CN106706773B - A kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method - Google Patents
A kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method Download PDFInfo
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- CN106706773B CN106706773B CN201610989728.0A CN201610989728A CN106706773B CN 106706773 B CN106706773 B CN 106706773B CN 201610989728 A CN201610989728 A CN 201610989728A CN 106706773 B CN106706773 B CN 106706773B
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- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 21
- 241000208125 Nicotiana Species 0.000 title claims abstract description 13
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 13
- 235000013773 glyceryl triacetate Nutrition 0.000 title claims abstract description 12
- 229960002622 triacetin Drugs 0.000 title claims abstract description 11
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 57
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 238000000199 molecular distillation Methods 0.000 claims abstract description 10
- 239000000470 constituent Substances 0.000 claims abstract description 6
- 238000004458 analytical method Methods 0.000 claims abstract description 4
- 239000002387 analytical standard solution Substances 0.000 claims abstract description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 51
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 42
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 35
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 20
- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 13
- 238000004587 chromatography analysis Methods 0.000 claims description 11
- 239000012086 standard solution Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000013558 reference substance Substances 0.000 claims description 6
- 239000011550 stock solution Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 230000004907 flux Effects 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000004364 calculation method Methods 0.000 claims description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 241001191009 Gymnomyza Species 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 235000019504 cigarettes Nutrition 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 8
- 230000001953 sensory effect Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 14
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 238000010812 external standard method Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 4
- 229940011051 isopropyl acetate Drugs 0.000 description 4
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 229940076134 benzene Drugs 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000000834 fixative Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 foundry industry Substances 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- G01N30/08—Preparation using an enricher
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 glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method.This method uses gas chromatograph-mass spectrometer (GC-MS) analytical standard solution first, draw the standard curve of tested component, then ether is added in triacetyl glycerine or methanol is that solvent carries out molecular distillation collection light component, and the light component of collection is entered into the data that gas chromatograph-mass spectrometer (GC-MS) analysis obtains various tested components in sample to be tested, then the content of the various tested components in sample to be tested is calculated by the standard curve drawn, the content need to obtain various tested constituent contents in former triacetyl glycerine sample divided by corresponding enrichment times.The present invention can be used for detecting the various volatile substances in triacetyl glycerine, it is possible to provide may influence the quantitative information of the volatile chemical component of cigarette sensory quality in triacetyl glycerine sample, have preferable practical value.
Description
Technical field
It is specific a kind of using to three triacetins the present invention relates to the detection of the volatile component of glycerol triacetate for tobacco
Volatile materials carries out separation and concentration in ester, and three acetic acid of cigarette of quantitative analysis are carried out in direct injected gas chromatograph-mass spectrometer
Glyceride volatile component GC-MS quantitative detecting method.
Background technique
Triacetyl glycerine is a kind of colorless and odorless oily liquids, can be miscible with ethyl alcohol, ether, chloroform and benzene, is slightly soluble in
Water and carbon disulfide.Because of its nontoxic, nonirritant feature, triacetyl glycerine makees perfume fixative, solvent, increasing by application
Tough dose, and the industries such as cosmetics, foundry industry, medicine, dyestuff and manufacturing industry can be widely used in.Purposes in cigarette is also very
Extensively, such as the solvent and fixative of box piece, tipping paper printing ink, cigarette filter binder, etc..Usual triacetyl glycerine
To there is glycerol and acid esterification to be prepared, therefore, impurity have ethyl alcohol, formaldehyde, acetic acid and acid anhydrides, acetone, benzene, toluene and
A variety of acetoglycerides etc..
