652 results about "Solid phase extraction" patented technology

The invention discloses a gas positive pressure type solid-phase extraction device and an extraction method, and relates to the technical field of solid-phase extraction devices. A gas positive pressure type solid-phase extraction device comprises a base and further comprises a first supporting column and a second supporting column which are both rotationally installed on the base, an upper rotary disc and a lower rotary disc are longitudinally installed on the first supporting column in a sliding mode, a plurality of placing holes are formed in the upper rotary disc and the lower rotary disc, and the first supporting column and the second supporting column are arranged on the base. An upper bottle body and a lower bottle body are inserted into the two sets of containing holes respectively, an opening and closing part for driving the upper rotary disc and the lower rotary disc to ascend and descend is arranged on the first supporting column, and a switching part for driving the first supporting column and the second supporting column to rotate is arranged on the base. According to the device, multiple steps of extraction can be automatically realized, the device is more convenient, labor-saving and efficient to use, and liquid can pass through the filler more quickly, so that the solid-phase extraction efficiency is improved.

The invention discloses a component detection method suitable for a plant extract, and relates to the technical field of plant extract detection, and the component detection method comprises the following steps: S1, carrying out enrichment treatment on a target component by using two-phase liquid-liquid extraction; s2, performing multi-dimensional attribute mapping and component factor construction by using the initial enrichment liquid; s3, performing correlation feature constraint calculation by using the target component response tensor; s4, performing ideal spectrum construction and response difference analysis by using the to-be-compared spectrum feature set; s5, performing mapping analysis by using ideal and actual spectrum residual signals; s6, performing spectrum correction by using the standard comparison spectrum set; the selectivity of target component enrichment is improved by setting biphasic solvent-liquid-liquid extraction, efficient extraction of target components in a plant extract complex system is achieved, compared with existing single solvent extraction or solid-phase extraction, the method has the advantages that the target components are optimally distributed among liquid phases by regulating and controlling interaction among solvents, and the extraction efficiency is improved. And co-extraction of non-target components is reduced.

The invention discloses a pretreatment method for determining perfluorinated and polyfluoroalkyl compounds in edible oil. The pretreatment method comprises the following steps: (1) extraction: weighing the edible oil, adding an isotope labeled standard substance, centrifugally extracting PFAS (perfluoroalkyl) in a shaking table, adding desalted water to accelerate lipid sedimentation, and performing refrigerated centrifugation to obtain an extracting solution; (2) enriching and purifying, namely enriching and purifying the extracting solution by using a method of combining liquid-liquid extraction and solid-phase extraction, freezing and centrifuging, and collecting supernate after nitrogen blowing to a constant volume. According to the pretreatment method disclosed by the invention, aiming at the characteristic that the edible oil is rich in protein and lipid content, a liquid-liquid extraction and solid-phase extraction combined method is selected to remove impurities such as protein, lipid and pigment, so that separation and purification of PFAS are realized, and the sample requirements of subsequent LC-MS / MS analysis are met. According to the pretreatment method, the sample amount is increased, the final constant volume is reduced, the detection limit of the method is reduced, the sample treatment speed is increased, rapid analysis can be carried out, and the stability is good.

The invention discloses a microwave digestion-liquid flash spectrometer strontium isotope rapid detection system for multiple types of samples. The automatic sample injection module automatically identifies, grabs and conveys a sample by means of an image and radio frequency identification technology. The microwave digestion module is provided with a self-adaptive program, temperature and pressure are dynamically regulated and controlled through a PID algorithm according to sample characteristics, and efficient and safe digestion is ensured. The automatic separation and purification module intelligently selects a solid-phase extraction column or an ion exchange resin column to purify a sample by matching spectral analysis with a database. The liquid flash spectrometer detection module accurately collects signals by means of a high-sensitivity element and an algorithm. The data processing and control system adopts a multi-layer perceptron neural network, so that the strontium isotope content can be intelligently judged, and the source of abnormal data can be traced. In addition, the system has the functions of automatic cleaning and maintenance, emergency detection flow and remote monitoring, all the modules are connected through standardized interfaces, and the expansibility is high. The system is high in automation degree and accurate in detection, and an efficient and reliable scheme is provided for strontium isotope detection.

