms per milliliter (μ g/mL).
10 measurements are carried out with the serial standard working solution of minimum concentration mixing containging interior traget, 4 kinds of features are calculated
The standard deviation of flavor component (ethyl acetate, ethyl lactate, ethyl hexanoate and cognac oil), using three times standard deviation as inspection
Rising limit, the results are shown in Table 1.
As shown in Table 2, related coefficient >=0.9992 of four kinds of analytes, method good linearity, and detection method are measured
Detection limit is low.
In order to investigate the reproducibility of the present embodiment the method, the mark of 4 kinds of characteristic chicken flavor ingredients is added into cambridge filter
Quasi- solution, prepare high (3 μ g/mL), in (1 μ g/mL), low (0.2 μ g/mL) three horizontal mark-on samples, then with the present invention
Measuring method analyzes it, deducts the content of 4 kinds of characteristic chicken flavor ingredients of blank test in sample, calculates its measured quantity, and by adding
Scalar sum measured quantity calculates the rate of recovery, and each concentration level does three in parallel, the results are shown in Table 2.
The result shows that three horizontal rate of recovery illustrate the rate of recovery of embodiment the method between 88.3-106%
Height, favorable reproducibility.
Above-mentioned low concentration mark-on sample (0.2 μ g/mL) in a few days and in the daytime put down for 6 times according to measuring method of the present invention
Row measurement, the results are shown in Table 3.
The result shows that each compound determination in a few days and in the daytime relative standard deviation illustrates the party between 0.8-4.1%
The reproducibility and stability of method are fine.
Releasing for lower four kinds of characteristic chicken flavors can be aspirated by mouth using the detection quick-fried pearl cigarette of aroma of detection method described in the present embodiment
High-volume, by instructing production of cigarettes to the analysis by mouth burst size of each characteristic chicken flavor.Fig. 6 is using described in the present embodiment
The quick-fried pearl cigarette sample of certain trade mark aroma is by the lower four kinds of characteristic chicken flavor composition analysis results of mouth suction in the market for method detection, from Fig. 6
In as can be seen that the trade mark characteristic chicken flavor ingredient by mouth discharge it is more consistent.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (8)
- The category feature fragrance ingredient measuring method 1. a kind of quick-fried pearl cigarette smoking of aroma is gone with wine, which is characterized in that method, which is directed to, to be contained The quick-fried pearl cigarette application of aroma, comprising the following steps:1) fragrance ingredient extracts: choosing several cigarettes to be tested, the quick-fried pearl in cigarette of crumbing lights cigarette to be tested, and trap Cigarette mainstream flue gas total particulate；The cigarette mainstream flue gas total particulate of trapping is dissolved in 25-35mL 1ug/mL D3Enanthic acid It in the methanol solution of ethyl ester and is extracted, obtains extract liquor；2) standard working solution configures: preparing has concentration gradient and contains internal standard D3The series standard working solution of cognac oil；3) GC-MS/MS measure: by step 1) extract liquor and step 2 obtained in standard working solution under the same conditions into Row GC-MS/MS measurement；4) result calculates: being quantified by the ratio between target analytes peak area and internal standard peak area using internal standard method.
- The category feature fragrance ingredient measuring method 2. the quick-fried pearl cigarette smoking of aroma as described in claim 1 is gone with wine, which is characterized in that institute It states test cigarette in step 1) to be pre-processed before suction, preprocess method are as follows: cigarette sample is placed in (22 ± 1) DEG C, 48h is balanced in the environment that relative humidity is (60 ± 2) %.
- The category feature fragrance ingredient measuring method 3. the quick-fried pearl cigarette smoking of aroma as described in claim 1 is gone with wine, which is characterized in that institute State the concrete mode that cigarette mainstream flue gas total particulate is trapped in step 1) are as follows: rotating disc type smoking machine is used, with diameter 92mm's Cambridge filter traps cigarette mainstream smoke total particulate matter.
- The category feature fragrance ingredient measuring method 4. the quick-fried pearl cigarette smoking of aroma as claimed in claim 3 is gone with wine, which is characterized in that step Rapid 1) the middle concrete mode extracted: 30mL 1ug/mL D is added in the filter disc that will trap cigarette mainstream flue gas total particulate3Enanthic acid In the methanol solution of ethyl ester, ultrasonic extraction 25-35 minutes, extract liquor is obtained.
- The category feature fragrance ingredient measuring method 5. the quick-fried pearl cigarette smoking of aroma as described in claim 1 is gone with wine, which is characterized in that institute State and prepare series standard working solution in step 2 detailed process is as follows: compound concentration gradient is 0.1,0.2,0.5,1,2,5 μ The hybrid standard working solution of g/mL, the internal standard D of the hybrid standard working solution of each concentration3The concentration of cognac oil is 1 μg/mL；Concentration gradient is in the hybrid standard working solution of 0.1,0.2,0.5,1,2,5 μ g/mL, ethyl acetate, ethyl lactate, The concentration of ethyl hexanoate and cognac oil is 0.1,0.2,0.5,1,2,5 μ g/mL respectively.
- The category feature fragrance ingredient measuring method 6. the quick-fried pearl cigarette smoking of aroma as described in claim 1 is gone with wine, which is characterized in that institute State in step 3) GC conditions in the determination condition of GC-MS/MS are as follows:280 DEG C of injector temperature；Temperature programming: 50 DEG C of column compartment initial temperature, 1min is kept, with the heating rate liter of 10 DEG C/min To 130 DEG C, 1min is kept；280 DEG C finally are warming up to 40 DEG C/min, keeps 8min；Split sampling, split ratio 18:1, into Sample amount 1.0uL；Carrier gas is helium, and pressure is 98kpa, flow velocity 1.58mL/min before column；Total run time is 20min.
- The category feature fragrance ingredient measuring method 7. the quick-fried pearl cigarette smoking of aroma as claimed in claim 6 is gone with wine, which is characterized in that institute Stating chromatographic column in step 3) is fused-silica capillary column, specification 30m*0.25mm*0.25um.
- The category feature fragrance ingredient measuring method 8. the quick-fried pearl cigarette smoking of aroma as described in claim 1 is gone with wine, which is characterized in that institute State in step 3) Mass Spectrometry Conditions in the determination condition of GC-MS/MS are as follows:Ion source be the source EI, ionization voltage 70eV, 280 DEG C of ion source temperature, 280 DEG C of interface temperature, scanning speed 1111s/ Dec, solvent delay 3min；Scanning mode: multiple-reaction monitoring.
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| CN110540899A (en) * | 2019-09-18 | 2019-12-06 | 成都中医药大学 | Zanthoxylum bungeanum flavor essence for cigarette bead blasting and application of zanthoxylum bungeanum flavor essence in cigarettes |
| CN114740126A (en) * | 2022-05-14 | 2022-07-12 | 河南中烟工业有限责任公司 | Method for determining quality of cigarette product containing bead blasting heating by using HPLC-IR-MS |
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| CN114740126B (en) * | 2022-05-14 | 2024-02-20 | 河南中烟工业有限责任公司 | Method for determining quality of explosive-containing bead heating cigarette product by utilizing HPLC-IR-MS |
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