Cigarette auxiliary materials are numerous using raw material type and specification, it is desirable that also diversified.The raw material of same title may be due to life
Production method is different, production technology is different, main component is different, producer's packing storage is different etc., causes impurity different, there are differences
The hidden danger of degree.Tobacco business is mostly used national standard YC 263-2014 and YC 171-2014 etc. whether to detect in material VOC content
It complies with standard.But this detects the investigation for being more focused on security risk, does not have considered critical to odoring substance and sense organ hidden danger, from
And the risk hidden danger that auxiliary material brings negative effect to cigarette product suction organoleptic quality can not be eliminated.Also, triacetyl glycerine
Viscosity is higher, and boiling point is higher, there are also some non-volatile polymeric impurities, unsuitable direct injected gaseous mass spectrum-chromatography (GC-MS) point
Analysis, can pollute instrument component, and existing method needs to be combined with head space instrument.Head space experiment it is higher to instrument requirements, signal response compared with
Weak, detection limit is higher, and part volatile materials is not easy accurately to be detected.
Summary of the invention
It is sweet with three acetic acid it is an object of the invention to provide a kind of cigarette for triacetyl glycerine used in cigarette auxiliary materials
Grease volatile component GC-MS quantitative detecting method, this method emphasis to the related volatile impurity component of organoleptic quality, and
Enrichment is collected, and the detection limit of target detection thing is improved, and promotes the accuracy of subsequent detection, is realized directly using head space series connection GC-
MS instrument and gas phase flame ionization ditector (GC-FID) do not measure, indeterminable target analyte detection works；It can be direct
Sample introduction GC-MS chromatography, is analyzed by quantified by external standard method, instrument component will not be caused to pollute.
Technical solution provided by the invention: a kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method,
Specific step is as follows:
(1) precise M1M is added in the triacetyl glycerine sample of g2The ether or methanol of g is that solvent carries out molecular distillation
Light component is collected, the vacuum degree of molecular distillation is 3~10MPa, and 50~70 DEG C of temperature, 1~5mL/min of sample rate, knifing turns
Fast 100-400r/min；Sample quality M1With solvent quality M2Meet following relationship: 5M2<M1<100M2；
(2) gas chromatograph-mass spectrometer (GC-MS) analytical standard solution is used, the standard curve of tested component, the standard are drawn
One coordinate of curve is the reference substance concentration of tested component, another coordinate is that the reference substance of tested component corresponds to the peak face at peak
Product；
(3) light component collected in step (1) is entered gas chromatograph-mass spectrometer (GC-MS) analysis to obtain in sample to be tested respectively
The data of kind tested component, and calculate by the standard curve in step (2) containing for various tested components in sample to be tested
Measure W2, which need to be divided by corresponding enrichment times M1/M2, obtain various tested constituent content W in former triacetyl glycerine sample1,
Its various tested constituent content calculation formula is as follows: W2=W1*M1/M2；
The chromatographic column of the gas chromatograph-mass spectrometer (GC-MS) uses specification for 60m × 0.32mm × 1.8um chromatographic column HP-
VOC capillary column, carrier gas: helium, purity 99.999%, 1~2mL/min of carrier gas flux；The gas chromatograph-mass spectrometer (GC-MS)
250 DEG C of injector temperature, sample volume 2~4 μ L, split ratio 2:1~5:1, shunt gas enters Mass Spectrometer Method；The gas phase color
Spectrum-mass spectrometer column oven temperature program: first keeping 2~3min under 40 DEG C of initial temperature, then presses 3~5 DEG C/min liter
Temperature is warming up to 200 DEG C of 5~10min of holding to 180 DEG C of holdings 1~4min, 6~10 DEG C/min.
The present invention preferably technical solution: the Mass Spectrometry Conditions of the gas chromatograph-mass spectrometer (GC-MS) are transmission line temperature 250
℃；230 DEG C of ion source temperature；1~3min of solvent delay.
The further technical solution of the present invention: it is tested group in the step (2) and is divided into volatile impurity composition, specifically includes third
Ketone, acetic acid, ethyl alcohol, isopropanol, ethyl acetate, n-propyl acetate, isopropyl acetate, benzene, toluene, ethylbenzene, one in dimethylbenzene
Kind is any several；Chromatographic solvent is absolute ether or methanol.
