CN106770752B - A kind of method for building up of Dalbergia timber thermal cracking finger-print and its application - Google Patents
A kind of method for building up of Dalbergia timber thermal cracking finger-print and its application Download PDFInfo
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- CN106770752B CN106770752B CN201611136575.1A CN201611136575A CN106770752B CN 106770752 B CN106770752 B CN 106770752B CN 201611136575 A CN201611136575 A CN 201611136575A CN 106770752 B CN106770752 B CN 106770752B
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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
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Abstract
The invention belongs to technical field of analysis and detection, more particularly to a kind of method for building up of Dalbergia timber thermal cracking finger-print, this method Dalbergia timber to be identified using Pintsch process, pyrolysis product enters gas chromatographic column with carrier gas and is separated, and analyzes to obtain Dalbergia timber finger-print by gas chromatography-mass spectrography.Dalbergia wood quality is identified using the method for building up of Dalbergia timber thermal cracking finger-print provided by the invention, the amount of samples is small, and it is not necessarily to any pre-treatment step, it avoids because pre-processing possible analysis distortion and loss for information about, and thermal cracking gas chromatography mass spectrogram favorable reproducibility, can reflect the fingerprint feature information of Dalbergia timber.
Description
Technical field
The invention belongs to technical field of analysis and detection, and in particular to a kind of foundation of Dalbergia timber thermal cracking finger-print
Method and its application.
Background technique
Dalbergia wood, drop smell good, and santal belongs to the expensive fragrant material of santal generic name.Dalbergia wood also known as rosewood；Drop smells good including two Guangdong Huang
Wingceltis, oblique leaf wingceltis is eponymous with agalloch eaglewood, is one of big fragrance of ancient times four；Santal also known as bath are fragrant, referred to as " tree of gold ", these types
Almost whole body is all precious to timber, and all has important medical value and economic value.
Due to the high economic value of these types of timber, all kinds of false timber in market can be found everywhere, simultaneously because drop smells good very
Rare and resource exhaustion has many people to replace the drop product that smell good fragrant or be used as medicine with Huanghua Pear；On the other hand because of the scientific name of Huanghua Pear
For " dalbergia odorifera ", some scholars and scientific research personnel are just that " drop with " dalbergia wood " thus in the case where no on-the-spot investigation
It is fragrant ".
Currently, come to identify the rare timber of Dalbergia from scientific angle there are no correlative study, it is main in the market to utilize observation
Appearance by virtue of experience identifies all kinds of timber, this ensure the accuracy of identification cannot.
In view of this, the present invention is specifically proposed.
Summary of the invention
The purpose of the present invention is to provide a kind of method for building up of Dalbergia timber thermal cracking finger-print, this method can be with
The cracking finger-print of different quality Dalbergia timber heat is accurately set up, and by comparing the difference between each finger-print
For identifying the true and false of Dalbergia timber and evaluating its quality, this method is more accurate compared to conventional identification method.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of method for building up of Dalbergia timber thermal cracking finger-print, Pintsch process timber to be identified, pyrolysis product with
Carrier gas enters gas chromatographic column and is separated, and analyzes to obtain Dalbergia timber thermal cracking fingerprint by gas chromatography-mass spectrography
Map.
Thermal cracking gas chromatography mass spectrography is under the operating condition of strict control, to make macromolecule by means of cracking technique
Compound or non-VOC are degraded to volatile products, by height explanation chromatographic isolation after again by or detector
It is identified.Due to the composition and relative amount and the structure of measured matter, composition, property of volatile products have it is certain corresponding
Relationship, every kind of substance its pyrogram under certain cracking condition have respective characteristic, referred to as fingerprint cracking pattern.
The type that thus can effectively identify high-molecular compound or non-VOC, qualitatively and quantitatively analysis of mixtures
In component.
The Dalbergia timber of different cultivars is analyzed by chromatographic fingerprinting and shows inherent a variety of chemical components as best one can
Now on complete one or several chromatograms, by it is inherent it is inconsistent, unstable show, foundation can reflect comprehensively
The type and quantity of Dalbergia timber intrinsic chemical ingredient, and then reflect different types of difference.Especially in yellow wingceltis at this stage
In the case that category timber finger-print research is less, the finger-print of Dalbergia timber is studied by the way of thermal cracking fingerprint,
The type of Dalbergia timber will effectively be characterized.
The characteristics of technology is that amount of samples is small, generally milligram grade, Gamma Magnitude, is not necessarily to any pre-treatment step, avoids
Because pre-processing possible analysis distortion and loss for information about, and thermal cracking gas chromatography mass spectrogram reproducibility
It is good, it can reflect the fingerprint feature information of timber.
