CN108562668A - A kind of method of GC-MS and tentaculum electric potential instrument combination analysis insect infochemical - Google Patents
A kind of method of GC-MS and tentaculum electric potential instrument combination analysis insect infochemical Download PDFInfo
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- CN108562668A CN108562668A CN201810410750.4A CN201810410750A CN108562668A CN 108562668 A CN108562668 A CN 108562668A CN 201810410750 A CN201810410750 A CN 201810410750A CN 108562668 A CN108562668 A CN 108562668A
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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
Abstract
The present invention proposes a kind of method of GC MS and tentaculum electric potential instrument combination analysis insect infochemical, belong to screening compound determination techniques field, it can ensure that the screening of insecticidal active substance is synchronous with the identification of sample material ingredient to carry out, experimental procedure is simplified, rapidly and efficiently, it can ensure the consistency of experimental data, and more economical practicality.The technical solution includes cutting the feeler of insect along base portion, and after removal top is a little, in vitro feeler both ends are separately fixed on the probe of tentaculum electric potential instrument with conducting resinl, and is connected with microelectrode；By in sample feeding to gas chromatograph, makings tentaculum electric potential instrument combination analysis is carried out；Mass Spectrometer Method is carried out to the peak that identical retention time occurs on gas chromatography mass spectrometry chromatogram and tentaculum electric potential instrument chromatogram, the mass spectrogram by checking standard spectrum library and n-compound identifies active insect infochemical.The present invention can be applied to insect to the impression mechanism of infochemical, screening activated information element ingredient or plant secondary substance etc..
Description
Technical field
The invention belongs to screening compound determination techniques field more particularly to a kind of GC-MS and the combinations point of tentaculum electric potential instrument
The method for analysing insect infochemical.
Background technology
With the rapid economic development in our country, people's living standard increasingly improves, especially to high-quality diet, life
The continuous improvement of the demands such as environment living, has expedited the emergence of the fast development of green agriculture, organic agriculture, and during production estimation
The problem of inevitably facing agricultural pests, therefore, forces people to look for the green prevention and control technology of pest control.Utilize elder brother
Worm infochemical inhibits pest to cause harm, and is lost caused by can reducing pest damage and preserves the ecological environment, ensures
Crop safety, the whole upgrading synergy for promoting agricultural product, meet the target of sustainable development of agricultural production, therefore, this
The research of aspect has become the research hotspot of insect chemistry ecology aspect.
Electroantennogram (EAG) and gas-chromatography-tentaculum electric potential (GC-EAD) are most important in Chemical ecology of insect
Electrophysiological technique, in research insect to the impression mechanism of infochemical, screening activated information element ingredient or Plant Secondary Materials
Substance etc. plays key effect.Tentaculum electric potential is the electrophysiological technique that direct detection insect reacts airborne signal chemical,
In pheromones and volatile plant secondary pollutant Quality Research, tentaculum electric potential technology law can identify sense of the insect to chemical signal
By channel, insect is filtered out from a series of chemical substance the reactive compound of physiological reaction, follow-up to greatly simplify
Research work.
EAG is usually used together with GC, referred to as tentaculum electric potential-gas spectrum combined instrument (GC-EAD), utilizes gas-chromatography energy
The advantage that microcomponent is detached from complex mixture, in conjunction with the high selectivity of EAG, it is not necessary to all to each section chemical composition
Detailed analysis is carried out, only considers that EAG has the substance of reaction, the rapid screening of chemical mixture may be implemented.GC-EAD is being studied
Insect has many successful stories with semiochemical, but needs the GC-MS that arranges in pairs or groups when in use, and in identical chromatographic condition
Under, it is qualitative to bioactive ingredients progress, it is complex for operation step, and the appearance time of the two can be variant.
Invention content
The present invention proposes a kind of method of GC-MS and tentaculum electric potential instrument combination analysis insect infochemical, this method
Ensure that the screening of insecticidal active substance is synchronous with the identification of sample material ingredient to carry out, experimental procedure is simplified, rapidly and efficiently, can
Ensure the consistency of experimental data, it is economical and practical.
