48results about How to "Accurate Qualitative and Quantitative Analysis" patented technology

The invention discloses a fast detection method for the surface enhanced Raman scattering of trace pesticide residues in oranges, and belongs to the technical field of fast pesticide detection. The fast detection method comprises the following steps: adopting acetonitrile, anhydrous magnesium sulfate and sodium chloride for mixing in a certain ratio so as to extract pesticide ingredients from the oranges as many as possible; mixing anhydrous magnesium sulfate, N-propyl ethylenediamine, C18 and graphitized carbon in a certain ratio; eliminating influences of fluorescent substances, such as organic acids, pigments, pectin and cellulose, in an extraction liquid. According to the fast detection method, the detection accuracy for the surface enhanced Raman scattering of the pesticide residues in the oranges is greatly increased, the aim of the fast detection of the trace pesticide residues is achieved, and the fast detection method basically meets the requirements of detection limit specified by the state; the fast detection method is adopted to detect the trace pesticide residues in the oranges, is simple in pre-processing of samples to be detected, fast in detection speed, low in detection cost and high in accuracy and precision, can fast and accurately analyze the trace pesticide residues in the oranges in a qualitative and quantitative manner, and can be used for on-site sample detection on a large scale.

The invention relates to a method for detecting polycyclic aromatic hydrocarbon component in a coking wastewater processing system, belonging to the technical field of analysis and detection of toxic pollutants in environmental monitoring. The detection method is composed of three steps: solvent extraction, extract liquor purification and gas chromatograph-mass spectrometer detection. Firstly, a pressure solvent extraction system is used for quickly extracting polycyclic aromatic hydrocarbon component in the residual sludge in the coking wastewater processing system under the condition of heating and pressurizing; then, a silica gel / alumina composite layer column is adopted to separate and purify extract liquor; and finally, collected leacheate is concentrated to proper volume, and the gas chromatograph-mass spectrometer is used for detection analysis under the condition of selecting ion modes. The invention has short time consumption for extraction, uses small amounts of extracting solvent, can effectively remove polar and nonpolar interfering components in sludge in the purification process, has high sensitivity and stable operation, can accurately and quantificationally analyze trace polycyclic aromatic hydrocarbon in the residual sludge in the coking wastewater processing system.

The invention provides a method for detecting 7 classes of 59 forbidden drugs in goat milk and goat milk products. The method comprises the following steps: (1) sample pretreatment: extracting a to-be-detected sample with an acid organic solvent, carrying out purification by virtue of an SPE column, dissolving a purified liquid by virtue of a primary flow phase, and carrying out UPLC-MS / MS detection; and (2) detection of 59 to-be-detected forbidden drugs: detecting the pretreated sample by virtue of an ultra-high performance liquid chromatography-mass spectrometry under specified instrument conditions of the method. The method has the advantages that many drugs can be detected, the type of the drugs is rich, the detection time is short, the sensitivity is high, and a result is accurate andstable; and meanwhile, the detection blank that multiple types and quantity of drugs in the goat milk and the goat milk products can be simultaneously detected is filled up, and the method has important significances to the guarantee of the body health of consumers and the increase of export trade competitiveness of the goat milk and the goat milk products.

The invention discloses a forensic medicine diatom test method.The forensic medicine diatom test method comprises the following steps that sulfamethazine, acrylic acid, acrylamide, N'N-methylene bisacrylamide, ammonium persulfate and deionized water are taken according to a proportion and fully mixed in a beaker; after oxygen is removed with nitrogen, the mixture is poured into a sandwich space formed by two glass slides and then put into an oven at the temperature of 60 DEG C for a polymerization reaction for 3 h, and film-state imprinting hydrogel is prepared; the obtained imprinting hydrogel is soaked in a 10% acetic acid solution, template molecules sulfadimidine in the imprinting hydrogel are removed through ultrasonic oscillation, then the imprinting hydrogel is soaked in a sample to be tested for 5-10 min and then taken out, and then the imprinting hydrogel is put under an optical microscope for observation; diatom on the filter film or a shot picture is checked, classified and counted in a manual recognition mode or an automatic computer recognition mode.The forensic medicine diatom test method is high in yield, efficiency and performance cost ratio, easy to popularize, accurate in qualitative and quantitative analysis and low in labor intensity.

