CN110068627A - A kind of method of derivative-pyrolysis-high resolution gas chromatography-mass spectrometry identification cashew nut paint - Google Patents
A kind of method of derivative-pyrolysis-high resolution gas chromatography-mass spectrometry identification cashew nut paint Download PDFInfo
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- CN110068627A CN110068627A CN201910405305.3A CN201910405305A CN110068627A CN 110068627 A CN110068627 A CN 110068627A CN 201910405305 A CN201910405305 A CN 201910405305A CN 110068627 A CN110068627 A CN 110068627A
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- 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
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Abstract
The invention discloses a kind of derivative-pyrolysis-high resolution gas chromatography-mass spectrometry identification cashew nut paint methods, and step includes: to be packed into heat cracker to carry out heating cracking after mixing cashew nut lacquer coat sample with methylating reagent, obtain pyrolysis product；Obtained pyrolysis product is imported into sample introduction in gas chromatograph-mass spectrometer (GC-MS), records GC-MS spectrogram；Gained spectrogram is analyzed, cashew nut paint can be analyzed and identified using comprising detection mass number for one or several characteristic peaks in 122,290,312,314,316,318 and 344.The invention belongs to be used to identify cashew nut lacquer coat for derivative-pyrolysis-high resolution gas chromatography-mass spectrography for the first time.The principle of the present invention is to form more stable ether structure after the phenolic hydroxyl group methylation in cashew nut paint is derived using methylating reagent, thus solves spectrogram tailing problem and simplifies GC/MS spectrogram.The method of identification cashew nut lacquer coat provided by the present invention also has many advantages, such as that accuracy is high, reproducible and simple and quick.
Description
Technical field
The present invention relates to cashew nut paints to identify field, and in particular to a kind of derivative-pyrolysis-high resolution gas chromatography-mass spectrometry identification
The method of cashew nut paint.
Background technique
Cashew nut paint, also known as synthetic oriental lacquer are using cashew nut shell liquid (cashew nut shell liquid or cashew
Nut shell oil) it is paint made of primary raw material.Cashew nut paint has the characteristics that stability is good and easy for construction, can be applied to bamboo
The surface of the wooden articles and noble furniture etc..Therefore, to the identification of cashew nut lacquer coat in trade disputes, judicial expertise and criminal investigation
Aspect has great importance.
Currently, pyrolysis-high resolution gas chromatography-mass spectrography common are to the identification method of cashew nut lacquer coat, and such as: there is document
(Niimura Noriyasu,Miyakoshi Tetsuo,Structural Characterization of a Modified
Cashew Nut Shell Oil Coating Film for Industrial Use[J],International Journal
Of Polymer Analysis and Characterization, 2005 (10), 141-151) use pyrolysis-high resolution gas chromatography-
Mass spectrography analyzes and researches to cashew nut lacquer coat, and analyzes its characteristic peak；However, the film forming matter of cashew nut lacquer coat
Matter molecule contains phenolic hydroxyl structure, easily decomposes, can trail on GC/MS spectrogram when being detected using GC/MS, fragment peak
More, gained spectrogram is difficult to use in identification and analysis.Therefore, a kind of analysis method right and wrong of more accurate identification cashew nut lacquer coat are developed
Often it is necessary to.
Summary of the invention
In view of the deficiencies of the prior art,
Solution of the invention is:
A kind of method of derivative-pyrolysis-high resolution gas chromatography-mass spectrometry identification cashew nut paint, the specific steps are as follows:
1) it is packed into heat cracker after mixing cashew nut lacquer coat sample with methylating reagent and carries out heating cracking, split
Solve product；
2) pyrolysis product obtained in step 1) is imported into sample introduction in gas chromatograph-mass spectrometer (GC-MS) (GC/MS) through interface,
Record GC-MS spectrogram；
Chromatographic condition is as follows: chromatographic column uses capillary gas chromatographic column；Using helium as carrier gas；Using shunting or not
Split sampling；Using temperature programming；
Mass spectrometry parameters are as follows: using level four bars mass detector；Using EI ion source；
3) GC-MS spectrogram is analyzed, is 122,290,312,314,316,318 and using comprising detection mass number
One or more characteristic peaks in 344 analyze and identify cashew nut paint；Or store the GC-MS spectrogram recorded and scanning
Standard spectrogram control, is identified according to spectrogram similarity degree.