In order to achieve the above object, the present invention provides a kind of makings and tentaculum electric potential instrument combination analysis insect chemoinformatics
The method of substance, includes the following steps：
The feeler of insect is cut along base portion, after removal top is a little, is fixed in vitro feeler both ends respectively with conducting resinl
It is connected on the probe of tentaculum electric potential instrument, and with microelectrode；
By in sample feeding to gas chromatograph, makings-tentaculum electric potential instrument combination analysis is carried out；
Mass Spectrometer Method is carried out to the peak that identical retention time occurs on gas chromatography mass spectrometry chromatogram and tentaculum electric potential instrument chromatogram,
Mass spectrogram by checking standard spectrum library and n-compound identifies active insect infochemical.
Preferably, adding two-way miniflow current divider in the gas chromatograph, mass spectrograph, another way connection are connected all the way
Tentaculum electric potential instrument, wherein the sample gas detached from gas-chromatography capillary column end is divided into two strands of air-flows with setting ratio, the former
It flows into mass spectrograph, after the latter is heated to proper temperature, imports in the cleaning gas tream persistently supplied and flow into tentaculum electric potential instrument
And blow to insect feeler.
The length of mass spectrograph and two branches for being connected to tentaculum electric potential instrument is connected in above-mentioned technical proposal by adjusting,
The wave crest that wave crest and EAG that makings chromatography obtains can be achieved records simultaneously, and realizes and effectively correspond to, and can make the chemistry of collection in this way
Information substance is screened rapidly, and the mass spectrogram by checking standard spectrum library and n-compound can be by efficient Rapid identification.It needs
Illustrate, when detecting different infochemicals for different insects species, set air-flow ratio can be different
, which can be realized by adjusting the length for two branches for being connected to mass spectrograph and being connected to tentaculum electric potential instrument.
Preferably, the insect feeler is the adult feeler of bollworm, oriental tobacco budworm or black cutworm.
Preferably, the sample gas detached from gas-chromatography capillary column end is with 1:3 ratio is divided into two strands of air-flows.
Preferably, gas chromatographic column is HP-5ms Ultra Inert, 30m × 250 μm ID, 0.25 μm；Mass chromatography
Column is DB5MS, 2.75m × 150 μm ID；Tentaculum electric potential instrument chromatographic column is DB5MS, 1m × 200 μm ID.In the technical solution, gas
Phase chromatographic column is included for instrument, the length of mass chromatography column and tentaculum electric potential chromatographic column be by measuring and calculating treated length, with
Ensure that the flow-rate ratio of two branches is 1:3.
Preferably, by sample feeding to when gas chromatograph use Splitless injecting samples, 2.0 μ L of sample size；Carrier gas is height
Pure helium, flow velocity 2.25mL/min；Temperature programming, 40 DEG C of initial temperature are kept for 2 minutes, are warming up to 260 DEG C with 5 DEG C/min, are protected
It holds 5 minutes.
Preferably, Mass Spectrometry Conditions：El ion sources, electron energy 70eV, proton scanning range 35-500amu, ion source
230 DEG C of temperature, 150 DEG C of level four bars temperature, 250 DEG C of transmission line temperature.
Preferably, providing stable cleaning gas tream using stimulation flow generator, and air-flow velocity is controlled in 20-
30ml/min。
Preferably, temperature is adjusted to 250 DEG C and is heated for sample gas by the connector in adjusting gas chromatograph,
To prevent sample gas from condensing.
It should be noted that Parameter Conditions sheet involved in above-mentioned gas-chromatography, mass spectrum and stimulation flow generator
Field technology personnel can rationally be adjusted according to different substances is detected, it is not limited to cited by above-mentioned technical proposal.
Preferably, the tentaculum electric potential instrument is arranged in faraday cup.In the program in order to avoid tentaculum electric potential instrument by
Therefore the interference of electromagnetic field drifted about to surrounding has carried out special setting to it.
Compared with prior art, the advantages and positive effects of the present invention are：
GC-MS provided by the present invention can make screening and the sample material ingredient of insecticidal active substance with EAG method for combined use
Identification synchronize carry out, can it is effective simplification experimental procedure while, ensure the consistency of experimental data.In addition, this method will
It originally makees two gas chromatographs that GC-MS and GC-EAD needs and is adjusted to one, in addition, when blocking towards the port of EAG
The needs of only GC-MS operations can be also completed, therefore more economical, it is cost-effective.