The invention relates to a method for simultaneously detecting multiple phosphorus-based flame retardants in plastics. The method comprises the following steps: (a) establishing a standard curve; (b) pretreating a sample; and (c) detecting the sample. The detection method has the beneficial effects that a selected chromatographic column can realize a good separating effect on the multiple phosphorus-based flame retardants; in addition, fast determination can be carried out on the multiple phosphorus-based flame retardants, and accurate qualitative and quantitative analysis are realized by the method; and the method is good in reproducibility, high in recovery rate, good in precision and simple in operation.

The invention discloses a surface enhanced Raman spectroscopy method for organo-chlorine pesticide residues of fruits and vegetables and belongs to the technical field of detection methods of pesticide residues. The method comprises the following steps: 1, preparing a copper foil substrate; 2, depositing silver nanoparticles on the surface of the copper foil; 3, modifying mercapto on the substrate; 4, performing surface enhanced Raman spectroscopy on organo-chlorine pesticide standard products; and 5, detecting the pesticide residues of the fruits and vegetables. According to the method disclosed by the invention, the sample pretreatment is simple, the detection speed is high, the detection cycle is shortened, the cost is low, and rapid detection of micro / trace pesticides of the fruits andvegetables is realized.

The invention discloses a method for determining residues of metabolites of four nitrofurans drugs in an animal glue traditional Chinese medicine. The method comprises the following steps: preparing to-be-tested sample solution; preparing standard solution; injecting a standard series of working solution into a liquid chromatograph / mass spectrometer, determining appearance positions of the metabolites of the four nitrofurans drugs and qualitative and quantitative determination ion pairs thereof, and making a standard curve equation by taking the abundance of the quantitative ion pairs as a vertical coordinate and taking the concentration as a horizontal ordinate; substituting data obtained by corresponding detection for the to-be-tested sample solution into the standard curve equation forcalculation, so as to obtain the contents of the metabolites of all the nitrofurans drugs in the to-be-tested sample. The metabolites of the four nitrofurans drugs are: a furanzolidon metabolite (AOZ), a furaltadone metabolite (AOMZ), a furacilin metabolite (SEM) and a furadantin metabolite (AHD).

The invention relates to an SER rapid detection method for patent blue V in beverage. The SER rapid detection method comprises the following steps: (1) preparing a gold nano reinforced substrate; (2)screening electrolyte; (3) producing a Raman spectrum peak standard line; (4) removing impurities of the beverage; (5) taking a plurality of commercial beverages free from a substance to be detected as a blank sample, removing volatiles in step (4), extracting, and separately preparing a coloring agent solution with the gradient concentration of a blank beverage matrix; uniformly mixing 50 micro liters of a solution to be detected, 500 micro liters of gold sol substrate prepared in step (1) and 100 micro liters of electrolyte solution obtained in step (2), and performing the Raman spectrum detection; (6) qualitatively analyzing pigments in a beverage test sample; and (7) half-quantitatively analyzing the pigments in the beverage test sample. According to the SER rapid detection method forthe patent blue V in the beverage, the pretreatment of a sample is simple and fast, a single sample can be detected only in about 10 minutes, the coloring agent in the beverage test sample can be rapidly, accurately, qualitatively and quantitatively analyzed, and the SER rapid detection method can be used for rapidly screening and detecting a great amount of samples on site.

The invention provides a method for detecting 8 categories of restricted drugs in goat milk and products thereof, wherein the number of the restricted drugs is 74. The method comprises: (1) pre-treating a sample: extracting a sample to be detected with an acid organic solvent, purifying with a SPE column, and dissolving the purified liquid by using an initial mobile phase so as to be used for detection with UPLC-MS / MS; and (2) determining 74 restricted drugs: determining the pre-treated sample by using ultra performance liquid chromatography-LC-MS under the instrument condition specified by the method. According to the present invention, the method has advantages of more types of detected drugs, rich variety, short detection time, high sensitivity and accurate and stable results, can makesup for the absence of the simultaneous detection of multiple drugs in goat milk and dairy products, and provides the important significance for the assurance of the health body of consumers and the improvement of the export competitiveness of goat milk and dairy products.