The present invention is worth the Dalbergia timber referred to, can be selected from Lignum Dalbergiae benthamii, oblique leaf wingceltis, rosewood, yellow wingceltis etc..
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, the item of the Pintsch process
Part are as follows:
Desiccated wood is ground into after fine powder and carries out thermal cracking in atmosphere of inert gases, cracking temperature is 350 DEG C
~500 DEG C, pyrolysis time is 20s~30s.
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, the inert gas are helium
Gas.
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, the timber to be identified
Dosage is 0.05mg~0.3mg.
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, the injection port of gas-chromatography
Temperature is 300 DEG C~400 DEG C.
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, the heating journey of gas-chromatography
Sequence are as follows:
1min~3min is kept at 60~100 DEG C, is warming up to 290 DEG C~320 DEG C with the rate of 6~12 DEG C/min, is protected
Hold 2min~8min.
Temperature programming significantly affects the separating effect of detection object and peak shape, and heating rate is larger, is unfavorable for
The separation of chaff interferent in object and matrix；Conversely, chromatography peak stretching, analysis time are longer.
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, the sample introduction item of gas-chromatography
Part are as follows:
Input mode is split sampling, split ratio (50~100): 1；Carrier gas is helium；Constant current mode, column flow 0.5
~1.5mL/min, 280 DEG C~330 DEG C of interface temperature.
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, hair used in gas-chromatography
Capillary chromatographic column is the UA5 (P) of Frontier company, Japan.
The capillary chromatographic column that the present invention uses is the UA5 (P) of Frontier company, Japan；Preferably, the capillary
The column length of chromatographic column is 30m, and diameter 0.25mm, film thickness is 0.25 μm.
Preferably, the method for building up of Dalbergia timber thermal cracking finger-print as described above, mass ion source is electronics
Bombardment source, ion source electron energy: 60eV~80eV；Scanning range: 35amu~500amu.
The method for building up of Dalbergia timber thermal cracking finger-print as described above in the identification Dalbergia timber true and false and its
Application in quality.
When detecting, standard items and sample to be tested are detected under identical conditions, then compares the two characteristic peak and goes out
Existing position, then quality more similar with standard items is also just closer, thus can the true and false, quality, the place of production etc. to sample to be tested
Information is identified.
Since the thermal cracking finger-print of the Dalbergia timber of different qualities has marked difference, those skilled in the art
The technical solution that can be recorded according to the present invention establishes the thermal cracking finger-print of high-quality Dalbergia timber, then by yellow wingceltis to be detected
The thermal cracking finger-print for belonging to timber is compared therewith, can be used to the true and false of identification Dalbergia timber, and can be used for evaluating
Its quality.
Wherein, it is preferred that the method for standard of comparison product and sample to be tested thermal cracking finger-print can be fuzzy clustering point
Analysis method specially carries out comprehensive analysis to map using fuzzy clustering data processing means；And for what is differed greatly, directly see
Examine the difference of characteristic peak.
Compared with prior art, the invention has the benefit that
Dalbergia wood quality is identified using the method for building up of Dalbergia timber thermal cracking finger-print provided by the invention,
The amount of samples is small, and is not necessarily to any pre-treatment step, avoid because pre-process possible analysis distortion with for information about
Loss, and thermal cracking gas chromatography mass spectrogram favorable reproducibility can reflect the fingerprint feature information of timber.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the finger-print result figure of 4 Lignum Dalbergiae benthamii of the embodiment of the present invention；
Fig. 2 is the finger-print result figure of the oblique leaf wingceltis of the embodiment of the present invention 5；
Fig. 3 is the finger-print result figure of 6 rosewood of the embodiment of the present invention；
Fig. 4 is the finger-print result figure of 7 sandalwood of the embodiment of the present invention.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
Present embodiments provide a kind of method for building up of Lignum Dalbergiae benthamii thermal cracking finger-print.
1, sample preparation
Dry yellow wingceltis timber is cut into small pieces, powder is milled into, 0.05mg powder is accurately weighed in cracking pot, wait split
Solution test is used.
2, cracking conditions
Sample is placed in pyrolysis furnace in the case where helium atmosphere encloses, 20s, the gas of generation are cracked under 500 DEG C of cracking temperature
Chromatographic column is brought by carrier gas to be separated.
3, GC-MS operating condition
It is GC injector temperature using the condition that GC-MS carries out separation detection to pyrolysis product: 300 DEG C；Carrier gas: helium；
Column oven program: heating initial temperature is 60 DEG C, keeps 3min, is warming up to 290 DEG C with the rate of 6 DEG C/min, protects
Hold 5min.