Description of the drawings
The GC-MS-EAG operating mode schematic diagrames that Fig. 1 is provided by the embodiment of the present invention；
The bollworm female moth that Fig. 2 is provided by the embodiment of the present invention is to the EAG response diagrams (A) of sample and corresponding sample
Product compound Mass Spectrometer Method figure (B).
Specific implementation mode
It will be provided for the embodiments of the invention makings and tentaculum electric potential instrument combination analysis insect infochemical below
Method in technical solution be clearly and completely described, it is clear that described embodiment is only that a present invention part is real
Example is applied, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creation
Property labour under the premise of the every other embodiment that is obtained, shall fall within the protection scope of the present invention.
Embodiment 1
One, experiment material
Benzaldehyde can cause bollworm adult antennae response, be solvent by solute, n-hexane of benzaldehyde, be configured to concentration
For the sample solution of 20ppm；2 days bollworm female adults after emergence.
Two, experimental method
Using gas-chromatography (GC)-mass spectrum (MS)-tentaculum electric potential instrument (EAG), (GC is for sample analysis identification
Agilent7890B, MS Agilent7010B, EAG originate from Syntech).
Method flow is as shown in Figure 1, include：
GC-MS conditions are as follows：Sample feeding chromatographic column be HP-5ms Ultra Inert (30m × 250 μm ID,
Filmthickness is 0.25 μm, Agilent Technologies), connection mass chromatography column is the DB5MS (μ of 2.75m × 150
MID, filmthickness be 0 μm, Agilent Technologies), connection tentaculum electric potential instrument chromatographic column for DB5MS (1m ×
200 μm of ID, filmthickness are 0 μm, Agilent Technologies)；Splitless injecting samples, 2.0 μ L of sample size；Carrier gas
For high-purity helium, flow velocity 2.25mL/min；Temperature programming, 40 DEG C of initial temperature are kept for 2 minutes, 260 are warming up to 5 DEG C/min
DEG C, it is kept for 5 minutes.Mass Spectrometry Conditions：El ion sources, electron energy 70eV, proton 35~500amu of scanning range, ion source temperature
230 DEG C, 150 DEG C of level four bars temperature, 250 DEG C of transmission line temperature；By checking standard spectrum library (NIST, willey) and standard chemical combination
The mass spectrogram of object carries out qualitative analysis according to the retention time of n-compound to extract components.
Prepared by feeler and tentaculum electric potential instrument determination condition is as follows：From the feeler base portion on bollworm female adult head by a feeler
It cuts, removes 2, top flagellum, the both ends of in vitro feeler, which are separately fixed at tentaculum electric potential, with 360 conducting resinls of Spectra visits
On head (PRG-2, Syntech), and it is connected with the microelectrode for being placed on micromanipulation platform (MP-15, Syntech)；By stimulation gas
Flow-generator (CS-55, Syntech) provides steady air flow, and control air-flow velocity is in 20-30ml/min；Gas-chromatography is adjusted to connect
Device (EC-03, Syntech) temperature is connect to 250 DEG C, substance heating is shunted for gas phase, prevents sample from condensing；Signal passes through binary channels
USB interface data acquisition controller (IDAC-2, Syntech) amplifies, and the signal of output is input in computer (Thinkpad
T410I), acquisition, the storage of data are carried out with GC-EAD signals recording analysing program (GC-EAD 2010V 1.2.2, Syntech)
It deposits and handles.
Start gas-chromatography, after preheating, start sample introduction, while gas chromatographic sample introduction, clicks GC-EAD signals record point
Analyse program, synchronous start recording.
Three, experimental result
As shown in Fig. 2, being measured by tentaculum electric potential instrument, there is a substance that can cause in sample in tentaculum electric potential instrument collection of illustrative plates (A)
The reaction of bollworm female moth feeler, appearance time 11.507min；The appearance time of the compound is corresponded in mass spectrogram (B)
It is almost the same with EAG appearance times (11.507min) for 11.481min, it is identified as target compound benzaldehyde.
The result shows that the method that the embodiment of the present invention is provided can quickly and effectively screen activated information compound, and energy
Ensure the consistency of experimental data, it is economical and practical, there is good application value.