The invention discloses a quick detecting method for sudan red in food, and relates to the field of food safety. The detecting method comprises the four steps of sample pretreatment, concentration and evaporating to dryness, film chromatography, and HPLC determination. The quick detecting method solves the problems that detecting instrument is expensive, complex to operate and not easy to popularize, has the characteristics of high extraction rate, high purifying purity, high recovery ratio and the like, and can achieve the purpose of being quick and reliable, simple and convenient to operate, and cost-saving.

The invention discloses a device and a method for collecting toxic gas in high-temperature decomposition of materials. The device comprises a tubular cracking furnace and a sample boat, and further comprises a double-hole ball head inlet connector, a quartz combustion cylinder, a double-hole ball head outlet connector, an anti-inverse-suction buffer bottle, a gas absorption bottle, a drying tube,a dust filter, a needle valve, a flow meter and a gas storage bag, wherein the quartz combustion cylinder is located in the tubular cracking furnace. After being put into the sample boat, a sample ispushed to the high-temperature quartz combustion cylinder for combustion through a sample pushing magnetic block; after a part of the generated toxic gas is absorbed by an absorption liquid, the restof the toxic gas is dried and subjected to dust filtration; and the filtered toxic gas is collected in the gas storage bag. By the adoption of the device and the method, under the condition that gas flow of carrier gas is not interrupted, the sample can be rapidly and accurately fed; the test failure caused by the fact that a gas path is opened by impulsion at the moment of combustion can be avoided; the device is simple in structure, high in universality, short in analysis time, low in cost and convenient to operate; and the toxic gas can be better subjected to accurate qualitative and quantitative analysis.

The invention discloses a qualitative and quantitative analysis method for an old negative plate of a lead acid battery. The method comprises the following steps: firstly, dissecting a tested battery, taking out the negative plate, and cleaning the surface separator of the negative plate; washing the negative plate with deionized water until the surface thereof becomes neutral; further soaking the negative plate in boric acid- salicylic acid impregnation liquid for more than 20 minutes while heating, and keeping temperature of the boric acid-salicylic acid impregnation liquid to be 60-80 DEG C during the soaking process; then, taking out and baking the negative plate to completely remove water on the surface thereof; and finally, taking down a lead paste from the dried negative plate, grinding the lead paste into powder, and carrying out qualitative and quantitative analysis on constituents of the negative plate through an XRD(X-Ray Diffraction)-Rietveld method. According to the invention, firstly, the old negative plate drawn out from the battery is pretreated, a protective layer is formed on the surface of the negative plate, oxidization of lead of the negative plate is avoided effectively and residual of sulfuric acid on the surface of the negative plate is removed, as a result, the negative plate can be dried directly by a normal drying method, and the qualitative and quantitative analysis method is high in testing accuracy, convenient and simple, low-cost and pollution-free.

The invention provides a method for detecting the content of monascus pigments in meat products, which comprises the steps of obtaining a proper amount of samples of the meat products to be tested, rubbing and enabling the samples to be uniform; weighing out the prepared samples; extracting with methanol + ethyl acetate solution, dehydrating by adding anhydrous sodium sulfate, and adding ascorbic acid to prevent monascus pigments in the samples from being oxidized; blowing the extract to be nearly dry, diluting the extract to volume with ethyl acetate + cyclohexane solution, and placing the extract for purification treatment; pouring the solution to be purified into a gel permeation chromatography column via a sampling ring; setting high performance liquid chromatography conditions; using the high performance liquid chromatography to determine the solution to be purified; and processing and analyzing data. The method is simple and convenient, rapid, sensitive, accurate and economic and is capable of detecting the monascus pigments in the meat products through qualitative and quantitative analyses of all components of the monascus pigments.

