27 results about "Solid-phase microextraction" patented technology

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 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.

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 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 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 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.

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 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.

The invention relates to a polydimethylsiloxane-reduced graphene oxide composite coating solid-phase extraction fiber as well as a preparation method and application thereof, and belongs to the technical field of sample pretreatment and trace analysis. Aiming at the problems of poor conductivity and insufficient coating stability of the traditional solid-phase microextraction fiber, a PDMS-rGO composite coating is constructed by a three-step method, graphene oxide is reduced by ascorbic acid and calcined to form a loose multi-layer structure, PDMS is loaded by a sol-gel method, and the coating fiber with the thickness of 40-60 microns and the conductivity of 30-35 k omega is obtained. In combination with an electrochemical enhanced solid-phase microextraction technology, the fiber is used for efficiently extracting amphetamine stimulants, and in combination with an online derivatization-gas chromatography-nitrogen and phosphorus detector, trace detection is realized. Experiments show that the composite coating has high affinity of PDMS and excellent conductivity of rGO, the thermal stability is improved to 800 DEG C or above, and the mechanical durability reaches 150 times of cyclic extraction. And a high-sensitivity solution is provided for rapid screening of amphetamine substances in a biological matrix.

A micro-syringe for inserting into a sample matrix. The micro-syringe includes a micro-syringe body having an orifice at an insertion end; and a plunger at least partially coated with a solid-phase micro-extraction (SPME) coating. The plunger is longitudinally movable between an internal position and an extended position. When the syringe is inserted into the sample matrix, the extraction phase is shielded from the sample matrix by the micro-syringe body when the plunger is in the internal position, and at least a portion of the extraction phase extends past the orifice and is exposed to the sample matrix when the plunger is in the extended position. The plunger is sized to fit the internal diameter of the micro-syringe body to draw a liquid into the micro-syringe body when the plunger is moved from the extended position to the internal position.

The utility model discloses a multifunctional sampling device which comprises a rack, a liquid tray and a quick release assembly, the rack is provided with a detection analyzer and a manipulator, the rack is provided with a cross beam, and the cross beam is provided with a sample preparation tray, a headspace heater and a solid-phase microextraction instrument; two connecting arms are arranged at one end of the liquid tray, and a mounting part is transversely arranged at the upper end of each connecting arm; the quick-release assembly comprises at least two inserting and pulling blocks, the inserting and pulling blocks are installed on the cross beam, inserting grooves are transversely formed in the inserting and pulling blocks, each inserting groove is provided with an upper groove wall, a lower groove wall, a left groove wall and a right groove wall, avoiding gaps are formed between the lower groove walls and the left groove walls, avoiding gaps are formed between the lower groove walls and the right groove walls, and the two installation parts are inserted into the two inserting grooves in a one-to-one correspondence mode. And the connecting arms pass through the corresponding avoiding gaps. According to the multifunctional sampling device provided by the utility model, the liquid tray can be conveniently disassembled and assembled, so that the liquid tray can be conveniently disassembled and assembled for cleaning in the later period.

This invention discloses a solid-phase microextraction probe for highly selective enrichment of perfluorinated and polyfluoroalkyl sulfonic acids (PFAS) and their substitutes, along with its preparation method and applications. The invention aims to improve solid-phase microextraction technology, enabling efficient and selective enrichment of PFAS and their substitutes, and achieving direct mass spectrometry analysis. To this end, this invention prepares a surface-modified coating through in-situ polymerization of a solid matrix, exhibiting highly selective adsorption capacity for enriching PFAS and their substitutes. This coating is simple to prepare, inexpensive, and exhibits good stability, avoiding cross-contamination issues. This method utilizes fluorine-fluorine interactions, hydrophobic interactions, and electrostatic interactions to efficiently enrich PFAS and their substitutes in complex biological samples, and is expected to play an important role in environmental analysis and biological sample detection.