Claims (10)
1. a kind of method of makings and tentaculum electric potential instrument combination analysis insect infochemical, which is characterized in that including following
Step：
The feeler of insect is cut along base portion, after removal top is a little, is separately fixed in vitro feeler both ends with conducting resinl tactile
On the probe of angle potentiometer, and it is connected with microelectrode；
By in sample feeding to gas chromatograph, makings-tentaculum electric potential instrument combination analysis is carried out；
Mass Spectrometer Method is carried out to the peak that identical retention time occurs on gas chromatography mass spectrometry chromatogram and tentaculum electric potential instrument chromatogram, is passed through
The mass spectrogram of verification standard spectrum library and n-compound identifies active insect infochemical.
2. according to the method described in claim 1, it is characterized in that, add two-way miniflow current divider in the gas chromatograph,
Connect mass spectrograph all the way, another way connects tentaculum electric potential instrument, wherein the sample gas detached from gas-chromatography capillary column end with
Setting ratio is divided into two strands of air-flows, the former flows into mass spectrograph, and after the latter is heated to proper temperature, remittance is persistently supplied clear
It is flowed into tentaculum electric potential instrument in clean air-flow and blows to insect feeler.
3. according to the method described in claim 2, it is characterized in that, the insect feeler is that bollworm, oriental tobacco budworm or small ground are old
The adult feeler of tiger.
4. according to the method described in claim 3, it is characterized in that, from gas-chromatography capillary column end detach sample gas with
1:3 ratio is divided into two strands of air-flows.
5. according to the method described in claim 3, it is characterized in that, gas chromatographic column be HP-5ms Ultra Inert, 30m ×
250 μm of ID, 0.25 μm；Mass chromatography column is DB5MS, 2.75m × 150 μm ID；Tentaculum electric potential instrument chromatographic column be DB5MS, 1m ×
200μmID。
6. according to the method described in claim 3, it is characterized in that, by sample feeding to when gas chromatograph using not being diverted into
Sample, 2.0 μ L of sample size；Carrier gas is high-purity helium, flow velocity 2.25mL/min；Temperature programming, 40 DEG C of initial temperature are kept for 2 minutes,
260 DEG C are warming up to 5 DEG C/min, is kept for 5 minutes.
7. according to the method described in claim 3, it is characterized in that, Mass Spectrometry Conditions：El ion sources, electron energy 70eV, proton
Scanning range 35-500amu, 230 DEG C of ion source temperature, 150 DEG C of level four bars temperature, 250 DEG C of transmission line temperature.
8. according to the method described in claim 3, it is characterized in that, providing stable cleaning gas using stimulation flow generator
Stream, and air-flow velocity is controlled in 20-30ml/min.
9. according to the method described in claim 3, it is characterized in that, temperature is adjusted to by the connector adjusted in gas chromatograph
250 DEG C are heated for sample gas, to prevent sample gas from condensing.
10. according to claim 1-9 any one of them methods, which is characterized in that the tentaculum electric potential instrument is arranged in faraday
In cage.
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| CN110771603A (en) * | 2019-11-08 | 2020-02-11 | 西北农林科技大学 | Method for testing citrus young fruit volatile matter with behavioral response to bactrocera minax imagoes |
| CN112385610A (en) * | 2020-11-10 | 2021-02-23 | 南通大学 | Detection method for biological antenna perception mechanism research |
| CN113466359A (en) * | 2021-06-04 | 2021-10-01 | 北京农业智能装备技术研究中心 | Volatile chemical pesticide spray drift pollution detection system |
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| CN110771603A (en) * | 2019-11-08 | 2020-02-11 | 西北农林科技大学 | Method for testing citrus young fruit volatile matter with behavioral response to bactrocera minax imagoes |
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| CN112385610B (en) * | 2020-11-10 | 2022-02-01 | 南通大学 | Detection method for biological antenna perception mechanism research |
| CN113466359A (en) * | 2021-06-04 | 2021-10-01 | 北京农业智能装备技术研究中心 | Volatile chemical pesticide spray drift pollution detection system |
| CN113466359B (en) * | 2021-06-04 | 2023-04-07 | 北京农业智能装备技术研究中心 | Volatile chemical pesticide spray drift pollution detection system |
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