A method for detecting polycyclic aromatic hydrocarbons in pitch fume in pitch pavement construction comprises the steps of placing adsorption resin in a smoke collecting pipe according to the requirement that 2-5 g of adsorption resin is needed for each gram of pitch sample, weighing the pitch sample, placing the pitch sample in a sample container, and pushing the sample container into the central position of a smoke generating pipe; leading gas in a gas cylinder into the smoke generating pipe, controlling the flow velocity in the smoke generating pipe to be 0.05-0.5 m / s, rising the temperature of a tube furnace to the pitch pavement construction temperature of 100-180 DEG C; after constant temperature for 2-5 h, using a solvent to extract the adsorption resin sample where smoke is adsorbed, performing concentration, and performing gas chromatography-mass spectrum online (GC / MS) detection. The method has the advantages of being simple, convenient, practical and accurate in qualification and quantification.

The invention belongs to the technical field of analytical chemistry, and provides a detection method of glucosinolate compounds. According to the method, common secondary mass spectrum fragments of glucosinolate compounds are adopted, so that the purpose of high-efficiency qualitative analysis is achieved; in the secondary mass spectrum fragments, a set of precursor ion mode scanning qualitative method is constructed based on the fragments with m / z of 96.0, so that the detection sensitivity can be ensured, the qualitative accuracy can be improved, and false positive detection results are reduced; on the basis that the fragments with the m / z of 96.0 are used as quantitative ions, a set of multi-reaction monitoring (MRM) mode scanning quantitative method is constructed by utilizing glucosinolate compound standard substances, quantitative analysis of all glucosinolate compounds in a sample is completed, the problem that quantitative analysis cannot be achieved due to the fact that some standard substances are difficult to obtain is solved, and individual quantification and total amount determination of the compounds in the sample are efficiently completed.

The invention discloses a rapid detection method of sudan red in food, and belongs to the field of food safety. The rapid detection method of sudan red in food comprises four steps including sample pre-treatment, concentration distillation drying, thin layer chromatography, and HPLC measuring. The rapid detection method is capable of solving problems in the prior art that detection instrument is expensive; operation is complex; and popularization is difficult. The advantages are that: the extraction rate is high; the purification purity is high; the recovery rate is high; the rapid detection is rapid and reliable; operation is convenient; and cost is reduced.

The invention relates to a rapid analysis method for a light hydrocarbon component in soluble organic matter of hydrocarbon source rock. The rapid analysis method comprises the following steps that (1) a grinded hydrocarbon source rock sample is accurately weighed and placed into a pyrolysis cup; (2) a C24D50 standard sample and a phenanthrene-d10 standard sample with known concentrations are sucked by a syringe and then added into the pyrolysis cup; (3) the pyrolysis cup is placed in a fume hood, and after standard sample solvents are completely volatilized, the pyrolysis cup is placed into apyrolysis furnace to prepare pyrolysis; (4) a multifunctional pyrolysis instrument is directly connected to a gas chromatography triple-quadrupole mass spectrometry; (5) a liquid nitrogen cold well device is started; (6) a temperature programming condition of the pyrolysis furnace is set; (7) pyrolysis begins, pyrolysis gas enters capillary column with the temperature controlled by a cold well and is enriched, and after a set pyrolysis program is finished, a GC / MS / MS analysis program is automatically started for analysis; (8) the component of a compound is determined by combining characteristic ions and relative retention time of products and searching in an NIST 11 spectral library. The method can be used for realizing rapid and accurate one-time qualitative and quantitative analysis ofsoluble organic components of the hydrocarbon source rock.

The invention provides a test device for a chemical evaporation kinetics behavior, which is used for simulating a pressurizing test of a containment of a nuclear power station, and comprises a simulated pressurizing system, a chemical evaporation system and an analysis system. Wherein the simulated pressurizing system is used to simulating the pressure condition of a pressurizing test of the containment of the nuclear power station, and providing gas with a predetermined pressure to the chemical evaporation system; the chemical evaporation system is used to simulating the evaporation conditions of chemicals in the containment under different gas pressures and flow rates; and the analysis system is used to determine the type of gas volatilized by the chemicals under different gas pressuresand flow rates and related parameters. The test device reproduces the on-site environment by using the simulated pressurizing system and the chemical evaporation system, and simulates the chemical evaporation environment under the pressurizing condition in the containment, the obtained result is true and reliable, and the device can accurately and quantitatively analyze various complex compounds.

