57 results about "Solid-phase microextraction" patented technology

The invention discloses a solid-phase microextraction derived fiber head and a preparation method and application thereof, the solid-phase microextraction derived fiber head comprises a solid-phase matrix and polystyrene microspheres adhered to the surface of the solid-phase matrix, and a chitosan cross-linked network layer is also cross-linked on the polystyrene microspheres; cysteine is also adsorbed on the polypropylene microsphere and chitosan cross-linked network layer. According to the solid-phase microextraction derivative fiber head, a large number of hydrophilic action sites such as amino groups and carboxyl groups exist on the surface, so that synchronous extraction and detection of the contents of three target analytes, namely cysteine-chlorothalonil association compounds, sulfydryl chlorothalonil and hydroxychlorothalonil, are realized.

The invention belongs to the field of chemical detection, and particularly relates to a method for detecting ethylene oxide, 2-chloroethanol and acetaldehyde in a frozen beverage by solid-phase microextraction gas chromatography-mass spectrometry. The invention relates to a method for detecting ethylene oxide, 2-chloroethanol and acetaldehyde in a frozen beverage by solid-phase microextraction gas chromatography-mass spectrometry, which comprises the following steps: S.1) taking a frozen beverage sample to be detected, homogenizing and uniformly mixing; s.2) weighing a certain amount of sample, and adding sodium chloride and hydrochloric acid; s.3) determining the sample by adopting a solid-phase microextraction gas chromatography-mass spectrometry method; and S.4) quantitatively analyzing the contents of ethylene oxide, 2-chloroethanol and acetaldehyde in the frozen drink sample to be detected by adopting an external standard method. According to the method disclosed by the invention, the derivatization reaction and the solid-phase microextraction process are combined into one, and the difficulties of complicated pretreatment, long time consumption, low accuracy, unstable result, high detection limit and the like in the traditional analysis technology are overcome. Meanwhile, the precision of a detection result is high, the influence of a complex matrix is removed, and the reproducibility is good.

This invention discloses a surface coating material, a solid-phase microextraction probe, its preparation method, and its application, relating to the field of veterinary drug detection technology. The probe comprises a metal rod and a coating applied to the outer surface of the metal rod. The surface coating material is prepared by electrospinning a mixture of SBA-15 material, polyacrylonitrile, and N,N-dimethylformamide. The ratio of SBA-15 material, polyacrylonitrile, and N,N-dimethylformamide is 100mg–300mg: 100mg–300mg: 2mL–4mL. This invention addresses the problems of inconvenient equipment portability and long detection times in existing technologies.

The application discloses a preparation method of zinc oxide nanoflower fibers and application thereof. The preparation method comprises the following steps: cleaning and acid treating a nickel-chromium alloy wire base; preparing a zinc oxide seed layer on the surface of the nickel-chromium alloy wire base through an immersion-calcination method; and growing zinc oxide nanoflowers on the seed layer in situ through a hydrothermal method to obtain the zinc oxide nanoflower fibers. The fiber has the nickel-chromium alloy wire as the base, is good in flexibility and high in strength, has a firm combination of the zinc oxide nanoflower coating on the surface, is large in specific surface area, has rich active sites, and exhibits excellent selective adsorption capacity to polycyclic aromatic hydrocarbons. The application also provides application of the fiber in solid-phase microextraction, in particular, application of the fiber in enrichment and detection of trace polycyclic aromatic hydrocarbons in environmental water samples. The fiber is used for solid-phase microextraction of polycyclic aromatic hydrocarbons and detection of trace polycyclic aromatic hydrocarbons in environmental water samples, is low in detection limit, is good in reproducibility, is suitable for environmental water monitoring, and has important practical application value.