The present invention preferably technical solution: the valid analysing range of step (2) the standard curve solution is as follows: institute
Stating acetone, acetic acid, ethyl alcohol, isopropanol, ethyl acetate, n-propyl acetate, isopropyl acetate is 5~160mg/L；The first
Benzene, ethylbenzene, dimethylbenzene are 0.5~16mg/L；The benzene is 0.2~6.4mg/L.
The present invention preferably technical solution: the preparation of standard solution described in the step (2) is divided into six grades, distinguishes first
Weigh acetone, acetic acid, ethyl alcohol, isopropanol, ethyl acetate, n-propyl acetate, the isopropyl acetate of 0.2~0.8g, 30~60mg
Toluene, ethylbenzene, dimethylbenzene, the benzene of 10~20mg obtains stock solution to 25ml using chromatography absolute ether or methanol constant volume；
Each stock solution 1mL is taken respectively, for chromatography absolute ether or methanol constant volume to 100ml, obtains first order standard solution；Take each one
Grade standard solution 5mL becomes secondary standard solution using chromatography absolute ether or methanol constant volume to 10mL；It is diluted according to above 2 times
Mode, prepare three to six grade standard solution respectively.
This hair utilizes molecular distillation apparatus, Selective Separation volatile impurity component (including acetone, acetic acid, ethyl alcohol, isopropyl
Alcohol, ethyl acetate, n-propyl acetate, isopropyl acetate, benzene, toluene, ethylbenzene, dimethylbenzene, etc.), more difficult volatilization impurity composition
(including triacetyl glycerine) and difficult volatilization impurity composition；Emphasis is and rich to the related volatile impurity component of organoleptic quality
Collection is collected, and is improved the detection limit of target detection thing, is promoted the accuracy of subsequent detection.For directly using head space series connection GC-MS
Instrument and gas phase flame ionization ditector (GC-FID) do not measure, indeterminable object, and this method can be completed to detect
Work；Can direct injected GC-MS chromatography, analyzed by quantified by external standard method, instrument component will not be caused to pollute；If necessary to use
High-purity triacetyl glycerine carries out other detections, the high boiling component after molecular distillation can also be carried out molecule steaming again
It evaporates, is only set as 90~120 DEG C with by temperature, distillating component is triacetyl glycerine.
Beneficial effects of the present invention:
(1) volatile component of triacetyl glycerine sample is separated by molecular distillation, and reaches the effect of enrichment
Fruit improves the concentration of volatile materials, can relatively detect the component that some conventional methods can not be detected accurately, reduces detection and misses
Difference；
(2) method in the present invention eliminates volatile-resistant substance interference, can direct injected GC-MS qualitative analysis, and to liter
Warm program and chromatographic column require to reduce, and detection process is quick and convenient；
(3) GC-MS quantitative analysis is carried out to specific components with external standard method, it can be one or more to be measured groups of unrestricted choice
Point, content results are accurate, high sensitivity.
The present invention can be used for detecting the various volatile substances in triacetyl glycerine, it is possible to provide triacetyl glycerine
The quantitative information of the volatile chemical component of cigarette sensory quality may be influenced in sample, and there is preferable practical value.
Specific embodiment
In order to further appreciate that the present invention, the preferred embodiment of the invention is described below with reference to embodiment.
The present invention is that a small amount of volatile solvent is added, by molecular distillation separation of volatile components and higher component；
Solvent usage is smaller, plays the effect to target analytes separation and concentration；External standard method direct injected GC-MS detects volatile component
Content.Should meet can be with the chromatographic basic demand of direct injected GC-MS for solvent in the present invention；Solvent is not deposit in sample to be tested
Low-boiling point material；Solvent and tested component intermiscibility are preferable, but polarity difference cannot be too close so that solvent chromatographic peak with
Tested component chromatographic peak can be kept completely separate；Solvent cannot be chemically reacted with component to be measured.Therefore solvent be preferably ether or
Methanol.