The invention relates to a method for measuring medicines and personal care products in water samples. The method comprises the following steps: 1) measuring standard samples of a target object and a substituent by using LC-MS / MS to calculate response factors of the target object and the substituent; 2) preparing simulated water samples and enriching the simulated water samples by connecting solid-phase extracting small columns with different polarity in series to calculate the absolute recovery rate of the target object and the substituent in the simulated water samples; 3) adding the substituent with a certain concentration into the to-be-detected water samples and enriching the water samples by using the solid-phase extracting small columns which are connected in series; 4) detecting the enriched water samples by using LC-MS / MS; 5) calculating the concentration Cx of the to-be-detected target object in the water samples. The method has the advantages of simplicity in pretreatment, low cost, low detection limit, high sensitivity and the like, and is suitable for sensitive and accurate qualitative and quantitative analysis of a trace amount of PPCPs in different water.

The invention provides a method for simultaneously detecting eight sterols in lucid ganoderma. The method comprises the following steps: a lucid ganoderma sample pretreatment step, an ultra-high performance liquid chromatography detection step, a compound mass spectrum information acquisition step, an ultra-high performance liquid chromatography triple quadrupole mass spectrum combined analysis method establishment step and a data analysis step. The method for simultaneously detecting the eight sterols in the lucid ganoderma can be used for carrying out accurate qualitative and quantitative analysis on eight sterols compounds in sporocarp, mycelia, spore powder and related products of the lucid ganoderma, is high in accuracy, high in sensitivity and strong in specificity, and overcomes thedefects of the conventional chemical method and high performance liquid chromatography.

The invention provides a method for extracting endocrine disruptors. The extraction method of the endocrine disruptor comprises the steps of firstly subjecting the sample to be tested to subcritical water extraction treatment, and then performing dispersion liquid-liquid micro-extraction treatment. The extraction method of endocrine disruptors of the present invention combines subcritical water extraction and dispersion liquid-liquid microextraction technology, so that the extraction method of endocrine disruptors of the present invention has high extraction efficiency for endocrine disruptors, and can effectively remove the influence of impurities, thereby realizing It can perform rapid and accurate qualitative and quantitative analysis of trace endocrine disruptors.

The invention provides a test device for a chemical evaporation kinetics behavior, which is used for simulating a pressurizing test of a containment of a nuclear power station, and comprises a simulated pressurizing system, a chemical evaporation system and an analysis system. Wherein the simulated pressurizing system is used to simulating the pressure condition of a pressurizing test of the containment of the nuclear power station, and providing gas with a predetermined pressure to the chemical evaporation system; the chemical evaporation system is used to simulating the evaporation conditions of chemicals in the containment under different gas pressures and flow rates; and the analysis system is used to determine the type of gas volatilized by the chemicals under different gas pressuresand flow rates and related parameters. The test device reproduces the on-site environment by using the simulated pressurizing system and the chemical evaporation system, and simulates the chemical evaporation environment under the pressurizing condition in the containment, the obtained result is true and reliable, and the device can accurately and quantitatively analyze various complex compounds.

The invention discloses a forensic medicine diatom test method.The forensic medicine diatom test method comprises the following steps that sulfamethazine, acrylic acid, acrylamide, N'N-methylene bisacrylamide, ammonium persulfate and deionized water are taken according to a proportion and fully mixed in a beaker; after oxygen is removed with nitrogen, the mixture is poured into a sandwich space formed by two glass slides and then put into an oven at the temperature of 60 DEG C for a polymerization reaction for 3 h, and film-state imprinting hydrogel is prepared; the obtained imprinting hydrogel is soaked in a 10% acetic acid solution, template molecules sulfadimidine in the imprinting hydrogel are removed through ultrasonic oscillation, then the imprinting hydrogel is soaked in a sample to be tested for 5-10 min and then taken out, and then the imprinting hydrogel is put under an optical microscope for observation; diatom on the filter film or a shot picture is checked, classified and counted in a manual recognition mode or an automatic computer recognition mode.The forensic medicine diatom test method is high in yield, efficiency and performance cost ratio, easy to popularize, accurate in qualitative and quantitative analysis and low in labor intensity.

