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3927 results about "Solid phase extraction" patented technology

Solid-phase extraction (SPE) is a sample preparation process by which compounds that are dissolved or suspended in a liquid mixture are separated from other compounds in the mixture according to their physical and chemical properties. Analytical laboratories use solid phase extraction to concentrate and purify samples for analysis. Solid phase extraction can be used to isolate analytes of interest from a wide variety of matrices, including urine, blood, water, beverages, soil, and animal tissue.

Hot pepper and determining method for 96 pesticide residues in product of hot pepper

The invention discloses hot pepper and a determining method for 96 pesticide residues in a product of the hot pepper. The determining method comprises the following steps: homogenously extracting residual pesticide in a sample with 1% acetic acid-acetonitrile solution, purifying the extracting solution with a Florisil solid phase extraction column, dispersing and purifying the extracting solution with ethylenediamine-N-propyl silane (PSA) and octadecyl silane bonded phase (C18) substrate, detecting 69 pesticide residuals in the purified concentrated liquid of the Florisil column by GC-MS (gaschromatographic mass spectrometry), detecting 27 pesticide residuals in the substrate dispersed purified liquid by liquid chromatography-tandem mass spectrometry (LC-MS / MS), using the black substrate solution dilution standard to construct the updated calibration curves, adopting an internal standard method to quantify when using GC / MS to detect the residuals, and adopting an external standard method to quantify when using LC-MS / MS to detect the residuals. The average recovery rate of the method is 70.7-118.6%; the average relative standard deviation (RSD) is 3.2-11.4%; the detection limit is 0.13-28.2 ug / kg. The determining method has the advantages of simplicity and convenience in operation, high speed, accuracy, high sensitivity and good repeatability.
Owner:INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU

Method for simultaneously detecting multi-kind pesticide residues in bee products

InactiveCN101358953ASolve the problem of matrix effectFast wayComponent separationRetention timePhosphate
The present invention relates to a method of simultaneously detecting a plurality of agro-veterinary drug residues in bee products. The extracted liquid trichloroacetic acid or perchloric acid and the extracted liquid acetate, phosphate or borate solution are added into a sample; the pH value is controlled between 4.5 and 9.0; the mixed solution is centrifuged, the filtrate is added into a solid phase extraction column to be extracted, the extraction column is eluted and dried, the column is washed by oxalic acid-methanol solution, the volume of the eluent is defined by the aqueous solution of methanol, the eluent is added into liquid chromatography-tandem mass spectrometry to be analyzed and tested, the acquired chromatographic peak is contrasted with the known standard chromatographic peak of the drug, and according to the retention time and the abundance of the mass spectrum ions, the specific name of the detected drug is determined. The method only requires one pre-treatment of the sample, and thus can simultaneously extract 11 classes and more than 60 kinds of veterinary drug residues, such as sulfonamides, quinolones, macrolides, lincomycins, nitroimidazoles, beta-lactams, tetracyclines, chloromycetins, trinethoprims, chlordimeform, triadimenol and the like, the efficiency of analysis is high, and the detection cost is greatly reduced.
Owner:中华人民共和国江苏出入境检验检疫局

Method for detecting tobacco-specific nitrosamines

The invention relates to a method for measuring tobacco-specific nitrosamines (TSNAs for short) by using a super efficient liquid chromatogram-tandem mass spectrum combined method, and belongs to a method for detecting TSNAs. The method comprises the following steps of: adding internal standard-containing aqueous solution of ammonium acetate into a filter sheet after trapping smoke and cigarette filters smoked completely under standard conditions or tobacco shreds, performing ultrasonic extraction, transferring 1 to 2mL of extract into a small solid-phase extraction column taking N-vinyl pyrrolidone-benzene sulfonic acid copolymer as filler, flushing the small column by using aqueous solution of methanoic acid and methanol, finally eluting the small column by using solution of aqueous ammonia and methanol solution, analyzing the eluant by using an ultra performance liquid chromatography-mass spectrometer/mass spectrometer (UPLC-MS/MS), and quantifying according to the area ratio of a component peak to an isotope internal standard peak. The detecting method can be used for detecting the TSNAs in cured and hybrid cigarette mainstream smoke, cigarette side-stream smoke, filter tip intercepting smoke and tobacco shreds, and has the advantages of simple pretreatment, accurate quantification, high instrument analysis speed, low detection limit, high sample treatment flux and the like.
Owner:HONGTA TOBACCO GRP