The preferred embodiment of the present invention is as follows:
(1) sample pre-treatments: accurately weighing triacetyl glycerine sample 1~4, is placed in molecular distillation apparatus sample room, and
It accurately weighs Chromatographic Pure Methanol and uses oil pump to be pumped to vacuum degree as 4mPa, temperature is set for collecting volatile component for solvent
It is set to 60 DEG C, sample rate 2mL/min, knifing rotating speed 180r/min；Triacetyl glycerine sample and Chromatographic Pure Methanol quality are such as
Shown in table 1；
Table 1 weighs sample and solvent quality and mass ratio
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | |
| Triacetyl glycerine M1(g) | 10.016 | 19.945 | 20.428 | 10.220 |
| Methanol M2(g) | 1.988 | 2.076 | 1.061 | 1.045 |
| M1/M2 | 5.038 | 9.607 | 19.254 | 9.780 |
(2) gas chromatograph-mass spectrometer (GC-MS) (GC-MS) chromatographic separation condition: chromatographic column HP-VOC capillary column (60m is used
×0.32mm×1.8um)；250 DEG C of injector temperature；Column oven temperature program: 2min is first kept under 40 DEG C of initial temperature, then
180 DEG C of holdings 2min, 10 DEG C/min, which are warming up to, by 4 DEG C/min is warming up to 200 DEG C of holding 6min；Carrier gas: helium, purity
99.999%；Carrier gas flux 2mL/min, split ratio 2:1；Shunt gas enters Mass Spectrometer Method；Mass Spectrometry Conditions are transmission line temperature
250℃；230 DEG C of ion source temperature；Solvent delay 2min；
(3) it is tested the configuration of volatile component standard liquid: weighing standard substance ethyl alcohol 0.405g, isopropanol 0.398g, third respectively
Ketone 0.415g, acetic acid 0.408g, n-propyl acetate 0.416g, benzene 0.017g, toluene 0.044g, dimethylbenzene 0.038g are set respectively
In 25mL volumetric flask, Chromatographic Pure Methanol is dissolved to 25ml, as stock solution；The stock solution 1mL of each volatile component is taken, respectively
It is placed in 100mL volumetric flask, chromatography absolute ether or methanol constant volume obtain first order titer to 100ml；Take each primary standard
Liquid 5mL becomes secondary standard liquid to 10mL with chromatography absolute ether or methanol constant volume respectively；Diluted according to above 2 times respectively
Mode prepares three to six grade standard liquid；
(4) it draws standard curve: six grade standard liquid is used into the gas chromatograph-mass spectrometer (GC-MS) (GC- in step (2) respectively
MS it) is analyzed, obtains each tested component respective standard curve, linear fit equation form is Y=aX+b.The standard curve
A coordinate be tested component reference substance concentration, another coordinate be to be tested the reference substance of component to correspond to the face Ji Feng at peak
Product；By one to six grade of standard liquid sample introduction GC-MS of each object, draws calibration curve equation formula and be listed in table 2.Wherein: described third
Ketone, acetic acid, ethyl alcohol, isopropanol, n-propyl acetate are in the about concentration range of 5~160mg/L, and linear good, R is above
0.999；The toluene is 0.55~17.60mg/L in concentration range, and mark is curvilinear good, and R is higher than 0.999；The dimethylbenzene
It is in 0.48~15.20mg/L in concentration range, mark is curvilinear good, and R is higher than 0.999；The benzene concentration range 0.21~
Mark in 6.80mg/L is curvilinear good, and R is above 0.999.