The invention relates to a solid-phase microextraction device, an extraction method thereof and a chromatographic analyzer. The solid-phase microextraction device comprises a rack, an analysis position and at least one extraction position, wherein the analysis position and the extraction position are mounted on the rack; the extraction device further comprises an SPME handle and an extraction head mounted on the handle; the extraction station comprises an extraction base, a heating sleeve and a first handle supporting seat, the extraction base is provided with an extraction groove, the first handle supporting seat is correspondingly mounted at a groove opening of the extraction groove, and the heating sleeve is mounted in the extraction groove and used for placing an extraction sample bottle and heating the extraction sample bottle; the extraction head is inserted into an extraction sample bottle for headspace extraction or immersion extraction; the heating area of the heating sleeve covers the extraction liquid of the extraction sample bottle and the extraction height position where the extraction head is inserted into the extraction sample bottle; the analysis position comprises a heater, an analysis tube and a second handle supporting seat, the heater is used for heating the analysis tube, an analysis port of the analysis tube is correspondingly provided with the second handle supporting seat, and the extraction head is inserted into the analysis tube for heating analysis. According to the invention, a headspace cooling area is thoroughly eliminated, and the volatilization mass transfer efficiency is improved.

The invention discloses a transfer pipette for integrated operation of solid-phase microextraction and electrospray ionization and a use method of the transfer pipette. The transfer pipette is mainly made of a polymer material, a conductive metal clamping sleeve is embedded in the outer surface of the front end of the transfer pipette, and a triangular porous matrix, an artificially synthesized bead, an adsorbent and a circular porous matrix are sequentially arranged at the inner front end of the transfer pipette. Based on the design of the integrated pipette, a complex sample to be detected can be directly injected into the pipette, and by utilizing the interaction between the sample and the adsorbent, after a spray solvent is added, elution of a sample matrix is effectively inhibited, and meanwhile, rapid desorption of a target compound is promoted. And then, voltage is applied to the conductive metal clamping sleeve at the front end of the pipette, so that the tip of the triangular porous substrate generates electrospray, and in-situ ionization is realized. The method is combined with a mass spectrum technology, and can be used for efficient pretreatment and in-situ, rapid and high-sensitivity mass spectrum analysis of a target compound in a complex sample.

The invention provides a method for detecting anisole and four halogenated anisole in water by headspace solid phase microextraction-gas chromatography-mass spectrometry, which comprises the following steps: adding a water sample to be detected into a headspace sample injection bottle, then adding sodium chloride and deuterated 1, 2-dichlorobenzene, screwing a bottle cap and shaking uniformly to obtain a liquid to be detected; a sample injector provided with an extraction head is aged and then transferred to the position above a headspace sample injection bottle for headspace extraction, the extraction temperature ranges from 40 DEG C to 70 DEG C, the rotating speed ranges from 350 r / min to 750 r / min, and the extraction time ranges from 10 min to 40 min; the extraction head adopts CAR / DVB / PDMS as extraction fibers; and after the extraction is completed, performing thermal desorption on the sample injector at a sample injection port of a gas chromatograph-mass spectrometer, performing gas chromatography and mass spectrometry detection, and reading a response value. According to the invention, CAR / DVB / PDMS is adopted as the extraction fiber, so that the adsorption extraction effect on anisole and four halogenated anisole odor substances in the water body can be greatly improved, and the detection limit can be greatly reduced by combining the gas chromatography-tandem mass spectrometry technology. The method has the advantages of high extraction speed, low operation cost, no need of operations such as solvent extraction and digestion, and the like.

The application patent belongs to the technical field of environmental monitoring, and specifically discloses a solid-phase microextraction probe material, a preparation method thereof and application of the solid-phase microextraction probe material in preparation of a solid-phase microextraction probe coating for detecting disinfection by-products and glucocorticoids. The solid-phase microextraction probe material provided by the scheme has a simple preparation process and a lower cost than the price of existing commercial solid-phase microextraction probes. By introducing carboxyl functional groups, the adsorption sites are enriched, and the pore elasticity is increased, so that the adsorption capacity for polar trihalomethane disinfection by-products and glucocorticoids is significantly improved, and rapid, efficient and sensitive sample pretreatment is achieved.