Full-automatic modular multi-sample intelligent processing system

The invention discloses a full-automatic modular multi-sample intelligent processing system, which comprises a liquid adding and homogenizing module, an automatic vacuuming and filtering module, an automatic nitrogen blowing and concentrating module, an automatic gelatum permeating and purifying module, an automatic slide phase extracting module, an automatic transmitting and heating module and an operation control module. Corresponding processing modules, experimental condition procedures and operation procedures are edited and selected by the operation control module according to the needs of different samples to be processed to carry out corresponding automatic processing. The full-automatic modular multi-sample intelligent processing system can synchronously process four samples, can continuously process fixteen samples, and carry out processing procedures of liquid adding, homogeneity extraction, filtration, gelatum purification, solid phase extraction, nitrogen blowing on the samples. The full-automatic modular food residual sample processing system realizes full automation of processing the samples, effectively improves the sample processing quantity, simplifies the operation process, improves the detection quality and improves the experimental safety.
Owner:CHINESE ACAD OF INSPECTION & QUARANTINE

Preparation method of covalent organic framework composite microspheres with core-shell structures

The invention relates to a preparation method of covalent organic framework composite microspheres with core-shell structures. The method comprises the following steps: dissolving silicon dioxide microspheres, a first construction element and a second construction element in an organic solvent; and after adding a catalyst, rapidly synthesizing into the composite microspheres with core-shell structures at a certain temperature. In a preparation process, reaction conditions are gentle, the method is simple, and the yield is high; the prepared covalent organic framework composite microspheres have the advantages of good core-shell morphology, high specific surface area, ordered pore structures, good mechanical stability, thermal stability, chemical stability and the like, if the microspheres are used as a chromatographic stationary phase, the chromatographic mass transfer resistance can be reduced effectively, the theoretical plate height is improved, and finally, column efficiency and degree of separation are improved; and if the microspheres are used as solid-phase extracting filler, the enrichment effect can be improved remarkably. The covalent organic framework composite microspheres with core-shell structures have good application prospects in the aspect of separation and enrichment of small organic molecules.
Owner:FUZHOU UNIV

Triazine weedicide, and metabolite molecular engram polymer microspheres, preparation method and application thereof

The invention discloses a triazine weedicide, and metabolite molecular engram polymer microspheres, a preparation method and an application thereof, which relate to molecular engram polymer microspheres and a preparation method and an application thereof and are used for solving the problem that the conventional molecular engram polymer can only specially absorb one kind of substance and realizing the effect of separating and enriching a plurality of triazine pesticide residues in a sample respectively. The molecular engram polymer microspheres are prepared by the following steps of: dissolving double template molecules and methacrylic acid into acetonitrile; oscillating; adding trimethylolpropane trimethylacrylate and azobisisobutyronitrile; performing ultrasonic treatment, charging nitrogen, removing oxygen and sealing; and heating in a constant-temperature water bath, cooling, grinding, sieving, eluting and drying. The molecular engram polymer microspheres are applied to a filling material of a solid phase extraction column. A product obtained in the invention has the advantages of high specificity, large absorption amount, wide application range, simple method and low cost. High specific separating and enriching characteristics on the triazine weedicide are achieved, the recovery rate is 65-110 percent, and the requirement of multiple residues can be met.
Owner:INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS

Method for analyzing and detecting a plurality of endocrine disruptors in food

The invention belongs to the field of food inspection, relates to an assay determination method for endocrine disruptors in food, and particularly relates to a method for analyzing and determining a plurality of endocrine disruptors in milk powder and liquid milk. The method comprises the steps of dissolving a sample with water, adding an organic solvent mixable with water, extracting a to-be-detected material by ultrasonic, adding a sodium salt to make the organic solvent separated from a water phase to realize liquid-liquid extraction, taking an organic solvent containing quantitative to-be-detected material, purifying by extraction with a solid phase filled with C 18 materials, deriving by dansyl chloride, and analyzing and detecting four types of 26 endocrine disruptors in the food by using ultra-high performance liquid chromatography-quadrupole-time of flight-mass spectrometry at the same time. The method can overcome the disadvantages that a conventional technology cannot realize simultaneous analysis of the plurality of the endocrine disruptors in the food by once chromatographic sample injection, can increase sensitivity of the quadrupole-time of the flight-mass spectrometry, and realize accurate analysis of the endocrine disruptors in the food by using the quadrupole-time of the flight-mass spectrometry.
Owner:FUDAN UNIV