Preferably, methylating reagent described in step 1) be selected from tetramethylammonium hydroxide (TMAH), dimethyl suflfate or
One of iodomethane.
Preferably, cracking condition described in step 1) are as follows: pyrolysis time 1s-3min, 300-750 DEG C of cracking temperature.
Preferably, the capillary gas chromatographic column is low-pole column.
Preferably, the carrier gas is constant current mode, and flow velocity is 0.6~2.0mL/min.
Preferably, the temperature program are as follows: 40 DEG C of initial temperature, keep 5min；320 DEG C are risen to 20 DEG C/min, is kept
10min。
Preferably, the split ratio of the split sampling is 5:1~50:1.
Preferably, the temperature of the level four bars is set as 150 DEG C.
Preferably, the energy of the EI ion source is 70ev, and ion source temperature is 250 DEG C.
The principle of the present invention is as follows:
Chromatograph-mass spectrometer coupling method is the powerful measure of identification, and the film forming matter molecule of cashew nut lacquer coat contains phenol hydroxyl
Based structures, easily decompose, detected using GC/MS when can trail on GC/MS spectrogram, fragment peak is more, and spectrogram is difficult to use
In identification and analysis.Therefore, methylating reagent can be used, such as: tetramethylammonium hydroxide (TMAH), dimethyl suflfate or iodomethane
More stable ether structure is generated after phenolic hydroxyl group methylation in cashew nut paint is derived, thus solves spectrogram tailing problem, and make GC/
MS spectrogram simplifies；It is compareed finally by the standard spectrogram with storage, or cashew nut paint is relatively identified by characterising mass spectrometry peak.
Gain effect of the invention is as follows:
The invention belongs to be used to identify cashew nut lacquer coat for derivative-pyrolysis-high resolution gas chromatography-mass spectrography for the first time, by institute
The GC/MS spectrogram of acquisition carries out detailed analysis and interprets, and has obtained cashew nut lacquer coat derivative-pyrolysis-high resolution gas chromatography-mass spectrogram
Characteristic pyrolysis products characteristic mass number is 122,290,312,314,316,318 and 344 etc..Identification cashew nut provided by the present invention
The method of lacquer coat also has many advantages, such as that accuracy is high, reproducible and simple and quick.
Specific embodiment
Further below in conjunction with the embodiments with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, specific quality, reaction time in example
With the example that temperature, technological parameter etc. are also only in OK range, those skilled in the art is according to the present invention above-mentioned
Some nonessential modifications and adaptations that content is made all belong to the scope of protection of the present invention.Particular technique is not specified in embodiment
Or condition person, it is described technology or conditions or to be carried out according to the literature in the art according to product description.It is used
Production firm person is not specified in reagent or instrument, is the conventional products that can be bought by market.
Embodiment 1
The unknown coating sample of 1mg is weighed, it is molten that the tetramethylammonium hydroxide that 5 microlitres of mass percent concentrations are 25% is added
Liquid is packed into heat cracker and is cracked；Cracking condition: 500 DEG C of cracking temperature, time 10s；The substance that cracking is generated imports
Gas chromatograph-mass spectrometer (GC-MS) (GC/MS), GC/MS condition: DB-5 capillary chromatographic column；Using helium as carrier gas, carrier gas is
Constant current mode, flow velocity 1mL/min；Using Splitless injecting samples；Temperature program: 40 DEG C are kept for 5 minutes, with the speed of 50 DEG C/min
To 320 DEG C, 10min is kept；The temperature of level four bars mass detector is set as 150 DEG C；The energy of EI ion source is 70ev, ion source
Temperature is 250 DEG C；TIC full scan；Total ion current figure is obtained, is compareed with the cashew nut paint standard spectrogram previously stored, similarity is big
In 90%.GC/MS spectrogram contains the special domestic animal peaks such as 122,290,312 and 314.Identified, which is cashew nut lacquer coat.