This invention belongs to the field of solid-phase microextraction fiber technology, specifically relating to covalent organic framework materials synthesized based on ionic liquid catalysis and solid-phase microextraction fibers, and their application in aflatoxin contamination early warning. This invention uses ionic liquids as solvents and catalysts in the synthesis reaction of covalent organic framework materials, rapidly synthesizing ionic liquid-containing COFs (IL-COFs) in an open system at room temperature and atmospheric pressure. The solid-phase microextraction fiber is obtained by coating stainless steel wire with IL-COFs and then curing it. Using this solid-phase microextraction fiber for the extraction of aflatoxin and its precursors achieves highly selective and efficient adsorption. Combining IL-COF-based solid-phase microextraction with ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS / MS) enables simultaneous, sensitive, and accurate determination of aflatoxin and its precursors in samples. Furthermore, this detection method can be used to obtain the dynamic relationship between aflatoxin and its precursors, thereby providing early warning of aflatoxin contamination.

The invention provides a bile acid high-throughput detection method based on ultra-high performance liquid chromatography-tandem mass spectrometry and application thereof. The method comprises the following steps: pre-treating a sample to be detected, passing through a C18 solid-phase microextraction column, and collecting an eluent as a test solution; carrying out separation and detection by adopting ultra-high performance liquid chromatography-tandem mass spectrometry; mobile phases adopted by the ultra-high performance liquid chromatography comprise a mobile phase A and a mobile phase B, wherein the mobile phase A is a 0.095-0.105% formic acid aqueous solution containing 4.95-5.05 mM ammonium acetate, and the mobile phase B is an acetonitrile-methanol solution with the volume ratio of 3: (0.95-1.05); carrying out gradient elution; and establishing a linear regression equation of each bile acid subtype for quantitative calculation by mixing standard substances with different concentrations. The efficient extraction and detection method for the bile acid sample is established, separation and accurate quantification of 50 bile acid compounds are achieved, and the false positive problem caused by co-elution of isomeride bile acid in a traditional detection method is remarkably solved.

The present application relates to a kind of fluorine-based three-dimensional covalent organic framework material and its preparation method and application, belong to covalent organic framework material technical field.The present application under the action of catalyst, first monomer (first monomer is selected from containing normal tetrahedron amino monomer or containing normal tetrahedron aldehyde group monomer) and second monomer (second monomer is selected from containing fluorine aldehyde group monomer or containing fluorine amino monomer) carry out condensation reaction in organic solvent, obtain fluorine-based three-dimensional covalent organic framework material, and further as adsorbent, in-situ growth on probe substrate surface preparation solid phase microextraction probe, then with open mass spectrometry, for detecting trace perfluorinated compound in complex matrix.The fluorine-based three-dimensional covalent organic framework material of the present application has good chemical stability, high hydrophobicity, good adsorption effect on perfluorinated compound, and high reusability.

The invention belongs to the field of environment detection, and discloses a rapid screening method for odor substances in water, which comprises the following steps: (1) constructing a screening database for the odor substances in water for common odor substances in any region by using an MRM mode of GC-MS / MS (Gas Chromatography-Mass Spectrometry / Mass Spectrometry); wherein the parameters comprise the name and / or the CAS number of the odor substance, the m / z of the characteristic ion pair and the collision voltage; (2) carrying out pretreatment on the water sample, and extracting odor substances in water by utilizing an online solid-phase microextraction method; and (3) creating an MRM screening method by using the constructed screening database, screening the odor substances in the water sample to be detected by using the method, and judging that the water sample contains the odor substances in the MRM screening database when the characteristic ion pairs exist in the retention time range and are identified. According to the invention, the rapid and broad-spectrum screening of dozens of odor substances can be realized at the same time, the screening work cost is reduced, and the efficiency is improved.

This invention discloses a solid-phase microextraction probe, its preparation method, and its application in the detection of alkylphenols. The solid-phase microextraction probe comprises a rod body and a coating located on the outer periphery of the rod body. The coating is made by electrospinning a mixture of 4-meso-UiO-66, DMF, and PAN onto the outer periphery of the rod body. The solid-phase microextraction probe of this invention maintains its extraction performance after 80 adsorption-desorption cycles, and this probe exhibits excellent applicability for the selective detection of alkylphenols (APs) in milk.