Gas chromatography detection method for enriching insect aggregation pheromones in air by using ionic liquid composite material
By preparing enrichment tubes using ionic liquid composite materials and combining them with gas chromatography detection methods, the problems of poor selectivity and slow adsorption rate of traditional adsorbents are solved, achieving efficient selective enrichment and quantitative detection of insect aggregation pheromones, which is applicable to the field of gas detection.
Patent Information
- Application Number
- CN202512010472.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-29
- Publication Date
- 2026-03-17
AI Technical Summary
In existing technologies, traditional adsorbents exhibit poor selectivity and slow adsorption rates when enriching insect aggregation pheromones, making accurate qualitative and quantitative detection of insect aggregation pheromones difficult, especially for α-pinene, which has a low recovery rate.
Ionic liquid composite materials are used as adsorbents. Enrichment tubes are designed and prepared based on the structural properties of ionic liquids. Combined with the enhancement of porous carriers, synergistic adsorption through multiple interactions such as electrostatics and hydrogen bonding is achieved. The selective strong interaction between ionic liquids and target pheromone molecules is utilized to form enrichment tubes for gas chromatography detection.
It significantly improves the selective enrichment effect of insect pheromones, and realizes the efficient enrichment and qualitative and quantitative detection of extremely low concentrations of insect aggregation pheromones. The operation is simple, the adsorbent can be reused, and the detection is achieved by heating to desorb, thus solving the problem of efficient enrichment of trace pheromone molecules.
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Figure CN121678885A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of gas detection technology, specifically relating to a gas chromatography detection method for enriching airborne insect aggregation pheromones with ionic liquid composite materials. Background Technology
[0002] Insect pheromones are trace behavioral regulatory substances produced and released by insects themselves to transmit information within or between species. The precursors of pheromones originate from the insect's food. Insects modify these precursor compounds to produce and release pheromones in response to changes in population density, location, and habitat. Insect aggregation pheromones are a type of insect pheromone secreted and released into the environment by insects to attract other insects of the same species to specific locations. Therefore, qualitative and quantitative analysis of the composition of insect aggregation pheromones in specific areas can provide valuable information for monitoring forest pests and detecting non-native invasive species. However, pheromone-producing insects only release pheromones at the nanogram level, and many pheromone molecules are unstable and easily degraded under oxygen and ultraviolet radiation, and are mixed with a large amount of volatile substances in forest air, such as α-pinene, β-pinene, limonene, myrcene, and terpinene, making direct qualitative and quantitative detection very difficult. Therefore, selective enrichment of pheromones in air samples is necessary.
[0003] Currently, the main methods for collecting ambient air samples include solution absorption sampling, adsorption tube sampling, filter membrane sampling, filter membrane-adsorbent combined sampling, direct sampling, and indirect sampling. Among these, adsorption tube sampling is widely used due to its portability and ease of operation. Adsorption tubes are ordinary glass tubes, quartz tubes, or stainless steel tubes filled with various adsorbents. The adsorption performance and selectivity of the adsorbent packing material determine the gas collection effect. Common solid adsorbents include activated carbon, silica gel, graphitized carbon black (Carbonpack series), carbon molecular sieves (Carboxen series), and porous organic polymers such as Tenax-TA and DVB. Previous studies have often directly used traditional commercial adsorbents to enrich insect pheromones, but these methods suffer from poor selectivity and slow adsorption rates, making accurate qualitative and quantitative detection of insect aggregated pheromones difficult. For example, Tenax packing material, widely used for pheromone enrichment, showed a recovery efficiency of only 47% for E8,E10-dodecadien-1-ylacetate after evacuating air at a flow rate of 17 L / min for 4 hours. Furthermore, studies by Sergio et al. have shown that Tenax TA has a recovery rate of less than 5% for α-pinene, and neither activated carbon nor silica gel can effectively adsorb α-pinene. Only Porapak Q and Porapak Rxn RP have a recovery rate of over 50% for α-pinene. Therefore, how to achieve efficient and selective enrichment of insect aggregation pheromone molecules for qualitative and quantitative detection of trace insect pheromones in the air is an urgent problem to be solved. Summary of the Invention
[0004] In view of this, the present invention provides a gas chromatography detection method for enriching airborne insect aggregation pheromones with ionic liquid composite materials, which solves the technical problems in the prior art.