Embodiment 2
The unknown coating sample of 1mg is weighed, the ethanol solution reaction of 10 microlitre of 10% dimethyl suflfate is added, is packed into hot tearing
It is cracked in solution device；Cracking condition: 300 DEG C of cracking temperature, time 3min；The substance that cracking is generated imports gas-chromatography-
Mass spectrometer (GC/MS), GC/MS condition: DB-5 capillary chromatographic column, using helium as carrier gas, carrier gas is constant current mode,
Flow velocity is 0.6mL/min；Using split sampling, split ratio 5:1；Temperature program: 40 DEG C are kept for 5 minutes, with 50 DEG C/min's
Speed keeps 10min to 320 DEG C；The temperature of level four bars mass detector is set as 150 DEG C；The energy of EI ion source is 70ev, from
Source temperature is 250 DEG C；TIC full scan；Obtain total ion current figure.GC/MS spectrogram contains the spies such as 122,290,312,314,316
Domestic animal peak.Identified, which is cashew nut lacquer coat.
Embodiment 3
The unknown coating sample of 1mg is weighed, the ethanol solution reaction of 10 microlitre of 10% iodomethane is added, is packed into heat cracker
Inside cracked；Cracking condition: 750 DEG C of cracking temperature, time 1s；The substance that cracking is generated imports gas chromatography-mass spectrometry
With instrument (GC/MS), GC/MS condition: DB-5 capillary chromatographic column is using helium as carrier gas, and carrier gas is constant current mode, and flow velocity is
2.0mL/min；With split sampling, split ratio 50:1；Temperature program: 40 DEG C keep 5 minutes, extremely with the speed of 50 DEG C/min
320 DEG C, keep 10min；The temperature of level four bars mass detector is set as 150 DEG C；The energy of EI ion source is 70ev, ion source temperature
Degree is 250 DEG C；TIC full scan；Obtain total ion current figure.GC/MS spectrogram contains the special domestic animal peaks such as 122,290,312,316.Through reflecting
Fixed, which is cashew nut lacquer coat.
Embodiment 4
The unknown coating sample of 1mg is weighed, 5 microlitre of 25% tetramethyl ammonium hydroxide solution is added, is packed into heat cracker
It is cracked；Cracking condition: 500 DEG C of cracking temperature, time 10s；The substance that cracking is generated imports gas chromatography-mass spectrography
Instrument (GC/MS), GC/MS condition: DB-5 capillary chromatographic column is using helium as carrier gas, and carrier gas is constant current mode, and flow velocity is
1mL/min；Using Splitless injecting samples；Temperature program: 40 DEG C are kept for 5 minutes, with the speed of 50 DEG C/min to 320 DEG C, are kept
10min；The temperature of level four bars mass detector is set as 150 DEG C；The energy of EI ion source is 70ev, and ion source temperature is 250 DEG C；
TIC full scan；Total ion current figure is obtained, is compareed with the cashew nut paint standard spectrogram previously stored, similarity is less than 20%.GC/MS
Spectrogram does not contain the special domestic animal peaks such as 122,290,312,314,316,318 and 344.Identified, which is not cashew nut lacquer coat.