The present application relates to the technical field of Fischer-Tropsch synthesis wax analysis chemistry, and in particular to a method for detecting oxygen-containing compound components in Fischer-Tropsch synthesis wax by using solid-phase microextraction and comprehensive two-dimensional gas chromatography-mass spectrometry. The method comprises the following steps: first, performing solid-phase microextraction on a to-be-tested wax sample to obtain an extract rich in oxygen-containing compound components; and then using comprehensive two-dimensional gas chromatography-mass spectrometry to qualitatively determine the composition of the oxygen-containing compound components contained in the extract. In the method, the content of the oxygen-containing compound components is less than or equal to 7 wt% based on the total weight of the Fischer-Tropsch synthesis wax. The method has the characteristics of high throughput, high sensitivity and high accuracy, and solves the problems of difficult analysis and separation and difficult qualitative determination of alcohol, aldehyde, ketone, acid, ester and other oxygen-containing compound components in Fischer-Tropsch synthesis wax.

The application discloses a kind of phosphoric acid group modified β-cyclodextrin-based polymer film microextraction coating material and its application.First, a kind of phosphoric acid group β-CD porous crosslinked polymer (DBP-β-BNCD) and its preparation method are provided.The DBP-β-BNCD has the advantages of large specific surface area, narrow pore size distribution, large pore volume, good thermal stability, etc., which is beneficial to the accessibility of adsorption sites.When adsorbing hydrophilic pollutants antibiotics, various adsorption mechanisms such as polarity interaction, hydrogen bond interaction and π-π interaction are introduced.Further, by using DBP-β-BNCD as a thin film solid phase microextraction coating material, a method combining TFME with high performance liquid chromatography-tandem mass spectrometry (HPLC-QqQ-MS) is established, and the results show that the coating material has great potential for the extraction of hydrophilic organic pollutants in the environment.

The invention belongs to the technical field of antibiotic residue detection, and particularly relates to a rapid detection method for quinolone antibiotics in dairy products. The preparation method comprises the following steps: preparing gold nanoparticles as gold seeds by using a sodium citrate reduction method, epitaxially growing an ultrathin Cr-MIL-101-NH2 shell layer by using a layer-by-layer self-assembly method, and constructing an Au-coated Cr-MIL-101-NH2 NPs core-shell structure; a solid phase microextraction-surface enhanced Raman spectroscopy (SPME-SERS) combined method is established on the basis of the material, a shell layer is used for efficiently extracting and selectively enriching a target object to a gold nanoparticle local plasma resonance area, strong SERS signal enhancement is achieved, and the shell layer guarantees that the gold nanoparticles are stable in performance in a complex matrix at the same time. Methodology verification proves that the method is wide in linear range, good in precision, high in recovery rate, low in detection limit, convenient in pretreatment and suitable for rapid high-throughput detection of antibiotic residues in food.

This invention discloses a method for preparing a solid-phase microextraction (SPME) device coated with a porous carbon material (DPCM) derived from a covalent organic framework (COF). The method primarily includes the following steps: preparing DPCM; preparing a DPCM sol-gel solution; inserting treated fibers into the DPCM sol-gel solution, extracting and curing them, and repeating this process multiple times to produce a DPCM-coated fiber. This fiber is then secured in a 1 mL microsyringe to form a solid-phase microextraction device. Combined with gas chromatography, the device is used for the extraction and analysis of trace phthalates (PAEs) in water samples, significantly improving detection sensitivity.

The application relates to a preparation method of a solid-phase microextraction coating, comprising the following steps: (1) dissolving a metal organic framework material MIL-101Cr as an adsorbent and a binder in a solvent to prepare a suspension; (2) uniformly mixing and ultrasonically treating the suspension, then inserting a stainless steel substrate into the suspension and slowly taking out the substrate, so that a coating is coated on the substrate, and the process is repeated for several times until the coating on the substrate reaches a required thickness. Compared with commonly used commercial solid-phase microextraction heads, the solid-phase microextraction fiber coating for sample pretreatment has better extraction effect than a two-in-one extraction head and is equivalent to a three-in-one extraction head, and the prepared solid-phase microextraction fiber coating has a long service life and can be repeatedly used for 160 times.