Input mode is split sampling, split ratio 50:1；Carrier gas is helium；Constant current mode, column flow 0.5mL/min,
280 DEG C of interface temperature；Capillary chromatographic column: UA5 (P) (column length 30m, diameter 0.25mm, the film of Japanese Frontier company
Thickness is 0.25 μm)
Mass ion source is electron bombardment ionization source (EI), ion source temperature: 220 DEG C；Quadrupole rod temperature: 140 DEG C；GC/MS connects
Mouth temperature: 270 DEG C；EI ion source electron energy: 60eV；Mass scan range: 35~500amu.
Embodiment 2
Present embodiments provide a kind of method for building up of Lignum Dalbergiae benthamii thermal cracking finger-print.
1, sample preparation
Dry yellow wingceltis timber is cut into small pieces, powder is milled into, 0.3mg powder is accurately weighed in cracking pot, wait split
Solution test is used.
2, cracking conditions
Sample is placed in pyrolysis furnace in the case where helium atmosphere encloses, 30s, the gas of generation are cracked under 350 DEG C of cracking temperature
Chromatographic column is brought by carrier gas to be separated.
3, GC-MS operating condition
It is GC injector temperature using the condition that GC-MS carries out separation detection to pyrolysis product: 400 DEG C；Carrier gas: helium；
Column oven program: heating initial temperature is 100 DEG C, keeps 1min, is warming up to 320 DEG C with the rate of 12 DEG C/min,
Keep 2min.
Input mode is split sampling, split ratio 100:1；Carrier gas is helium；Constant current mode, column flow 1.5mL/min,
330 DEG C of interface temperature；Capillary chromatographic column: UA5 (P) (column length 30m, diameter 0.25mm, the film of Japanese Frontier company
Thickness is 0.25 μm)
Mass ion source is electron bombardment ionization source (EI), ion source temperature: 240 DEG C；Quadrupole rod temperature: 160 DEG C；GC/MS connects
Mouth temperature: 290 DEG C；EI ion source electron energy: 80eV；Mass scan range: 35~500amu.
Embodiment 3
Present embodiments provide a kind of method for building up of yellow wingceltis cracking finger-print.
1, sample preparation
Dry yellow wingceltis timber is cut into small pieces, powder is milled into, 0.2mg powder is accurately weighed in cracking pot, wait split
Solution test is used.
2, cracking conditions
Sample is placed in pyrolysis furnace in the case where helium atmosphere encloses, 25s, the gas of generation are cracked under 400 DEG C of cracking temperature
Chromatographic column is brought by carrier gas to be separated.
3, GC-MS operating condition
It is GC injector temperature using the condition that GC-MS carries out separation detection to pyrolysis product: 350 DEG C；Carrier gas: helium；
Column oven program: heating initial temperature is 70 DEG C, keeps 2min, is warming up to 300 DEG C with the rate of 9 DEG C/min, protects
Hold 3min.
Input mode is split sampling, split ratio 70:1；Carrier gas is helium；Constant current mode, column flow 1.2mL/min,
300 DEG C of interface temperature；Capillary chromatographic column: UA5 (P) (column length 30m, diameter 0.25mm, the film of Japanese Frontier company
Thickness is 0.25 μm)
Mass ion source is electron bombardment ionization source (EI), ion source temperature: 230 DEG C；Quadrupole rod temperature: 150 DEG C；GC/MS connects
Mouth temperature: 280 DEG C；EI ion source electron energy: 70eV；Mass scan range: 35~500amu.
Embodiment 4
Present embodiments provide a kind of method for building up of Lignum Dalbergiae benthamii thermal cracking finger-print.
1, sample preparation
Dry yellow wingceltis timber is cut into small pieces, powder is milled into, 0.1mg powder is accurately weighed in cracking pot, wait split
Solution test is used.
2, cracking conditions
Sample is placed in pyrolysis furnace in the case where helium atmosphere encloses, 25s, the gas of generation are cracked under 420 DEG C of cracking temperature
Chromatographic column is brought by carrier gas to be separated.
3, GC-MS operating condition
It is GC injector temperature using the condition that GC-MS carries out separation detection to pyrolysis product: 320 DEG C；Carrier gas: helium；
Column oven program: heating initial temperature is 80 DEG C, keeps 2min, is warming up to 320 DEG C with the rate of 10 DEG C/min, protects
Hold 4min.