The invention provides a method for rapidly determining the content of 4, 4-dichlorodihydroxydiphenyl ether in a laundry detergent, and belongs to the technical field of detergent component content detection. According to the method, the content of 4, 4-dichlorodihydroxydiphenyl ether in the laundry detergent is measured by adopting a high performance liquid chromatography. In the determination process, an acetonitrile-water-sodium chloride three-phase mixture is used for removing impurities, and a mixed solution of acetonitrile and toluene is used as an extracting agent for solid-phase elution; a flowing phase A is an acetic acid aqueous solution with the pH value of 3.5-4, and a flowing phase B is acetonitrile. According to the method, the high performance liquid chromatography is combined with the solid phase extraction technology, high-sensitivity and high-accuracy determination can be achieved, a standard curve is established, and the reliability and accuracy of a result are further guaranteed. The method disclosed by the invention is simple to operate, good in stability and repeatability, and capable of accurately and rapidly measuring the content of 4, 4-dichlorodihydroxydiphenyl ether.

The invention provides a method for detecting fluorine compounds in shrimps, which comprises the following steps: S1, sample preparation: removing shells of to-be-detected shrimps, and crushing and homogenizing muscular tissues of the to-be-detected shrimps to obtain a to-be-detected sample; s2, extraction: extracting a sample to be detected, retaining an organic phase, and concentrating to obtain a concentrated solution; then adding water which is 5-15 times of the concentrated solution for dilution to obtain a to-be-purified solution; the extraction solvent is an aqueous solution of an organic solvent; s3, purification: purifying the to-be-purified liquid by using a solid-phase extraction column to obtain a purified liquid; s4, concentration and constant volume: concentrating the purified liquid to be nearly dry, redissolving, and filtering to obtain filtrate; and S5, sample detection: detecting the filtrate by using a liquid chromatograph-mass spectrometer, and carrying out qualitative and quantitative analysis on the fluorine compounds in the prawns by adopting a standard curve method. The method can be used for simultaneously determining the contents of 41 PFASs compounds with different physicochemical properties in shrimps.

The invention relates to a method for detecting perfluorinated compounds in water, which comprises the following steps: carrying out solid-liquid separation on a water sample to prepare a liquid to be detected; carrying out on-line solid phase extraction-liquid chromatography-mass spectrometry detection on the to-be-detected liquid, and calculating the content of the perfluorinated compounds in the to-be-detected liquid by an internal standard method. The detection method is high in automation degree, simple and rapid to operate and capable of accurately detecting the perfluorinated compounds in the water.

The application relates to the field of food detection, and discloses a sample pretreatment device for food safety detection, which comprises a shell, a crushing mechanism, a centrifugal mechanism, a material distribution mechanism, a solid-phase extraction mechanism and a nitrogen blowing mechanism are arranged in the shell; juice is obtained after the food sample is crushed, and the juice is subjected to centrifugal treatment in the centrifugal mechanism; the supernatant after centrifugation is temporarily stored and distributed in the material distribution mechanism; the multiple samples after distribution are subjected to solid-phase extraction in the solid-phase extraction mechanism; and the nitrogen blowing mechanism cooperates with the solid-phase extraction mechanism to complete nitrogen blowing work. Through structural innovation and function integration, the crushing, centrifugal, material distribution, extraction and nitrogen blowing concentration five function modules are integrated in the same equipment, the equipment floor area is reduced, the operation process is optimized, the manual intervention frequency is reduced, and the efficiency and reliability of the food safety detection sample pretreatment are remarkably improved.

The invention relates to a UPLC-MS / MS (Ultra Performance Liquid Chromatography-Mass Spectrometry / Mass Spectrometry) detection method for simultaneously determining 150 stimulant substances in cosmetics, and belongs to the technical field of stimulant detection. According to the detection method, a solid-phase extraction and QuECHERS combined pretreatment technology is adopted, firstly, an acetonitrile ultrasonic extraction mode in a QuECHERS method is adopted, secondly, a matrix is purified in a solid-phase extraction mode, an extraction tube adopts a filter type solid-phase extraction column, namely an Agilent Captiva EMR-Lipid filter column, different from a traditional HLB solid-phase extraction column, the filter column does not need to be activated and balanced, and the detection method is simple and convenient to operate. Gravity self-elution can be achieved in the sample purification process, and only 20% of pure water needs to be added into an extracting solution to achieve the purpose of activating a filtering column; and water can also be used as a dispersing agent and an impurity removing agent at the same time, so that impurities dissolved in water can be adsorbed while the sample is dispersed. The detection method provided by the invention can realize LC-MS / MS determination of 150 stimulant substances in cosmetics under the condition of simultaneously satisfying a pretreatment method for extracting 150 stimulant substances in cosmetics.