The application discloses application of a zwitterionic covalent organic framework solid-phase microextraction fiber in neurotransmitter analysis, wherein the zwitterionic covalent organic framework material is prepared by Schiff base reaction condensation with ethidium bromide, 2,5-diaminobenzoic acid and triformylphloroglucin as functional monomers and acetic acid as a catalyst to obtain the zwitterionic covalent organic framework material. The coating of the zwitterionic covalent organic framework solid-phase microextraction fiber prepared in the application has good hydrophilicity, and the structure is rich in functional groups such as hydroxyl groups, carboxyl groups, phenyl groups and quaternary ammonium groups, which can interact with target analytes through ion exchange, pi-pi stacking, hydrogen bonding and hydrophilic-hydrophobic interaction, thereby showing strong specific adsorption and high enrichment capacity for neurotransmitters. The zwitterionic covalent organic framework solid-phase microextraction fiber prepared in the application realizes efficient enrichment and extraction analysis of neurotransmitters with different polarities in complex biological sample matrices.

The utility model provides a special fixing device for gas phase / gas chromatography-mass spectrometry solid phase microextraction, which relates to the technical field of laboratory devices and comprises an extraction component, a sample bottle clamping component and a solid phase microextraction clamping component are arranged on the extraction component, and the extraction component comprises a base. The solid-phase microextraction clamping assembly comprises a mounting plate and a fastening bolt. According to the utility model, the air cylinder is controlled to extend synchronously, so that the clamping plate is pushed to move, the solid-phase microextraction parts are limited by the clamping plate, the solid-phase microextraction parts with different sizes can be effectively fixed, the practicability and the flexibility are improved, and after the solid-phase microextraction parts are clamped and fixed by the clamping plate, the solid-phase microextraction parts are clamped and fixed by the clamping plate. The limiting plates penetrate through the interiors of the single clamping plates, the springs are stressed and compressed by pulling the limiting rods upwards, after the clamping plates clamp and fix the solid-phase microextraction part, the limiting rods are loosened, the limiting rods penetrate through the interiors of the single limiting grooves through the elasticity of the springs, and limiting is facilitated.

The invention discloses a preparation method and application of a carboxyl functionalized MON (at) ZIF-8-NH2 solid phase microextraction material. The preparation method comprises the following steps: taking ZIF-8-NH2 as an inner core and MON-2COOH as a shell to obtain a carboxyl-functionalized MON-coated ZIF-8-NH2 material, then fixing the carboxyl-functionalized MON-coated ZIF-8-NH2 material on a substrate by adopting a physical coating technology to obtain a solid-phase micro-extraction coating fiber based on carboxyl-functionalized MON-coated ZIF-8-NH2, and using the extraction fiber to measure hydroxyl polycyclic aromatic hydrocarbon in urine. The solid-phase micro-extraction coating fiber disclosed by the invention is thinner in coating, better in extraction effect, longer in service life and higher in stability. The method can be used for extracting various hydroxyl polycyclic aromatic hydrocarbons in urine at the same time by being combined with liquid chromatography-mass spectrometry, and has good stability, meanwhile, the determination method has excellent accuracy, and the recovery rate and the detection limit meet the detection requirements of trace analysis.

The invention relates to the technical field of food analytical chemistry, and particularly discloses a method for analyzing volatile components in rice, which comprises the following steps: S1, aging a fiber head: aging a solid phase microextraction fiber head at a gas chromatography sample inlet at 270 DEG C for 30 minutes; s2, sample preparation: weighing 3g of a rice sample, putting the rice sample into a headspace sample injection bottle, adding 6mL of water, and sealing the headspace sample injection bottle; s3, headspace balancing: stirring and balancing the sealed sample injection bottle at the temperature of 80 DEG C at the speed of 250 rpm; s4, headspace extraction: placing the aged fiber head at a position 3 cm above the headspace of the sample, and carrying out adsorption extraction for 30 minutes; s5, thermal desorption: inserting the extracted fiber head into a GC-MS (Gas Chromatography-Mass Spectrometer) sample inlet, and desorbing for 6 minutes at 230 DEG C; and S6, performing chromatographic analysis on the desorbed sample. The method is simple, convenient and rapid to operate, capable of completing large-scale detection in a short time and wide in application range.