Preparation method of magnetic metal organic framework material and application of magnetic metal organic framework material

The invention discloses a preparation method of a magnetic metal organic framework material and an application of the magnetic metal organic framework material. The preparation method comprises the steps of synthesizing a nano magnetic material Fe3O4 by adopting a coprecipitation method, adding the nano magnetic material Fe3O4, FeCI3.6H2O and terephthalic acid into DMF, carrying out ultrasonic mixing, and synthesizing Fe3O4/MIL-101(Fe) by adopting a hydrothermal method; separating a product by utilizing a magnetic field, washing with hot ethyl alcohol, and drying overnight so as to obtain the Fe3O4/MIL-101(Fe). The Fe3O4/MIL-101(Fe) obtained by the method is applied to separating and enriching organophosphorus in urine. The magnetic metal organic framework material is uniform in particle size, is relatively strong in magnetism, and is good in dispersibility; MIL-101(Fe) formed by the coordination of oxygen bearing carboxylate ligand and a metal ion F3<3+> is adopted as an adsorption separation medium and is combined with a magnetic solid phase extraction technique for being combined with chromatography so as to determine trace organophosphorus residues in urea, and the magnetic metal organic framework material is relatively high in flexibility.
Owner:HANGZHOU DIANZI UNIV

Method for simultaneously detecting a plurality of mycotoxins in sesame paste

The invention relates to a method for detecting a plurality of mycotoxins in a sesame paste, and particularly relates to a method which carries out pre-treatment by an optimized dispersive solid-phase extraction method (QuEChERS), and simultaneously detects 26 mycotoxins in sesame paste by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS / MS). The method particularly comprises: extracting a sample twice with acid-containing acetonitrile-aqueous solutions with different concentrations, adding magnesium sulfate and sodium chloride into the sample extract for salting out, performing centrifugation, adding n-hexane into the obtained supernatant, performing vortex oscillation and degreasing, purifying the product with C18 and magnesium sulfate, performing vacuum concentration, dissolving the residues again with methanol and water in order to obtain a sample analytic solution, and detecting the solution by a multi-reaction monitoring mode of ultra-high performance liquid chromatography-tandem mass spectrometry. The method improves the detection efficiency, saves detection cost, is high in sensitivity, high in repeatability, and high in adding standard recovery rate, and can be extended to detection of other samples with a high grease content.
Owner:PEOPLES REPUBLIC OF CHINA BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU

Method for simultaneously measuring multiple residues of organic chloride and pyrethroid pesticides

The invention discloses a method for simultaneously measuring multiple residues of organic chloride and pyrethroid pesticides. The method comprises the following working procedures: crushing a tobacco sample until grain diameters are less than 450 mu m; adding 10 to 20ml of extracting solution and internal standard solution into every program of tobacco sample; extracting the mixed solution by using ultrasonic wave; filtering the mixed solution by using a funnel filled with anhydrous sodium sulfate to obtain the extracting solution; adding the extracting solution into a Florisil solid extraction column for extracting and eluting; collecting an eluent; analyzing the eluent by using a gas chromatograph, wherein the analysis comprises the following conditions: adopting an Elite 5MS capillary column, high-purity N2 as a carrier gas, a constant flow mode in which the flow rate is 0.5 to 1.5 ml/min, a sample inlet temperature of between 280 and 320 DEG C, a detector temperature of between 330 and 370 DEG C, splitless sampling in which the sampling volume is between 1 and 2 mu L, and an initial temperature of 100 DEG C which rises from 100 to 180 DEG C at a speed of 8 DEG C/min, is kept for 4 minutes, rises from 180 to 270 DEG C at the speed of 5 DEG C/min and is kept for 15 minutes until all sample flows out completely; and determining the nature of the sample by using the retaining time of a standard sample and quantifying by using an internal standard method. In the method, ultrasonic wave is adopted for extracting and a solid extraction column is adopted for purifying, so that the method has the advantages of operating step simplification, high work efficiency, good purification effect, capability of simultaneously measuring multiple residues of 25 kinds of pesticides including 17 organic chloride pesticides of hexachlorocyclohexane, DDT and the like, seven pyrethroid pesticides such as fenpropathrin and the like, and one plant growth regulator.
Owner:YUNNAN ACAD OF TOBACCO AGRI SCI
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