The invention discloses a high-throughput screening method for broad-spectrum new pollutants, which comprises the following steps: pre-treating a sample to be detected by using a mixed extracting agent of methanol and dichloromethane and an HLB solid-phase extraction small column, extracting the broad-spectrum new pollutants, and detecting the broad-spectrum new pollutants by using an ultra-high performance liquid chromatography-high resolution mass spectrometry technology. And carrying out data acquisition on the extracting solution in a full-scanning and full-ion fragmentation scanning mode. And then, the collected high-resolution mass spectrum data is compared with a self-established suspected target screening database containing N pollutants, and the data is integrated and analyzed according to a set screening and filtering standard, so that efficient and rapid matching and identification of the N pollutants in the sample are realized. According to the detection method, the to-be-detected sample can still be rapidly screened in the suspected target screening database under the condition that no standard substance exists, the detection speed and efficiency are remarkably improved, and meanwhile the detection cost is reduced.

The solid-phase extraction device with the cleaning structure comprises a base, a supporting frame is arranged at the top end of the base, and a lifting plate is connected into the supporting frame in a sliding mode; a moving mechanism is arranged at the top end of the base, and an adjusting assembly is arranged on one side of the supporting frame. Wherein the moving mechanism comprises a moving plate slidably connected to the interior of the top end of the base, supporting plates are symmetrically installed on the two sides of the top end of the moving plate, supports are symmetrically slidably connected to the interior of the top end of the moving plate, fixing seats are symmetrically installed at the top end of the base, and rotating plates are rotatably connected to the interiors of the fixing seats; therefore, the effect of rapidly adjusting and switching the collecting pipe can be achieved, the effect of cleaning waste liquid while solid-phase extraction in the liquid can be achieved, the solid-phase extraction efficiency in the liquid is greatly improved, the cleaning speed of the collecting pipe can be further improved, and the phenomenon that the use efficiency of the device is affected due to operation conflict of the two is avoided.

The present invention provides a kit and a detection method for synchronously detecting catecholamines and their metabolites, which relates to the technical field of analytical detection. The kit contains a diluent, a solid-phase extraction reagent, an LC-MS / MS detection reagent, a solid-phase extraction device, and a solid-phase extraction packing material. Among them, the solid-phase extraction packing material creatively adopts zwitterionic exchange microspheres containing both carboxyl and quaternary ammonium groups. The kit can not only synchronously and efficiently separate and detect 8 kinds of catecholamines and their metabolites in urine samples, but also separate and detect 6 kinds of amino-containing catecholamines and their metabolites in blood samples. When the above kit is used to separate and detect catecholamines and their metabolites, the extraction recovery rate is relatively high, and the linear range covers the reference value range of normal detection, which can significantly shorten the detection time of urine samples, improve the detection efficiency of mass spectrometry, and is conducive to popularization and application in clinical detection.

The application provides a pretreatment and detection method of tetrabromobisphenol A and ten common derivatives thereof in sludge, which comprises the following steps: (1) sample pretreatment: after mixing the frozen and dried sludge sample and the isotopic internal standard, oscillation extraction is carried out, and the extraction liquid is obtained after centrifugation by a centrifuge; the extraction liquid is purified by solid phase extraction to obtain a sample to be detected; (2) the sample to be detected obtained in the step (1) is detected by high performance liquid chromatography-tandem mass spectrometry; (3) the content of tetrabromobisphenol A and ten common derivatives thereof in the sample is calculated according to the internal standard method. The application provides a rapid and sensitive analysis and quantitative method of tetrabromobisphenol A and ten common derivatives thereof in sludge samples.