The application discloses preparation of silver nanocluster functionalized monolithic column and selective solid phase microextraction application thereof. The application takes urea and formaldehyde as matrix monomers, takes glutathione or p-aminobenzenesulfonic acid as functionalization-reaction catalysis bifunctional agent, and prepares glutathione functionalized monolithic column or p-aminobenzenesulfonic acid functionalized monolithic column through one-step polycondensation. Then, the multiple interactions between glutathione or p-aminobenzenesulfonic acid and silver ions are utilized to reduce and fix silver nanoclusters in situ on the surface of the monolithic column, so that the silver nanocluster functionalized monolithic column is prepared. The application provides a new way of combining cluster materials with monolithic columns, and the prepared monolithic column can be used as an in-tube solid phase microextraction stationary phase to realize online selective enrichment and high-sensitivity analysis of trace trans fatty acids in complex samples. The application has the advantages of ingenious process, simple operation, no need of expensive instruments, easiness in popularization and strong specificity of analysis objects.

The invention provides a method for detecting geranyl pyrophosphoric acid in water by headspace solid-phase microextraction / gas chromatography-mass spectrometry, which utilizes the characteristic that geranyl pyrophosphoric acid is easy to decompose into linalool under an acidic condition, adsorbs linalool by headspace solid-phase microextraction, and indirectly quantifies geranyl pyrophosphoric acid in combination with a gas chromatography-mass spectrometry technology. The method is easy to operate, low in instrument cost, high in sensitivity and suitable for detecting geranyl pyrophosphoric acid in water bodies such as source water, the generation risk of 2-methylisoborneol can be pre-judged through the content of geranyl pyrophosphoric acid, and technical support is provided for water supply safety.

The invention discloses a high polymer material radiolysis micromolecule product detection method which comprises the following steps: S1, filling a high polymer material into a solid phase microextraction device to form a negative pressure state; s2, performing gamma ray irradiation on the solid-phase microextraction device; s3, solid-phase microextraction fibers in the solid-phase microextraction device are taken out, and radiolysis micromolecule products adsorbed on the solid-phase microextraction fibers are analyzed through a gas chromatography-mass spectrometer; and S4, analyzing and determining the chemical structure of the radiolysis small molecule product, establishing a quantitative working curve between the peak area and the concentration of the standard product by combining the standard product, and calculating to obtain the content of the radiolysis small molecule product of the high polymer material under the radiation dose. According to the invention, solid-phase microextraction is combined with gas chromatography-mass spectrometry to analyze small molecular substances after high polymer materials such as rubber, resin and the like are irradiated, so that the ray irradiation resistance of the high polymer materials is evaluated; by combining qualitative and quantitative analysis methods, the content of micromolecular products of the high polymer material under different radiation doses can be obtained.

The invention belongs to the technical field of analysis and detection, and particularly relates to a method for screening volatile and semi-volatile odor markers in raw and auxiliary materials of paper printed matters. The data obtained by the headspace solid-phase microextraction gas chromatography / mass spectrometry is qualitatively analyzed on the basis of a triple confirmation mechanism constructed by a deconvolution method, a matching degree method and a retention index method, and the problem of inaccurate qualitative analysis in a complex matrix is solved. In the semi-quantitative analysis, compounds with different polarities are used as internal standard substances, and a calibration strategy is optimized according to the polarity difference of a target object, so that the reliability of an analysis result is improved. In addition, the components of the odor activity values are subjected to intersection analysis to screen out key odor markers. According to the model, the risk of misjudgment of high-concentration low-threshold substances in a traditional method is avoided by quantifying the contribution degree of a single component to the overall smell.