[0005] The technical solution of this invention is: A gas chromatography detection method for enriching airborne insect aggregation pheromones with an ionic liquid composite material includes the following steps: An ionic liquid methanol solution was used as the impregnation solution, and an adsorption carrier was added. The mixture was impregnated at room temperature, and after removing the methanol by rotary evaporation, it was dried to obtain an ionic liquid composite material. The ionic liquid methanol solution included cations and anions. The cations were at least one of ethanolamine, ethylamine, 1-butyl-3-methylimidazolium, 1-hexyl-3-methylimidazolium, 1-octyl-3-methylimidazolium, and tetramethylguanidine. The anions were at least one of tetrafluoroborate, hexafluorophosphate, acetate, and bis(trifluoromethanesulfonyl)imide. Ionic liquid composite materials were used as adsorbents, and nitrogen was used as a carrier gas to activate and remove impurities from the adsorbents. Gas samples were collected using the activated and purified adsorbent to obtain a sampling column; The sampling column was thermally desorbed, and the content of insect aggregation pheromones in the sampling column was determined by gas chromatography.
[0006] Furthermore, the adsorption carrier is at least one of high molecular organic polymers, inorganic adsorption materials, carbon-based adsorption materials, and nanofiber materials.
[0007] Furthermore, the concentration of the ionic liquid methanol solution is 5 mg / mL to 25 mg / mL. After adding the adsorbent carrier to the ionic liquid methanol solution, it is impregnated at room temperature for 24 h to 48 h. After removing the methanol by rotary evaporation, it is vacuum dried at 60 °C to 80 °C for 8 h to 12 h.
[0008] Furthermore, the activation and purification of the adsorbent using an ionic liquid composite material as the adsorbent and nitrogen as the carrier gas includes the following steps: An ionic liquid composite material is filled into an empty tube, and the two ends of the empty tube are sealed with glass wool and 80-100 mesh sieves to form an enrichment tube. The enrichment tube was activated at a temperature of 250 ℃~300 ℃ with nitrogen as the carrier gas at a flow rate of 100~150 mL / min for 2 h~4 h to remove impurities; After activation, the enrichment tube was cooled to room temperature under continuous nitrogen flow before being removed.
[0009] Furthermore, gas sample collection includes the following steps: Connect one end of the activated enrichment tube to the sampling pump and sample the gas at a rate of 0.1 L / min to 1 L / min for 1 min to 60 min. After sampling, obtain the sampling column and seal both ends of the sampling column for later use.
[0010] Furthermore, the thermal desorption adopts a two-stage desorption mode, with nitrogen as the desorption gas; the first stage is enrichment tube desorption, with a desorption temperature of 230℃~280℃, a desorption time of 5min~15min, a desorption flow rate of 100mL / min~200mL / min, and a cold trap collection temperature of -30℃~0℃; the second stage is cold trap desorption, with a desorption temperature of 250℃~300℃, a desorption time of 1min~5min, a pre-trap split ratio of 0~3, and a post-trap split ratio of 0~3.
[0011] Furthermore, when determining the insect aggregation pheromone content in the sampling column using gas chromatography, a DB-5MS column was used; the carrier gas was nitrogen, the injection port was in pressure control mode and set to 100 kPa; the initial column temperature was 31℃, increased to 100℃ at a rate of 10℃ / min, then increased to 150℃ at a rate of 5℃ / min and held for 1 min; the injector temperature was 200℃; an FID detector was used at a temperature of 250℃; and the initial split ratio was 10:1.
[0012] Furthermore, the content of insect aggregation pheromones in the sampling column was determined by gas chromatography, including the following steps: Determine the standard working curve for each insect aggregation pheromone; The sampling column was placed in a thermal desorption instrument for desorption, and then introduced into a gas chromatograph to obtain the response peak. The response peak of each insect aggregation pheromone was substituted into the corresponding standard working curve, and linear regression was performed to obtain the mass of the insect aggregation pheromone. The content of the insect aggregation pheromone was obtained by dividing the mass of the insect aggregation pheromone by the volume of the collected gas.