The invention discloses a method for detecting multiple perfluorinated compounds in a water environment. The method comprises the steps of sample collection and preservation, sample pretreatment and LC-MS / MS detection. According to the invention, trace detection is carried out on common perfluorinated compounds in a water environment by adopting solid-phase extraction-liquid chromatography-electrospray-tandem triple quadrupole mass spectrometer, a more perfect and comprehensive LC-MS / MS detection method for multi-medium concentration of perfluorinated compounds is provided, and on the premise that the recovery rate and the accuracy of a detection result are ensured, the detection efficiency is improved. The sample pretreatment modes in different media are optimized and adjusted, so that the experiment process is more convenient and faster, time and labor are saved, the use of traditional glass material consumables is avoided, and the experiment error is reduced; meanwhile, the method disclosed by the invention is wider in application range, can meet trace detection of perfluorinated compounds in surface water, underground water, domestic sewage, industrial wastewater, river sediment and residual sludge of a sewage plant, and provides data support for quality supervision and risk early warning in a water environment.

The invention discloses a method for separating and enriching 24 perfluorinated compounds in a water environment. The method comprises the following steps: collecting a to-be-detected water sample, filtering, and adding an isotope labeled recovery rate indicator to obtain a pretreated water sample; activating a PWAX solid-phase extraction column by using a 0.1% ammonia water methanol solution, methanol and ultrapure water in sequence, and enriching a water sample through the column; leaching the PWAX solid-phase extraction column with a 25 mM ammonium acetate aqueous solution (pH = 4) to remove water-soluble interference impurities; carrying out vacuum freeze drying on the solid-phase extraction column, and eluting with methanol and 0.1% ammonia water methanol solution; and blowing the collected eluent to 200 L under nitrogen flow, adding 1: 1 methanol and aqueous solution into the obtained residue, redissolving to 1.00 mL, filtering with a filter membrane, and putting into a polypropylene sample injection bottle to complete separation and enrichment. The method disclosed by the invention is simple and convenient to operate, can enrich various types of perfluorinated compounds (including carboxylic acids, sulfonic acids, fluorosulfonic acids and the like) in water, and is wide in application range and relatively high in accuracy.

The invention relates to the technical field of analytical chemistry, in particular to a method for simultaneously determining seven fat-soluble vitamin compounds. The method comprises the following steps: in 0-4.5 minutes, transferring a sample solution into an on-line solid-phase extraction column by a sample loading pump, and communicating an analysis pump with a liquid chromatographic analysis column through a switching valve for balancing; in 4.5-6.5 min, adjusting the state of a switching valve, respectively communicating two ends of the online solid-phase extraction column with an analysis column and an analysis pump of the liquid chromatography, and backflushing the analyte from the online solid-phase extraction column and transferring the analyte into the analysis column of the liquid chromatography by a mobile phase of the analysis pump; and 6.5-42 min, adjusting the state of the switching valve, flushing and balancing the on-line solid phase extraction column by the sample loading pump, and completing separation and analysis of the analyte by matching the analysis pump with the analysis column of the liquid chromatography. According to the method disclosed by the invention, saponification liquid can be directly analyzed on a machine, and seven target compounds can be separated and detected within 42 minutes.

The invention relates to the technical field of food safety detection, in particular to solid-phase extraction filler for detecting pesticide residues in food and a preparation method and application thereof.The solid-phase extraction filler comprises a magnetic filler core and a selective adsorption layer wrapping the magnetic filler core; wherein the interior of the magnetic filler core at least comprises magnetic particles and a coating layer for improving the stability of the magnetic particles; the selective adsorption layer is composed of a porous organic framework material which is chemically grafted outside the coating layer; and a temperature-sensitive polymer gel layer also covers the outer part of the selective adsorption layer. According to the solid-phase extraction filler disclosed by the invention, through an innovative hierarchical structure design, the extraction of trace pesticide residues in food can be effectively improved, the extraction difficulty is reduced, and the extraction efficiency and the extraction selectivity are improved.