The calibration curve equation formula that each tested component GC-MS of table 2 is analyzed
| Object | Standard curve | Relative deviation R |
| Ethyl alcohol | Y=0.489X-1.066 | 0.99994 |
| Isopropanol | Y=1.343X-0.590 | 0.99990 |
| Acetone | Y=0.973X-0.146 | 0.99989 |
| Acetic acid | Y=1.306X-0.571 | 0.99986 |
| Benzene | Y=0.406X-0.004 | 0.99991 |
| N-propyl acetate | Y=1.065X-1.840 | 0.99996 |
| Toluene | Y=0.131X-0.007 | 0.99998 |
| Dimethylbenzene | Y=0.820X-0.068 | 0.99992 |
Remarks: X is the peak area that object corresponds to peak；Y is target concentration (mg/L)
(5) triacetyl glycerine volatile component content measures: the methanol solution after 1~4 separation and concentration of sample is direct
GC-MS detection is carried out in sampling step (2) in gas chromatograph-mass spectrometer (GC-MS), obtains acetone, acetic acid, ethyl alcohol, isopropanol, second
The peak area of sour n-propyl, benzene,toluene,xylene will respectively mark Qu Fangcheng in peak area substitution table 2 respectively, can get volatility
Constituent content.Quantified by external standard method analyzes result divided by corresponding enrichment times (M1/M2) obtain volatilizing in triacetyl glycerine sample
Property content of material, by calculate after obtain each volatile component in sample 1~4 content it is as shown in table 3.
Each volatile component content of table 3
It there may be the substance of influence include acetone, isopropanol, acetic acid, benzene,toluene,xylene etc. on cigarette product.By
The above results can be seen that the aspect of triacetyl glycerine sample volatile impurity provided by four producers, and there are larger differences.
Wherein, the isopropanol of sample 4, acetone, benzene, toluene level are higher, volatile impurities content highest；Acetone, the diformazan of sample 2
Benzene is higher；In contrast, sample 1 is ideal, is product first choice.
Therefore, the content of each volatile component in glycerol triacetate for tobacco is detected using detection method provided by the invention,
As a result relatively accurate, and the nuance of each producer's triacetyl glycerine volatile impurity can be distinguished, tobacco enterprise inside is selected
It selects triacetyl glycerine and theoretical foundation is provided.
Claims (5)
1. a kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method, the specific steps are as follows:
(1) precise M1M is added in the triacetyl glycerine sample of g2The ether or methanol of g is that solvent carries out molecular distillation collection
Light component, the charging rate 2mL/min of molecular distillation, vacuum degree 4MPa, temperature 60 C, scraper plate revolving speed 180rpm/min；Sample
Quality M1With solvent quality M2Meet following relationship: 5M2<M1<100M2；
(2) gas chromatograph-mass spectrometer (GC-MS) analytical standard solution is used, the standard curve of tested component, the standard curve are drawn
A coordinate be tested component reference substance concentration, another coordinate be to be tested the reference substance of component to correspond to the peak area at peak；
(3) light component collected in step (1) is entered into gas chromatograph-mass spectrometer (GC-MS) analysis and obtains various quilts in sample to be tested
The data of component are surveyed, and calculate by the standard curve in step (2) the content W of the various tested components in sample to be tested2,
The content need to be divided by corresponding enrichment times M1/M2, obtain various tested constituent content W in former triacetyl glycerine sample1, each
The tested constituent content calculation formula of kind is as follows: W2=W1*M1/M2；
The chromatographic column of the gas chromatograph-mass spectrometer (GC-MS) uses specification for 60m × 0.32mm × HP-VOC maos of 1.8um chromatographic column
Buttress shaft, carrier gas: helium, purity 99.999%, 1~2mL/min of carrier gas flux；The sample introduction of the gas chromatograph-mass spectrometer (GC-MS)
Mouthfuls 250 DEG C of temperature, sample volume 2~4 μ L, split ratio 2:1~5:1, shunt gas enters Mass Spectrometer Method；Gas-chromatography-the matter
It composes the column oven temperature program of combined instrument: first keeping 2~3min under 40 DEG C of initial temperature, be then warming up to by 3~5 DEG C/min
180 DEG C of holdings 1~4min, 6~10 DEG C/min are warming up to 200 DEG C of 5~10min of holding.
2. a kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method according to claim 1, special
Sign is: the Mass Spectrometry Conditions of the gas chromatograph-mass spectrometer (GC-MS) are 250 DEG C of transmission line temperature；230 DEG C of ion source temperature；It is molten
Agent postpones 1~3min.