Claims (9)
1. a kind of derivative-pyrolysis-high resolution gas chromatography-mass spectrometry identification cashew nut paint method, it is characterised in that specific step is as follows:
1) it is packed into heat cracker after mixing cashew nut lacquer coat sample with methylating reagent and carries out heating cracking, obtained cracking and produce
Object；
2) pyrolysis product obtained in step 1) is imported into sample introduction in gas chromatograph-mass spectrometer (GC-MS) (GC/MS), record through interface
GC-MS spectrogram；
Chromatographic condition is as follows: chromatographic column uses capillary gas chromatographic column；Using helium as carrier gas；Using shunting or do not shunt
Sample introduction；Using temperature programming；
Mass spectrometry parameters are as follows: using level four bars mass detector；Using EI ion source；
3) GC-MS spectrogram is analyzed, is in 122,290,312,314,316,318 and 344 using comprising detection mass number
One or more features peak cashew nut paint is analyzed and identified；Or the standard for storing the GC-MS spectrogram recorded and scanning
Spectrogram control, is identified according to spectrogram similarity degree.
2. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
Tetramethylammonium hydroxide (TMAH), one in dimethyl suflfate or iodomethane are selected from, methylating reagent described in step 1)
Kind.
3. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
In cracking condition described in step 1) are as follows: pyrolysis time 1s-3min, 300-750 DEG C of cracking temperature.
4. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
In the capillary gas chromatographic column is low-pole column.
5. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
In the carrier gas is constant current mode, and flow velocity is 0.6~2.0mL/min.
6. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
In the temperature program are as follows: 40 DEG C of initial temperature, keep 5min；320 DEG C are risen to 20 DEG C/min, keeps 10min.
7. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
In the split ratio of the split sampling is 5:1~50:1.
8. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
In the temperature of the level four bars is set as 150 DEG C.
9. derivative-pyrolysis-high resolution gas chromatography according to claim 1-mass spectrometry identification cashew nut paint method, feature exist
In the energy of the EI ion source is 70ev, and ion source temperature is 250 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS552642A (en) * | 1978-06-20 | 1980-01-10 | Sumitomo Chem Co Ltd | Preparation of n-methyl-benzthiazolone derivative |
| CN103439429A (en) * | 2013-08-30 | 2013-12-11 | 江苏正大清江制药有限公司 | Method for measuring residual amount of trifluoroacetic acid in organic medicine |
| CN106872615A (en) * | 2017-03-06 | 2017-06-20 | 杭州普洛赛斯检测科技有限公司 | Methylate treatment vapor detection analysis method |
| CN107688065A (en) * | 2017-09-11 | 2018-02-13 | 上海药明康德新药开发有限公司 | The gas chromatography combined with mass spectrometry detection method that chloromethyl methyl ether remains in bulk drug |
-
2019
- 2019-05-16 CN CN201910405305.3A patent/CN110068627A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS552642A (en) * | 1978-06-20 | 1980-01-10 | Sumitomo Chem Co Ltd | Preparation of n-methyl-benzthiazolone derivative |
| CN103439429A (en) * | 2013-08-30 | 2013-12-11 | 江苏正大清江制药有限公司 | Method for measuring residual amount of trifluoroacetic acid in organic medicine |
| CN106872615A (en) * | 2017-03-06 | 2017-06-20 | 杭州普洛赛斯检测科技有限公司 | Methylate treatment vapor detection analysis method |
| CN107688065A (en) * | 2017-09-11 | 2018-02-13 | 上海药明康德新药开发有限公司 | The gas chromatography combined with mass spectrometry detection method that chloromethyl methyl ether remains in bulk drug |
Non-Patent Citations (3)
| Title |
|---|
| FRANCESCA CAPPITELLI ET AL1: "An initial assessment of thermally assisted hydrolysis and methylation-gas chromatography/ mass spectrometry for the identification of oils from dried paint films", 《JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS》 * |
| SEUNG WOOK KIM ET AL: ""Direct Analysis of Tackifying Resins in Vulcanized Rubber by Simultaneous Pyrolysis Methylation-Gas Chromatography/Mass Spectrometry", 《BULL. KOREAN CHEM. SOC》 * |
| 付迎春 等: "应用热辅助水解甲基化裂解气相色谱质谱技术对古代漆器漆膜的分析研究", 《文物保护与考古科学》 * |
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