The invention relates to the technical field of detection of organic nitrate, in particular to a method for detecting granular organic nitrate in soil. The method comprises the following steps: collecting a representative soil sample, labeling information, properly storing, carrying out freeze drying treatment on the sample, removing moisture, grinding the dried sample into fine powder, sieving to remove impurities, extracting the sample, obtaining a target compound, further purifying an extracting solution through a solid-phase extraction technology, removing interferents, and obtaining the target compound. And concentrating the purified solution to a proper volume by using a nitrogen blowing concentrator, redissolving the concentrated solution, fixing the volume to an accurate volume, and detecting the organic nitrate in the sample after the volume is fixed. The detection sensitivity of the organic nitrate is improved, a standard curve is established by adopting standard substance preparation and detection, the concentration of the organic nitrate in a sample is calculated by combining an external standard method, and the accuracy of a detection result is ensured.

The invention belongs to the field of soil dissolved organic matter analysis, and provides a multispectral-based DOM detection and reclamation influence evaluation method, which comprises the following steps: step 1, collecting dry farmland soil samples of different reclamation years, and obtaining soil column samples of a plough layer, a plow pan and subsoil; 2, extracting, centrifuging and filtering the soil sample to obtain a DOM solution; 3, detecting the DOM solution by adopting an ultraviolet-visible absorption spectrum; step 4, adopting a three-dimensional fluorescence spectrum and combining parallel factor analysis to obtain fluorescence components and source characteristics of the DOM solution; step 5, analyzing molecular composition and characteristic parameters of the DOM solution by adopting solid-phase extraction in combination with Fourier transform ion cyclotron resonance mass spectrometry; and step 6, based on the detection data in the steps 3-5, evaluating the influence of reclamation years on the composition, structure and degradation characteristics of the DOM. According to the method, multi-dimensional detection of soil DOM is realized through a multi-spectrum and mass spectrum combined technology, and DOM is comprehensively analyzed from a macrostructure to molecular composition.

The present invention relates to a method for detecting and / or quantifying an analyte in a sample using mass spectrometry. The method of the invention comprises: extracting the analyte from the sample using solid phase extraction (SPE) so as to obtain an SPE extract comprising the analyte, concentrating the analyte, said concentrating comprising evaporating solvent from the SPE-extract; and detecting and / or quantifying the analyte in the sample using mass spectrometry.

Methods and kits are provided for detecting and quantifying a PFAS compound or a mixture of PFAS compounds in a sample. The method includes the steps of providing a complex of a cyclodextrin and an indicator molecule, contacting the complex with the sample and measuring a parameter of the indicator molecule. The parameter is correlated with an extent of displacement of the reporter molecule from the cyclodextrin and binding of the PFAS compound to the cyclodextrin. This indicates the presence and quantity of the PFAS compound in the sample. The method is useful for monitoring samples such as environmental water samples. The kits include assay solutions for performing the methods and may also include solid-phase extraction matrices for pre-treatment of samples.

The invention relates to the field of food detection, and discloses a sample pretreatment device for food safety detection.The sample pretreatment device comprises a shell, a crushing mechanism, a centrifugal mechanism, a material distributing mechanism, a solid-phase extraction mechanism and a nitrogen blowing mechanism are arranged in the shell, and after a food sample is crushed by the crushing mechanism, juice enters the centrifugal mechanism to be subjected to centrifugal treatment; the material separation mechanism is used for temporarily storing and separating centrifuged supernate, the solid-phase extraction mechanism is used for carrying out solid-phase extraction on a plurality of separated samples, and the nitrogen blowing mechanism and the solid-phase extraction mechanism are matched to complete nitrogen blowing work. Through structural innovation and function integration, five functional modules including crushing, centrifuging, material separation, extraction and nitrogen blowing concentration are integrated into the same equipment; the occupied area of the equipment is reduced, the operation process is optimized, the manual intervention frequency is reduced, and the pretreatment efficiency and reliability of the food safety detection sample are remarkably improved.