The invention relates to a method for detecting trace nonylphenol (NP) in a soil sample or a plant sample, wherein the method includes the steps: 1) determining standard samples of nonylphenol and a substitute by GC-MS to calculate the relative response factor of nonylphenol and the substitute; 2) pretreating the soil sample and the plant sample; 3) adding the substitute with a certain concentration into the pretreated samples to be detected, and enriching nonylphenol and the substitute in the samples by Soxhlet extraction; 4) detecting the enriched soil and plant samples by GC-MS; and 5) calculating the concentration Cx of nonylphenol in the samples. The method has the advantages of simple pretreatment, low cost, low detection limit, high sensitivity and the like, and is suitable for sensitive and accurate qualitative and quantitative analysis of trace nonylphenol in bottom sediment, farmland and other soil samples and plant samples.

The invention provides a method for detecting 8 categories of restricted drugs in goat milk and products thereof, wherein the number of the restricted drugs is 74. The method comprises: (1) pre-treating a sample: extracting a sample to be detected with an acid organic solvent, purifying with a SPE column, and dissolving the purified liquid by using an initial mobile phase so as to be used for detection with UPLC-MS / MS; and (2) determining 74 restricted drugs: determining the pre-treated sample by using ultra performance liquid chromatography-LC-MS under the instrument condition specified by the method. According to the present invention, the method has advantages of more types of detected drugs, rich variety, short detection time, high sensitivity and accurate and stable results, can makesup for the absence of the simultaneous detection of multiple drugs in goat milk and dairy products, and provides the important significance for the assurance of the health body of consumers and the improvement of the export competitiveness of goat milk and dairy products.

The invention discloses a method for detecting a formaldehyde carbonylation reaction product by high performance liquid chromatography. The method comprises the following steps: (1) preparing a liquid chromatography mobile phase; (2) preparing a mixed standard stock solution, namely respectively weighing glycollic acid, ethylene glycol, a glyoxylic acid aqueous solution, acetic acid, acetaldehyde and a formaldehyde aqueous solution, putting into a volumetric flask, fixing the volume by using an organic solvent, and uniformly shaking to obtain the mixed standard stock solution; (3) preparation of standard solutions: respectively taking 5 parts of the mixed standard stock solution in the step (2), putting the mixed standard stock solution into the volumetric flask, fixing the volume by using an organic solvent, and uniformly shaking to obtain 5 series of standard solutions with different concentrations; (4) establishment of chromatographic analysis conditions; (5) making a standard curve: performing liquid chromatographic analysis, and fitting by taking the concentration as an abscissa and the peak area as an ordinate to obtain the standard curve; and (6) analyzing a reaction product. The method provided by the invention is simple and convenient to operate, good in repeatability, small in analysis error, high in precision and good in sensitivity.

The invention relates to the field of algae inspection, and specifically discloses a forensic diatom inspection method based on a filter membrane. In the present invention, after the vacuum-filtered filter membrane is transparentized, the transparent filter membrane can be directly observed under an optical microscope. The detection method of the invention is easy to operate, high in detection efficiency, does not need to rely on complex instruments, and can be detected in basic forensic laboratories, and has wider applicability.

The invention discloses a derivatizing reagent of polyhydroxy compound. The reagent is composed of DMSO, 1-methylimidazole and acetic anhydride. The reagent of the invention can carry out acetylation derivatization reaction on the basis of maintaining native conformation of simple sugar, single derivatization product can be obtained after derivatization reaction, and qualitative or quantitative analysis can be accurately carried out on various polyhydroxy compounds, thereby avoiding the interference of various derivatization products in analysis.

The invention belongs to the technical field of detection methods and in particular relates to a method for detecting iso-octyl p-methoxycinnamate in textiles. The method comprises the following steps: 1, sampling textiles; 2, weighing a certain amount of samples to be added into a container, adding methanol into the container, and performing ultrasonic extraction on the container in an ultrasoniccleaner for 10 minutes to an hour so as to obtain an extracting solution; 3, filtering the extracting solution obtained in the second step so as to obtain a to-be-detected solution; 4, analyzing theto-be-detected solution obtained in the third step by using an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MSMS). Compared with the prior art, the method disclosed by the invention can simply, rapidly, accurately and reliably detect the content of the iso-octyl p-methoxycinnamate in textiles and meet detection requirements of the iso-octyl p-methoxycinnamate in Washington Child Product Safety Act.