The invention discloses a bifunctional triazine covalent organic framework material, a solid-phase microextraction probe and application, and the bifunctional triazine covalent organic framework material is prepared from 2, 4, 6-tri (4-formyl-biphenyl-4-yl)-1, 3, 5-triazine, 5 '-(4-amino-3, 5-difluorophenyl)-3, 3', 5, 5 '-tetrafluoro-[1, 1': 3 ', 1'-triphenyl]-4, 4, 6-triazine-1, 3, 5-triazine-1, 3, 5 '-tetrafluoro-[1, 1': 3 ', 1'-triphenyl]-1, 3, 5 '-tetrafluoro-[1, 1': 3 ', 1 ''-triphenyl]-4, 4, 6-triazine-1, 3, 5]- The polymer is formed by polymerizing three monomers, namely 1, 4 ', 4'-diamine and diethyl phosphite. The TFP-COF disclosed by the invention is a porous material containing aromatic rings, fluorine atoms and nitrogen heteroatoms, and has a relatively large conjugated system and a plurality of recognition sites; the hydrophilicity and hydrophobicity of the COFs are adjusted through functionalization of the diethyl phosphite, the hydrophilicity is enhanced, the adsorption performance of the TFP-COF on medium and strong polarity analytes is enhanced, and then high-precision detection of the mycotoxins in a wide polarity range is achieved.

The utility model discloses a multichannel solid-phase microextraction device adaptable to sample bottles of various specifications, which relates to the technical field of solid-phase microextraction, and comprises an instrument body and an adapter, and the top surface of the instrument body is provided with an extraction hole site; the top end of the adapter is provided with a positioning groove matched with the probe handle; the bottom end of the adapter is provided with a mounting groove matched with the bottle cap of the sample bottle, and the adapter is provided with a fixing piece for fixing the bottle cap of the sample bottle; the adapter is provided with a probe channel, and the probe channel extends from the positioning groove to the installation groove. When in use, the height of the small-diameter sample bottle is increased by the adapter, so that the small-diameter sample bottle can be conveniently taken out from the sample bottle, and the instrument body is adaptive to the technical processing of sample bottles of various specifications.

The invention relates to a prediction model for the suitable storage period of cigarette box skins based on the volatile component loss characteristic and application thereof.The construction method comprises the steps that a to-be-detected sample is put into a headspace bottle to be subjected to solid-phase microextraction, and the content of volatile components is obtained through a gas chromatography-mass spectrometry detection method; and calculating the relative retention rate of the volatile component, substituting the relative retention rate into the diffusion empirical equation, and selecting the diffusion empirical equation with the maximum R2 as a prediction model. According to the method, a volatile component loss kinetic model is established for a box skin packaging material with peculiar smell, smell evaluation of the peculiar smell of the box skin is combined, and the optimal storage period of the cigarette box skin material in a specific storage environment before the cigarette box skin material is used on a machine is calculated and predicted through a kinetic equation.

The application discloses a kind of covalent organic framework material solid-phase microextraction fiber and its application in alkaloid metabolism and neurotransmitter analysis.The covalent organic framework material (COFs) includes the repeating structural unit of 4,4',4"-(1,3,5-triazine-2,4,6-triazyl) tri[benzaldehyde] connected by imine bond, ethidium bromide and 2,5-diaminobenzenesulfonic acid.The COFs material is used as the adsorbent of solid-phase microextraction fiber surface coating, and the COFs is coated on the surface of stainless steel fiber by polyacrylonitrile glue.The COFs solid-phase microextraction fiber of the application can be used to extract rhizoma coptidis alkaloids and neurotransmitters in the brain and blood of living rats, and after sampling extraction, it is directly combined with LC-MS / MS for mass spectrometry analysis, with very high sensitivity, and can be used for rapid, accurate and sensitive analysis of trace rhizoma coptidis alkaloid metabolites and neurotransmitters in vivo.