The invention discloses a method for detecting perfluoroalkyl (polyfluoroalkyl) compounds in sludge, which comprises the following steps: screening concentrated sludge of a sewage plant, removing foreign matters, pretreating, putting into a centrifugal tube, and adding an extraction internal standard; the method comprises the following steps: extracting PFAS in sludge by using an alkaline organic solvent to obtain a PFAS extracting solution; filtering and acidifying the PFAS extracting solution to obtain an acidified extracting solution; purifying and eluting the acidified extracting solution through a solid-phase extraction column to obtain an eluent; drying the eluent, re-dissolving to 1mL by using methanol, filtering, and collecting the supernate into a sample injection bottle; and adding a sample introduction internal standard into the sample introduction bottle, mixing, and determining the PFAS in the sludge by using a liquid chromatography tandem mass spectrometer. By optimizing a pretreatment method for determining the PFAS in the sludge and a mode for reducing the matrix effect, a method capable of accurately quantifying the PFAS (51 different types) in complex environmental samples such as the sludge and biological solids is developed, and the analysis range and accuracy of the PFAS in the sludge are improved.

The invention provides a full-automatic online detection method for trace polycyclic aromatic hydrocarbon derivatives (SPAHs) in water, which comprises the following steps: (1) pretreatment: standing a water sample, centrifugally filtering to remove suspended matters, adding a prepared mixed standard solution, and directly loading on a machine; (2) enrichment and separation: adopting a Turbo flow C18-XL on-line solid phase extraction column to realize automatic enrichment and matrix purification of the 15 SPAHs, and combining an ultra-high performance liquid chromatography gradient elution program (methanol-ultrapure water system) to realize efficient enrichment and separation; and (3) detection and analysis: performing Full MS-ddMS2 scanning in an APCI (Amplified Peripheral Component Interconnect) source-Orbitrap high-resolution mass spectrum positive and negative ion switching mode to realize synchronous detection of hydroxyl, nitro and oxygen-containing SPAHs. According to the method, a unified detection system covering six hydroxyl polycyclic aromatic hydrocarbons, six oxygen-containing polycyclic aromatic hydrocarbons and three nitro polycyclic aromatic hydrocarbons is constructed for the first time, the detection limit is as low as 0.02 ng / L, and compared with a traditional GC-MS method, the sensitivity is greatly improved, and the sample pretreatment time is greatly shortened. Compared with the prior art, derivatization treatment is not needed, continuous sample injection is achieved through an online solid-phase extraction column regeneration technology, complex matrix interference is effectively eliminated in cooperation with a dynamic elimination function, and a high-sensitivity and high-throughput analysis method is provided for ecological risk assessment of trace SPAHs in underground water and surface water.

The invention provides a collection and detection method for electronic cigarette atomized released substances, and belongs to the technical field of electronic cigarette detection. The method comprises the following steps: step 1, adsorbing and collecting aerosol release substances generated after atomization of electronic cigarette atomized liquid by using a solid-phase extraction column, wherein the solid-phase extraction column is filled with an adsorbing material polyethylene divinylbenzene; step 2, eluting the solid-phase extraction column after adsorption in the step 1 to obtain an eluent as a to-be-detected sample solution; and 3, detecting the content of a sweetening agent in the to-be-detected sample solution obtained in the step 2 by using a liquid chromatograph, and detecting the content of a cooling agent and a flavor substance in the to-be-detected sample solution by using a gas chromatograph-mass spectrometer. The method provided by the invention has very good trapping efficiency on substances with various phase states and pH values in aerosol release substances of the electronic cigarette, especially has a relatively strong adsorption effect on low-carbon ester and terpene flavor substances, improves the detection accuracy, and is suitable for simultaneous detection of various components in electronic cigarette products.

The invention relates to the technical field of environmental analysis and testing, and discloses a method for detecting perfluorinated compounds in soil, which comprises the following steps: (1) crushing and sieving a soil sample to be detected, then carrying out pressurized fluid extraction, carrying out rotary evaporation concentration on the obtained extract, and dissolving with methanol again to obtain a concentrated solution; (2) purifying the concentrated solution through a solid-phase extraction column, and then concentrating to a constant volume to obtain a to-be-detected solution; (3) detecting the type and the content of the perfluorinated compounds in the to-be-detected liquid by adopting a liquid chromatography-tandem mass spectrometry method; wherein in the step (1), an extracting solvent is a NaOH methanol solution; in the step (3), in the liquid chromatography-tandem mass spectrometry, the liquid chromatographic condition is as follows: a liquid chromatographic column is a C18 chromatographic column. The detection method provided by the invention is simple to operate, high in accuracy, good in repeatability, capable of analyzing multiple PFAS types (17 types) and low in detection limit, meets the analysis requirements, and can be used for analyzing and monitoring common PFAS in soil.