[0013] Furthermore, the method for determining the standard working curve for each insect aggregation pheromone includes the following steps: Using a microsyringe, mixed standard solutions of different concentration ranges with preset mass were aspirated and injected into the prepared enrichment tubes. The enrichment tubes were placed in a thermal desorption instrument for desorption, and the solutions were introduced into a gas chromatograph to generate response peaks. The different masses of insect aggregation pheromones were linearly fitted with their corresponding response peaks to obtain standard working curves.
[0014] Furthermore, the concentration of the mixed standard solution is 0.005 mg / mL to 1 mg / mL.
[0015] Compared with existing technologies, the present invention provides a gas chromatography detection method for enriching airborne insect aggregation pheromones using an ionic liquid composite material. The method utilizes an ionic liquid methanol solution as an impregnating liquid, adds an adsorbent carrier, and then treats the mixture to obtain an ionic liquid composite material. The ionic liquid composite material is used as an adsorbent to form an enrichment tube, which is activated using nitrogen as a carrier gas. One end of the activated enrichment tube is connected to a sampling pump for gas sample sampling. After sampling, a sampling column is obtained. The sampling column is then thermally desorbed, and the content of insect aggregation pheromones in the sampling column is determined by gas chromatography. This invention utilizes the structural properties of ionic liquids to designably prepare ionic liquid composite materials as adsorbents, achieving synergistic adsorption through multiple interactions such as electrostatics and hydrogen bonding. Combined with the synergistic effect of porous carriers, this significantly increases the specific surface area and adsorption site density. Furthermore, based on the structural differences between target pheromone molecules and background gas molecules, ionic liquids with strong selective interactions with the target are designed to enhance the selective enrichment of insect pheromones. This achieves selective enrichment of extremely low concentrations of target insect aggregation pheromones. The operation is simple, the adsorbent is reusable, and desorption is achieved by heating to disrupt the interactions. This solves the problem of efficient enrichment of trace pheromone molecules, enabling qualitative and quantitative detection of trace insect pheromones in the air. It is highly practical and worthy of widespread application. Attached Figure Description
[0016] Figure 1 GC spectrum of ionic liquid blank control (taking [BMIM][BF4] as an example): This shows that due to the high thermal stability and low volatility of ionic liquids, no detectable organic pollutants were found in the sampling column detected by this method.
[0017] Figure 2 GC chromatogram of mixed reference standards: This illustrates the separation and identification of mixed standard reference standards using this method. 1. 2-Methyl-3-ethylene-2-ol (MB), 2. α-pinene, 3. β-pinene, 4. 3-carene, 5. limonene, 6. terpinene, 7. myrtol, 8. verbenatone.
[0018] Figure 3 GC spectrum of pheromones in enriched samples: This illustrates the determination of insect aggregation pheromones in simulated air using this method. 1. 2-Methyl-3-ethylene-2-ol (MB), 2. α-pinene, 3. β-pinene, 4. 3-carene, 5. limonene, 6. terpinene, 7. myrtol, 8. verbenatone. Detailed Implementation
[0019] Insect pheromones are trace behavioral regulatory substances produced and released by insects themselves to transmit information within or between species. The precursors of pheromones originate from the insect's food. Insects modify these precursor compounds to produce and release pheromones in response to changes in population density, location, and habitat. Insect aggregation pheromones are a type of insect pheromone secreted and released into the environment by insects to attract individuals of the same species to specific locations. Therefore, qualitative and quantitative analysis of the composition of insect aggregation pheromones in specific areas can provide valuable information for monitoring forest pests and detecting non-native invasive species. However, pheromone-producing insects only release pheromones at the nanogram level, and many pheromone molecules are unstable and easily degraded under oxygen and ultraviolet radiation. Furthermore, they are mixed with a large amount of volatile substances in forest air (such as α-pinene, β-pinene, limonene, myrcene, and terpinene), making direct qualitative and quantitative detection very difficult. Therefore, selective enrichment of pheromones in air samples is necessary.