The application discloses a detection method for detecting drug amount based on solid phase microextraction and real-time analysis mass spectrum, which comprises the following steps: preparing a solid phase microextraction head by using a coating material, preparing a standard sample to form a standard curve solution, detecting the standard curve solution by solid phase microextraction and real-time direct analysis mass spectrum, obtaining a mass spectrum diagram of the standard curve solution, and then obtaining a standard curve equation of the standard curve solution; obtaining a peak area value of a to-be-detected sample by solid phase microextraction and real-time direct analysis mass spectrum, and substituting the peak area value into the standard curve equation to obtain the concentration of corresponding drugs. By setting the method process, the detection steps of the application are obviously simplified, the constant volume, detection and calculation operations can be carried out on site according to actual needs, the operation mode and operation site are flexible, and the beneficial effect of improving the detection efficiency can be achieved.

The invention belongs to the technical field of food detection, and particularly relates to a solid-phase microextraction probe based on a COF (co) copolymer microsphere / MXene coating as well as a preparation method and application of the solid-phase microextraction probe. The preparation method comprises the following steps: carrying out amination treatment on a support carrier to obtain an aminated support carrier; the preparation method comprises the following steps: preparing an aminated support carrier, then loading a reaction monomer and a polymer skeleton on the surface of the aminated support carrier, then adding 2, 6-dialdehyde-1, 5-dihydroxynaphthalene (DHNDA), MXene and glacial acetic acid for in-situ assembly to obtain the solid-phase microextraction probe, and improving the extraction efficiency of the probe on an organophosphorus pesticide through a COF (copolymerized microsphere / MXene coating. The high-selectivity and high-sensitivity detection on the organophosphorus pesticide in the tea leaf sample is realized.

The invention provides a fluorine-functionalized super-crosslinking material, a preparation method thereof and application of the fluorine-functionalized super-crosslinking material in cold-assisted solid-phase microextraction. The invention belongs to the technical field of headspace solid-phase microextraction. The fluorine-functionalized super-crosslinked coating is prepared by carrying out a reaction on C-methyl calix [4] hydrocarbon resorcinol, 4-(trifluoromethyl) benzyl bromide, ferric trichloride and dichloroethane in an oil bath at the temperature of 100 DEG C. The fluorine-functionalized super-crosslinking coating can be used for preparing a solid-phase micro-extraction fiber coating, and the solid-phase micro-extraction fiber coating can realize efficient adsorption of polychlorinated naphthalene through F-pi bonds, electrostatic adsorption and other acting forces. The invention further provides a self-made portable cold-assisted solid-phase microextraction device which can assist in extraction of high-boiling-point components in polychlorinated naphthalene. Compared with other solid-phase microextraction cold auxiliary devices, the solid-phase microextraction cold auxiliary device is simple in structure, convenient to operate and convenient to commercialize. The method has a wide application prospect in the aspects of environmental monitoring, food safety and the like.

This invention belongs to the field of component detection technology and discloses a method and application for the detection of octadecyl vinyl ether. Using ginseng prepared by co-fermentation of ginseng powder and bacterial enzymes as the sample, a three-step pretreatment method is employed: ethanol extraction combined with liquid-liquid extraction of a toluene:n-hexane mixture (5:1 volume ratio) and PDMS solid-phase microextraction. This is combined with gas chromatography-tandem mass spectrometry (GC-MS) to achieve qualitative and quantitative analysis of octadecyl vinyl ether. The three-step pretreatment method uses ethanol extraction combined with liquid-liquid extraction of a toluene:n-hexane mixture and PDMS solid-phase microextraction. The ethanol extractant is consistent with the solvent used in the preparation of fermented ginseng, ensuring sufficient dissolution of the target analyte. The toluene-n-hexane mixed solvent efficiently separates the target analyte from polar matrix impurities, and the boiling point difference facilitates subsequent solvent removal. PDMS solid-phase microextraction further enriches trace amounts of the target analyte. Compared with the reduced pressure concentration method, the detection sensitivity is improved by more than 2 times, and matrix interference is removed more thoroughly.