3. a kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method according to claim 1, special
Sign is: being tested group in the step (2) and is divided into volatile impurity composition, specifically includes acetone, acetic acid, ethyl alcohol, isopropanol, second
One of sour n-propyl, benzene,toluene,xylene are any several；Chromatographic solvent is absolute ether or methanol.
4. a kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method according to claim 3, special
Sign is that the valid analysing range of the step (2) standard curve solution is as follows: the acetone, acetic acid, ethyl alcohol, isopropyl
Alcohol, n-propyl acetate are 5~160mg/L；The toluene, dimethylbenzene are 0.5~16mg/L；The benzene be 0.2~
6.4mg/L。
5. a kind of glycerol triacetate for tobacco volatile component GC-MS quantitative detecting method according to claim 3, special
Sign is that the preparation of standard solution described in the step (2) is divided into six grades, weighs acetone, the second of 0.2~0.8g respectively first
Acid, ethyl alcohol, isopropanol, n-propyl acetate, toluene, the dimethylbenzene of 30~60mg, the benzene of 10~20mg use chromatography absolute ether
Or methanol constant volume obtains stock solution to 25ml；Each stock solution 1mL is taken respectively, is used for chromatography absolute ether or methanol constant volume extremely
100ml obtains first order standard solution；Each primary standard solution 5mL is taken, extremely using chromatography absolute ether or methanol constant volume
10mL becomes secondary standard solution；According to above 2 times of diluted modes, three to six grade standard solution are prepared respectively.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006180869A (en) * | 2004-11-30 | 2006-07-13 | Q P Corp | Retort rice gruel and method for producing the same |
| CN101666785A (en) * | 2009-09-09 | 2010-03-10 | 广东中烟工业有限责任公司 | Method for quantitatively detecting components in glycerol triacetate for tobacco |
| CN101701949A (en) * | 2009-11-05 | 2010-05-05 | 中国烟草总公司郑州烟草研究院 | Measurement method of volatile organic compound in tobacco lining paper |
| CN104165958A (en) * | 2014-08-20 | 2014-11-26 | 云南中烟工业有限责任公司 | Method for measuring content of benzene and benzene series in glycerol triacetate |
| CN104330490A (en) * | 2014-10-29 | 2015-02-04 | 广东中烟工业有限责任公司 | External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130337477A1 (en) * | 2012-06-14 | 2013-12-19 | ChemiSensor LLP | Distributable Chemical Sampling and Sensing System Process |
-
2016
- 2016-11-10 CN CN201610989728.0A patent/CN106706773B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006180869A (en) * | 2004-11-30 | 2006-07-13 | Q P Corp | Retort rice gruel and method for producing the same |
| CN101666785A (en) * | 2009-09-09 | 2010-03-10 | 广东中烟工业有限责任公司 | Method for quantitatively detecting components in glycerol triacetate for tobacco |
| CN101701949A (en) * | 2009-11-05 | 2010-05-05 | 中国烟草总公司郑州烟草研究院 | Measurement method of volatile organic compound in tobacco lining paper |
| CN104165958A (en) * | 2014-08-20 | 2014-11-26 | 云南中烟工业有限责任公司 | Method for measuring content of benzene and benzene series in glycerol triacetate |
| CN104330490A (en) * | 2014-10-29 | 2015-02-04 | 广东中烟工业有限责任公司 | External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry |
Non-Patent Citations (3)
| Title |
|---|
| 全二维气相色谱-飞行时间质谱法分析广藿香浸膏中挥发性有机物;邹西梅等;《理化检验-化学分册》;20151231;第51卷(第3期);312-316 |
| 分子蒸馏/气相色谱-质谱法分析火麻仁精油挥发性组分;李文峰等;《中国粮油学报》;20120831;第27卷(第8期);113-118 |
| 烟用三醋酸甘油酯的质量评价方法;孔浩辉等;《现代食品科技》;20101231;第26卷(第12期);1403-1408 |
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