[0020] Currently, the main methods for collecting ambient air samples include solution absorption sampling, adsorption tube sampling, filter membrane sampling, filter membrane-adsorbent combined sampling, direct sampling, and indirect sampling. Among these, adsorption tube sampling is widely used due to its portability and ease of operation. Adsorption tubes are ordinary glass tubes, quartz tubes, or stainless steel tubes filled with various adsorbents. The adsorption performance and selectivity of the adsorbent packing material determine the gas collection effect. Common solid adsorbents include activated carbon, silica gel, graphitized carbon black (Carbonpack series), carbon molecular sieves (Carboxen series), and porous organic polymers such as Tenax-TA and DVB. Previous studies have often directly used traditional commercial adsorbents to enrich insect pheromones, but these adsorbents often suffer from poor selectivity and slow adsorption rates due to the lack of specific functional groups. For example, although Tenax packing material is widely used for pheromone enrichment, after evacuating air at a flow rate of 17 L / min for 4 hours, its recovery efficiency for E8,E10-dodecadien-1-ylacetate was only 47%. Furthermore, research by Sergio et al. showed that Tenax TA had a recovery rate of less than 5% for α-pinene, and neither activated carbon nor silica gel could effectively adsorb α-pinene. Only Porapak Q and Porapak Rxn RP achieved a recovery rate of over 50% for α-pinene. Therefore, it is necessary to design adsorbent materials specifically for the insect pheromones that need to be enriched to achieve efficient pheromone enrichment.
[0021] Ionic liquids are special salts composed of cations and anions at room temperature and near-room temperature. They are a novel type of organic solvent and a functional material with designable structural properties. By designing suitable ionic liquids based on the structural differences between target pheromones and background gas molecules, a new option for enriching insect pheromones in the air can be provided. The application of ionic liquids also simplifies complex pretreatment processes.
[0022] Based on the application technology of ionic liquids, this invention provides a gas chromatography detection method for enriching airborne insect aggregation pheromones with ionic liquid composite materials, in order to solve the above-mentioned existing technical problems. In order to enable those skilled in the art to better understand the technical solution of this invention and implement it, the technical solution of this invention will be clearly and thoroughly described below with reference to the accompanying drawings.
[0023] In the description of this invention, it should be understood that the experimental and detection methods described in the following embodiments are conventional methods unless otherwise specified; and the reagents and materials described are commercially available unless otherwise specified.
[0024] Example 1 A gas chromatography detection method for enriching airborne insect aggregation pheromones with an ionic liquid composite material includes the following steps: 1. Preparation of enrichment tubes Taking 1-butyl-3-methylimidazolium tetrafluoroboric acid as an example, enrichment tube A was prepared. First, 0.2 g of ionic liquid was weighed and then dissolved in 20 mL of methanol solution as an impregnation solution. Then, 1 g of activated carbon was added, and the mixture was impregnated at room temperature for 24 h, rotary evaporated at 50 ℃ for 10 min, and vacuum dried at 80 ℃ for 8 h to obtain the ionic liquid composite material. 200 mg of the ionic liquid composite material was weighed and filled into an empty tube with an inner diameter of 6 mm and a length of 89 mm. Both ends were fixed with glass wool and an 80-mesh sieve. The filled enrichment tube was activated at 300 ℃. Nitrogen was used as the carrier gas and activated at a flow rate of 100 mL / min for 2 h to remove impurities. After activation, the temperature of the enrichment tube was reduced to below 30 ℃ under continuous nitrogen flow. The tube was then removed, sealed at both ends with rubber sleeves, and placed in a desiccator for later use.
[0025] Ethanolamine hexafluorophosphate was used as an example to prepare enrichment tube B. First, 0.2 g of ionic liquid was weighed and dissolved in 20 mL of methanol solution as an impregnation solution. Then, 1 g of activated carbon was added, and the mixture was impregnated at room temperature for 24 h. The mixture was then rotary evaporated at 50 °C for 10 min and vacuum dried at 80 °C for 8 h to obtain the ionic liquid composite material. 200 mg of the ionic liquid composite material was weighed and filled into an empty tube with an inner diameter of 6 mm and a length of 89 mm. Both ends were fixed with glass wool and an 80-mesh sieve. The filled enrichment tube was activated at 300 °C. Nitrogen was used as the carrier gas, and activation was carried out at a flow rate of 100 mL / min for 2 h to remove impurities. After activation, the temperature of the enrichment tube was lowered to below 30 °C under continuous nitrogen flow. The tube was then removed, sealed at both ends with rubber sleeves, and placed in a desiccator for later use.