This invention discloses a method and apparatus for identifying modified recycled materials based on machine learning algorithms. The method includes: obtaining recycled plastics and virgin materials of the same type, mixing them in a certain proportion and melt-extruding them to obtain modified virgin material and modified recycled material samples; performing solid-phase microextraction and thermal desorption treatment on the two samples to obtain volatile component data; establishing and optimizing a model based on the data to obtain an identification model, which is then used to predict blind samples, and the category of the blind samples is determined by a result in which more than half of the samples are consistent. This invention proposes a method and apparatus for identifying modified recycled materials based on machine learning algorithms. By obtaining volatile component information data of modified virgin materials and modified recycled materials through extraction and thermal desorption treatment, it can provide a clear basis for identification. By establishing a model and determining the category of blind samples by a prediction result in which more than half of the samples are consistent, the accuracy of identification can be improved, and the problem of difficulty in efficiently and accurately identifying modified recycled materials and modified virgin materials of the same type of plastic can be solved.

The invention provides a rapid extraction and purification device for soil organic pollutants, and belongs to the technical field of soil analysis and detection. Comprising a soil crushing unit, a liquid phase extraction unit and a solid phase extraction unit for purifying extracted organic matters, according to the device, the organic pollutants are transferred into water or an organic phase through the liquid phase extraction unit, the organic pollutants are transferred into an organic solvent by directly utilizing portable gas chromatography, portable gas chromatography-mass spectrometry and other devices for sample introduction after being enriched through the solid phase microextraction sample introduction needle, and the solid phase extraction unit is utilized for on-site purification treatment. By means of the technical advantages of multi-mode extraction, efficient enrichment, on-site purification and portable combination, the defects that in traditional soil organic pollutant analysis, the process is tedious, consumed time is long, and dependence is made on a laboratory are overcome, and the method is particularly suitable for environment emergency, pollution investigation and field monitoring scenes.

The application provides a chlorine-functionalized covalent organic framework / graphene aerogel material, a preparation method and application thereof. The chlorine-functionalized covalent organic framework / graphene aerogel material is prepared by the following method: using an amino-containing silane reagent to modify graphene oxide under low-temperature conditions, then reducing the modified graphene oxide at high temperature, and freeze-drying to obtain amino-functionalized graphene aerogel; placing the amino-functionalized graphene aerogel in a solvent, sequentially adding chlorine-functionalized aldehyde ligands and amino ligands of a covalent organic framework, and through Schiff base reaction under catalysis of an acetic acid aqueous solution, a chlorine-functionalized covalent organic framework / graphene aerogel material is prepared. The chlorine-functionalized covalent organic framework / graphene aerogel material can be used to prepare a solid-phase microextraction fiber coating, and the obtained solid-phase microextraction fiber coating can be applied to efficient enrichment and sensitive detection of halogenated aromatic pollutants such as polychlorinated naphthalenes in environmental samples.

The present application relates to the field of analytical instrument, especially to a detection device and method for membrane-protected solid phase microextraction and ion chromatography. The device comprises a membrane-protected solid phase microextraction instrument and an ion chromatography instrument; the outer surface of the extraction head of the membrane-protected solid phase microextraction instrument is wrapped with a polypropylene porous membrane; the extraction head is inserted into a desorption cell for release after adsorbing a sample in a sample bottle; the ion chromatography instrument comprises a mobile phase delivery system, a six-way valve, a separation system, a monitoring and data processing system; the six-way valve is connected with the mobile phase delivery system, a liquid inlet pipeline, a waste liquid bottle and the separation system respectively; the separation system is connected with the monitoring and data processing system; one end of the desorption cell is connected with the mobile phase delivery system, and the other end is connected with a sample inlet pipeline; a sample inlet pump and a degassing box are arranged on the sample inlet pipeline. The present application realizes accurate monitoring of trace level anions such as F ‑ , Cl ‑ , SO4 2‑ in the primary coolant of a nuclear power plant.