The invention belongs to the field of liquid chromatography-mass spectrometry detection, and discloses a liquid chromatography-mass spectrometry detection method for trace target objects in seawater, which comprises the following steps: firstly, configuring and precisely calibrating parameters such as flow velocity, column temperature, ion source voltage and the like for a liquid chromatography system, a chromatographic column, an automatic sampler and a tandem mass spectrometer; then, a methanol-water (containing 0.1% formic acid) system is adopted to implement linear gradient elution, polar difference component separation is considered, and analysis duration is compressed; a sample is subjected to solid-phase extraction, purification and concentration, then is automatically injected, is subjected to chromatographic separation and then enters an electrospray ion source; a mass spectrum end selects a dynamic multi-reaction monitoring (dMRM) mode, characteristic ion pairs are collected in a preset time window, and selective scanning and baseline noise suppression are achieved; and finally, utilizing retention time matching and internal standard correction to obtain a pg.L <-1 > magnitude quantitative result.

A method for obtaining the detection limit of 23 perfluorinated compounds in water relates to the technical field of pollutant detection, and comprises the following steps: step S1, taking a sufficient amount of a water sample and placing the water sample in a fluoride-free volumetric flask to obtain a water sample containing methanol; s2, preparing a water quality sample to be detected; s3, detecting the water quality sample to be detected by adopting a high performance liquid chromatography tandem mass spectrometer; s4, setting an elution program of a mobile phase; and S5, testing, and calculating the concentrations of 23 perfluorinated compounds in the water quality sample to be detected. According to the method, the detection limits of 23 perfluorinated compounds in water are obtained by utilizing a liquid chromatography-triple quadrupole mass spectrometer and adopting an online solid-phase extraction method, so that the detection efficiency is improved, the personal error is reduced, and the consumption of an organic solvent and the use of a traditional solid-phase extraction column are reduced.

The invention discloses a liquid chromatography-tandem mass spectrometry detection method for catecholamine and metabolites thereof, which comprises the following steps: step 1, sequentially adding a sample to be detected, an internal standard solution, a derivatization buffer solution and a derivatization solution into holes in the third / ninth column of a 96-well plate, oscillating at room temperature, replenishing water, and continuing oscillating; step 2, adding an activating solution and magnetic beads into the first / seventh column of the 96-well plate; adding equilibrium liquid into the second / eighth column; a first leacheate is added into the fourth column and the tenth column; adding a second leacheate in the fifth / eleventh column; adding the eluent into the 6 / 12th column; then placing the sample on a 32-channel sample pretreatment system for magnetic solid-phase extraction; and step 3, liquid chromatography-tandem mass spectrometry detection. According to the method, the sample is firstly derivatized and then is subjected to magnetic solid-phase extraction, so that only less sample size is needed, the sensitivity is higher, and the economical efficiency is better; according to the method for directly derivatizing the sample, the sample does not need to be derivatized after being subjected to protein precipitation and supernatant removal, and the steps are simpler, more convenient and more automatic.

The invention discloses a high-throughput detection method for liquid crystal monomers in sediments, which comprises the following steps: extracting, enriching, purifying and removing impurities from the sediments, measuring by using a gas chromatograph-quadrupole rod-electrostatic field ion orbitrap combined high-resolution mass spectrometer, and analyzing to obtain the types and contents of the liquid crystal monomers in the sediments. According to the method, various liquid crystal monomers can be simultaneously and rapidly determined, impurity interference in a sample is effectively removed by utilizing extraction, enrichment and purification impurity removal, the chromatographic separation efficiency is improved, the anti-interference capability is improved by utilizing the extremely high resolution of the electrostatic field ion orbitrap high-resolution mass spectrum, the background interference is effectively reduced, and the detection accuracy is improved. Meanwhile, ultrasonic-assisted extraction and solid-phase extraction technologies are combined to purify a target object, so that the tedious steps of sample pretreatment are simplified, and the detection limit of the detection method is reduced.