[0026] 2. Establishment of analytical methods 2.1 Establishment of Gas Chromatography Conditions The DB-5MS column was used as the stationary phase; nitrogen was used as the carrier gas; the injection port was in pressure control mode and set to 100 kPa; the initial column temperature was 31 °C, increased to 100 °C at a rate of 10 °C / min, then increased to 150 °C at a rate of 5 °C / min and held for 1 min; the injector temperature was 200 °C; a flame ionization detector (FID) was used at a temperature of 250 °C; and the initial split ratio was 10:1.
[0027] 2.2 Establishment of thermal desorption conditions The desorption mode is a two-stage process using nitrogen as the desorption gas. The first stage involves desorption through an enrichment tube at a temperature of 230℃ to 280℃, a desorption time of 5 to 15 minutes, and a desorption flow rate of 100 mL / min to 200 mL / min. The cold trap temperature is -30℃ to 0℃. The second stage involves desorption through a cold trap at a temperature of 250℃ to 300℃, a desorption time of 1 to 5 minutes, a pre-trap split ratio of 0 to 3, and a post-trap split ratio of 0 to 3. The six-way valve temperature and the transmission line temperature are both 230℃ to 280℃.
[0028] 3. Preparation of standard solutions Accurately weigh 0.1 g each of myrtol, verbenatone, 2-methyl-3-vinyl-2-ol (MB), α-pinene, β-pinene, limonene, terpinene, and 3-carene, and dilute to 50 mL in a volumetric flask with methanol to prepare a stock solution with a concentration of 2 mg / mL. Using methanol as the solvent, serially dilute the above stock solution to prepare a series of standard mixed solutions with concentrations of 1 μg / mL, 5 μg / mL, 10 μg / mL, 20 μg / mL, 50 μg / mL, and 100 μg / mL, and store them in a refrigerator at -20 ℃ for later use.
[0029] Example 1 The determination of insect aggregation pheromone content in a sampling column using gas chromatography includes the following steps: Using a microsyringe, different concentration ranges of mixed standard solutions of a predetermined mass were injected into the prepared enrichment tubes. The concentration range of the mixed standard solutions was 0.005 mg / mL to 1 mg / mL. The enrichment tubes were placed in a thermal desorption instrument for desorption, and then introduced into a gas chromatograph to generate response peaks. The different masses of insect aggregation pheromones were linearly fitted with their corresponding response peaks to obtain standard working curves.
[0030] The sampling column was placed in a thermal desorption instrument for desorption, and then introduced into a gas chromatograph to obtain the response peak. The response peak of each insect aggregation pheromone was substituted into the corresponding standard working curve, and linear regression was performed to obtain the mass of the insect aggregation pheromone. The content of the insect aggregation pheromone was obtained by dividing the mass of the insect aggregation pheromone by the volume of the collected gas.
[0031] In the actual experiment, 1 μL of mixed standard solutions with concentrations of 1 μg / mL, 5 μg / mL, 10 μg / mL, 20 μg / mL, 50 μg / mL, and 100 μg / mL were accurately pipetted into enrichment tube A using a microsyringe. The solutions were then measured under thermal desorption and gas chromatography conditions. A standard working curve was plotted with concentration as the abscissa and peak area as the ordinate.
[0032] The linear equations are shown in Table 1 below. The linear correlation coefficients of the standard working curves of the eight substances are all greater than 0.99, indicating good linear correlation.
[0033] Table 1. Linear equations, correlation coefficients, and detection limits of eight substances in enrichment tube A. Example 2 Accurately pipette 1 μL of mixed standard solutions with concentrations of 1 μg / mL, 5 μg / mL, 10 μg / mL, 20 μg / mL, 50 μg / mL, and 100 μg / mL into enrichment tube B using a microsyringe. Determination is performed under thermal desorption and gas chromatography conditions. Working curves are plotted with concentration on the x-axis and peak area on the y-axis. The linear equations are shown in Table 2 below. The linear correlation coefficients of the eight standard curves are all greater than 0.99, indicating good linear correlation.
[0034] Table 2. Linear equations, correlation coefficients, and detection limits of eight substances in enrichment tube B. Example 3 Standard solutions with concentrations of 5 μg / mL, 10 μg / mL, and 20 μg / mL were used to perform precision and recovery experiments using enrichment tubes A and B. The precision and recovery results are shown in Table 3 below. The precision of this method ranges from 2.7% to 9.1%, and the recovery rate ranges from 90.12% to 112.85%, meeting the requirements for precision and accuracy.