Input mode is split sampling, split ratio 50:1；Carrier gas is helium；Constant current mode, column flow 1.0mL/min,
320 DEG C of interface temperature；Capillary chromatographic column: UA5 (P) (column length 30m, diameter 0.25mm, the film of Japanese Frontier company
Thickness is 0.25 μm)
Mass ion source is electron bombardment ionization source (EI), ion source temperature: 230 DEG C；Quadrupole rod temperature: 150 DEG C；GC/MS connects
Mouth temperature: 280 DEG C；EI ion source electron energy: 70eV；Mass scan range: 35~500amu.
As a result as shown in Figure 1.
Embodiment 5
Oblique leaf wingceltis is detected according to the experiment condition of embodiment 4, the results are shown in attached figure 2.
Embodiment 6
Rosewood is detected according to the experiment condition of embodiment 4, the results are shown in attached figure 3.
Embodiment 7
Sandalwood, the results are shown in attached figure 4 are detected according to the experimental condition of embodiment 4
The purpose of the present invention is to provide a kind of method for building up of Dalbergia timber thermal cracking finger-print, this method can be with
Accurately set up the thermal cracking finger-print of different quality Dalbergia timber.By embodiment 4~6 as can be seen that identical
Testing conditions under, different types of Dalbergia timber has dramatically different thermal cracking finger-print, accordingly can be to Dalbergia
The information such as the true and false, quality and the place of production of timber are identified.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, but those skilled in the art should understand that: its
It is still possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features
It is equivalently replaced；And these are modified or replaceed, various embodiments of the present invention skill that it does not separate the essence of the corresponding technical solution
The range of art scheme.
Claims (3)
1. a kind of method for building up of Dalbergia timber thermal cracking finger-print, which is characterized in that be ground into desiccated wood tiny
Thermal cracking is carried out after powder in atmosphere of inert gases, cracking temperature is 350 DEG C ~ 500 DEG C, and pyrolysis time is 20s ~ 30s, cracking
Product enters gas chromatographic column with carrier gas and is separated, and analyzes to obtain Dalbergia timber hot tearing by gas chromatography-mass spectrography
Solve finger-print；
The dosage of the timber is 0.05mg ~ 0.3mg；
Chromatographic column used in gas-chromatography is the UA5(P of Frontier company, Japan) capillary chromatographic column；Mass ion source is electricity
Sub- bombardment source, ion source electron energy: 60eV ~ 80eV；Scanning range: 35amu ~ 500amu；
The temperature program of gas-chromatography are as follows: keep 1min ~ 3min at 60 ~ 100 DEG C, be warming up to the rate of 6 ~ 12 DEG C/min
290 DEG C ~ 320 DEG C, keep 2min ~ 8min；
The injector temperature of gas-chromatography is 300 DEG C ~ 400 DEG C；
Input mode is split sampling, split ratio (50 ~ 100): 1；Carrier gas is helium；Constant current mode, column flow be 0.5 ~
1.5mL/min, 280 DEG C ~ 330 DEG C of interface temperature.
2. the method for building up of Dalbergia timber thermal cracking finger-print according to claim 1, which is characterized in that described lazy
Property gas be helium.
3. the method for building up of Dalbergia timber thermal cracking finger-print of any of claims 1 or 2 is true in identification Dalbergia timber
Application in pseudo- and its quality.
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| CN107703231A (en) * | 2017-11-13 | 2018-02-16 | 中山市中广测协同创新中心 | A kind of method based on finger-print quick nondestructive identification broad-leaved yellow wingceltis Tenon product |
| CN110780014B (en) * | 2019-10-24 | 2022-07-19 | 莆田市家具产品质量监督检验中心 | Method for identifying gall-containing wood by gas chromatography-mass spectrometry technology |
| CN111948329A (en) * | 2020-06-01 | 2020-11-17 | 上海市质量监督检验技术研究院 | Method for identifying pteroceltis tatarinowii and pteroceltis tenuipes |
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| CN101637484A (en) * | 2009-09-08 | 2010-02-03 | 青海大学 | Active extract for sanwei sandalwood as well as extraction method and medical application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101637484A (en) * | 2009-09-08 | 2010-02-03 | 青海大学 | Active extract for sanwei sandalwood as well as extraction method and medical application thereof |
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| Title |
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| Catalytic pyrolysis of waste wood chip over mesoporous materials using Py-GC/MS;Seung-Soo Kim et al.;《Res Chem Intermed》;20111231;第37卷;全文 * |
| Thermal transformations of pine wood components under pyrolysis/gas chromatography/mass spectrometry conditions;M.E.Arias et al.;《J.Anal.Appl.Pyrolysis》;20061231;第77卷;第64页，图1-2 * |
| 檀香叶抽提物成分的Py-GC/MS分析;彭万喜 等;《华南理工大学学报(自然科学版)》;20081130;第36卷(第11期);第39页 * |
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