[0035] Table 3. Precision and recovery of the three spiked samples Comparative Example Using the above method, samples were collected for 100 min at a rate of 0.1 L / min in laboratory environment A, simulated gas environment B, and pine forest environment C, respectively. The 1-methyl-3-butylimidazolium tetrafluoroborate enrichment tube α and commercial activated carbon enrichment tube β prepared by the above method were used.
[0036] Specifically, simulated gas B includes myrtol, verbenaone, and 2-methyl-3-vinyl-2-ol at a concentration of 5 ppm, and α-pinene, β-pinene, limonene, terpinene, and 3-carene at a concentration of 50 ppm.
[0037] Specifically, pine forest environment C contains volatile pine substances.
[0038] After sampling, the sampling column was placed in the thermal desorption instrument and thermal desorption-gas chromatography analysis was performed according to the established method. The contents of the target gas in different environments were measured as shown in Table 4.
[0039] Table 4. Detection results of actual samples It is evident that the target gas content measured using commercial activated carbon enrichment tubes is lower than that measured using ionic liquid composite materials as enrichment tubes, indicating that the ionic liquid composite materials have a better enrichment effect.
[0040] Compared with existing technologies, the present invention provides a gas chromatography detection method for enriching airborne insect aggregation pheromones using an ionic liquid composite material. The method utilizes an ionic liquid methanol solution as an impregnating liquid, adds an adsorbent carrier, and then treats the mixture to obtain an ionic liquid composite material. The ionic liquid composite material is used as an adsorbent to form an enrichment tube, which is activated using nitrogen as a carrier gas. One end of the activated enrichment tube is connected to a sampling pump for gas sample sampling. After sampling, a sampling column is obtained. The sampling column is then thermally desorbed, and the content of insect aggregation pheromones in the sampling column is determined by gas chromatography. This invention utilizes the structural properties of ionic liquids to design and prepare ionic liquid composite materials as adsorbents. Based on the structural differences between target pheromone molecules and background gas molecules, an ionic liquid with strong selective interactions with the target is designed to enhance the selective enrichment of insect pheromones. This achieves selective enrichment of extremely low concentrations of target insect aggregation pheromones with good enrichment effect. The operation steps are simple, the adsorbent can be reused, and desorption is achieved by heating to destroy the interactions. This solves the problem of efficient enrichment of trace pheromone molecules, enabling qualitative and quantitative detection of trace insect pheromones in the air. It is highly practical and worthy of promotion.
[0041] The above-disclosed embodiments are merely preferred embodiments of the present invention. However, the embodiments of the present invention are not limited thereto, and any variations that can be conceived by those skilled in the art should fall within the protection scope of the present invention.
Claims
1. A method for the detection of insect aggregation pheromones in air by gas chromatography using an ionic liquid composite, characterized in that, The method comprises the following steps: The ion liquid methanol solution is taken as the impregnation solution, the adsorption carrier is added, and impregnation is carried out at room temperature; after methanol is removed by rotary evaporation, drying is carried out to obtain an ion liquid composite material; wherein the ion liquid methanol solution comprises a cation and an anion; the cation is at least one of ethanolamine, ethylamine, 1-butyl-3-methylimidazole, 1-hexyl-3-methylimidazole, 1-octyl-3-methylimidazole and tetramethylguanidine; and the anion is at least one of tetrafluoroborate, hexafluorophosphate, acetate and bistrifluoromethanesulfonylimide; The ion liquid composite material is taken as an adsorbent, and nitrogen is taken as a carrier gas to activate and remove impurities from the adsorbent; The activated adsorbent is used for gas sample sampling to obtain a sampling column; Thermal desorption is carried out on the sampling column, and gas chromatography is used to determine the content of insect aggregation pheromone in the sampling column.
2. The gas chromatography detection method for enriching airborne insect aggregation pheromones with ionic liquid composite materials according to claim 1, characterized in that, The adsorption carrier is at least one of a high-molecular organic polymer, an inorganic adsorption material, a carbon-based adsorption material and a nanofiber material.
3. The gas chromatography detection method for enriching airborne insect aggregation pheromones with ionic liquid composite materials according to claim 1, characterized in that, The concentration of the ion liquid methanol solution is 5 mg / mL to 25 mg / mL; the ion liquid methanol solution is impregnated with the adsorption carrier at room temperature for 24 h to 48 h; after methanol is removed by rotary evaporation, vacuum drying is carried out at a temperature of 60 ℃ to 80 ℃ for 8 h to 12 h.
4. The method of claim 1, wherein the ion liquid composite is used for the detection of gaseous phase chromatography of insect aggregation pheromones in the air. The ion liquid composite material is taken as an adsorbent, and nitrogen is taken as a carrier gas to activate and remove impurities from the adsorbent, which comprises the following steps: The ion liquid composite material is filled into an empty tube, and the two ends of the empty tube are respectively packaged with glass wool and a 80-mesh to 100-mesh sieve sheet to form an enrichment tube; The enrichment tube is activated at a temperature of 250 ℃ to 300 ℃ with nitrogen as a carrier gas at a flow rate of 100 mL / min to 150 mL / min for 2 h to 4 h to remove impurities; After the activation is completed, the temperature of the enrichment tube is lowered to room temperature without interruption of the nitrogen gas flow, and then the enrichment tube is taken out.
5. The method of claim 4, wherein the ion liquid composite is used for the detection of gaseous phase chromatography of insect aggregation pheromones in the air. The gas sample sampling comprises the following steps: One end of the activated enrichment tube is connected to a sampling pump, and gas sample sampling is carried out at a rate of 0.1 L / min to 1 L / min for 1 min to 60 min; after the sampling is completed, a sampling column is obtained, and the two ends of the sampling column are sealed for standby use.
6. The method of claim 5, wherein the ion liquid composite is used for the gas chromatography detection of insect aggregation pheromones in the air. Thermal desorption is carried out in a two-stage desorption mode, and nitrogen is used as a desorption gas; the first-stage desorption is carried out on the enrichment tube, the desorption temperature is 230 ℃ to 280 ℃, the desorption time is 5 min to 15 min, the desorption flow rate is 100 mL / min to 200 mL / min, the cold trap capture temperature is -30 ℃ to 0 ℃, the second-stage desorption is carried out on the cold trap, the desorption temperature is 250 ℃ to 300 ℃, the desorption time is 1 min to 5 min, the pre-trap split ratio is 0 to 3, and the post-trap split ratio is 0 to 3.
7. The method of claim 6, wherein the ion liquid composite is used for the gas chromatography detection of insect aggregation pheromones in the air. When the content of insect aggregation pheromone in the sampling column is determined by gas chromatography, a DB-5MS chromatographic column is used; nitrogen is used as a carrier gas, the inlet is in pressure control mode and is set to 100 kPa; the initial column temperature is 31 ℃, which is increased to 100 ℃ at a rate of 10 ℃ / min, then increased to 150 ℃ at a rate of 5 ℃ / min and maintained for 1 min; the temperature of the sample injector is 200 ℃; An FID detector is used, and the temperature is 250 ℃; the initial split ratio is 10:
1.
8. The method of claim 7, wherein the ion liquid composite is used for the gas chromatography detection of insect aggregation pheromones in the air. The content of the insect aggregation pheromone in the sampling column is determined by gas chromatography, including the following steps: A standard working curve of each insect aggregation pheromone is determined; The sampling column is placed in a thermal desorption instrument for desorption, and then enters a gas chromatograph to obtain a response peak value; the response peak value of each insect aggregation pheromone is substituted into the corresponding standard working curve, and the mass of the insect aggregation pheromone is obtained by linear regression; and the content of the insect aggregation pheromone is obtained by dividing the mass of the insect aggregation pheromone by the volume of the collected gas.
9. The method of claim 8, wherein the ion liquid composite is used for the gas chromatography detection of insect aggregation pheromones in the air. The method for determining the standard working curve of each insect aggregation pheromone comprises the following steps: Different concentrations of mixed standard solutions with a preset mass are respectively sucked by a microsyringe, and then injected into a prepared enrichment tube; the enrichment tube is placed in a thermal desorption instrument for desorption, and then enters a gas chromatograph to generate a response peak value; and the mass of different insect aggregation pheromones is respectively linearly fitted with the corresponding response peak value to obtain a standard working curve.
10. The method of claim 9, wherein the ion liquid composite is used for the gas chromatography detection of insect aggregation pheromones in the air. The concentration of the mixed standard solution is 0.005 mg / mL to 1 mg / mL.