100results about How to "Qualitative and quantitative accuracy" patented technology

The invention discloses decompressed purge-and-trap processing equipment for a non-volatile organic compound in a water sample and a processing method thereof. The invention is characterized in that the equipment is formed by sequentially connecting a sample heater (1), a purge bottle (2), a trapper (3), a pressure controller (4) and a pump (5), wherein purge gas (6) is connected with the purge bottle (2) through a purge gas inlet (7); the purge bottle is connected with the trapper (3) through a purge gas outlet (8); the trapper (3) is connected with the pump (5) through the pressure controller (4); the gas trapped by the trapper (3) is taken out and then placed into a heater (13) of the trapper; chromatographic carrier gas (14) is connected with a chromatographic injection port (12) in a column oven (11) through the trapper (3) and a transmission pipeline (15); and the chromatographic injection port is connected with a chromatographic detector (9) through a chromatographic column (10). The processing method comprises the following steps: forming a negative pressure environment around a test sample under the action of the pump, and increasing the vapor pressure of the non-volatile organic compound under the negative pressure environment; purging the bottom of the sample by utilizing inert gas so that the target compound can be trapped by the trapper after being blown out from the sample; and finally, resolving the target compound at high temperature and then carrying out chromatographic analysis.

The invention belongs to the field of analytical chemistry detection, and relates to a method for detecting valsartan and content of N-nitrosodimethylamine in the preparation thereof. The detecting method comprises the steps of: grinding an object under test and weighing fine powder; adding a polar organic solvent in the powder and filtering by a filter membrane to prepare a solution under test; preparing a standard curve solution; acquiring a standard chromatogram map and a regression equation; detecting the solution under test by a gas chromatography-thermal energy analyzer to acquire a chromatogram map of the solution under test; if a chromatographic peak corresponding to the chromatographic peak in a standard curve chromatogram map exists in the chromatogram map of the solution under test, showing that the solution under test contains the N-nitrosodimethylamine; and calculating to acquire the concentration of the N-nitrosodimethylamine according to the area of the chromatographic peak in the chromatogram map of the solution under test. The principle of the method is reliable; the experimental operation is simple; the measuring precision and accuracy are ensured by using the high-separation efficiency of the capillary gas chromatography and the high-selectivity and the high-sensitivity of the thermal energy analyzer; and thus, the analysis time and test cost are greatly saved.

The invention relates to a method for detecting the liquid quality of an antipsychotic drug in serum or plasma and pretreatment of a specific purification material of the antipsychotic drug. The method comprises the following steps: a serum or plasma sample is subjected to protein precipitation by a certain proportion of organic reagents; a supernatant obtained through centrifugal precipitation ispretreated with a specific purification material to obtain a purified sample solution, the purified sample solution is subjected to liquid chromatography-tandem mass spectrometry detection and analysis, and eight antipsychotic drugs including olanzapine, clozapine, quetiapine, aripiprazole, flupiperidinol, risperidone, pariperidone and ziprasidone in serum or plasma are detected at the same time.The pretreatment of the specific purification material is a mixed solid-phase extraction column taking silica gel as a matrix, and the blood is purified by the specific purification material, so thatthe interference of the matrix in the blood can be removed, the matrix effect of eight antipsychotic drugs can be improved, and the recovery rate of the antipsychotic drugs can be better ensured.

The invention discloses a rapid detecting method for measuring the acrylamide content in liquid state seasoning with a complex matrix by means of a combination of a matrix solid-phase dispersion method and an ultra-high performance liquid chromatography-cascading quadrupole gas chromatograph-mass spectrometer, and belongs to the field of detecting methods for acrylamide. According to the rapid detecting method for the acrylamide, samples are extracted and purified by means of the matrix solid-phase dispersion method to obtain a product A; rotary evaporation and concentration are carried out on the product A, the product A is washed by means of ethyl acetate and blown to be dried by means of nitrogen, and water ultrasonic dissolution is carried out on the product A; debinding is carried out by means of normal hexane, a lower layer solution is filtered after centrifugal separation, then UPLC/MS/MS detection is carried out, and quantification is achieved by means of an internal standard method. Compared with an existing general detecting method, the rapid detecting method is high in throughput, rapid, accurate, efficient and safe, can accurately detect the content of the acrylamide in the seasoning of acrylamide and the like with complex matrixes, and meets normal monitoring requirements for food safety in production of enterprises.

The invention discloses an all-isotope internal standard mass spectrometry quantitative method for a neurotransmitter metabolite. The method is an all-isotope derivative internal standard quantitative method for the neurotransmitter metabolite by adopting a neurotransmitter metabolite standard substance and a derivative of a stable isotope labeling reagent as quantitative internal standard references and a liquid chromatography-tandem quadrupole mass spectrometry as detection means. Qualitative and quantitative analysis can be carried out on a plurality of neurotransmitter metabolites at the same time, so that the all-isotope internal standard mass spectrometry quantitative method has the advantages of being simple in sample preparation, accurate in qualitative and quantitative analysis, high in throughput and low in cost, and has an expectable clinical application prospect. According to the method disclosed by the invention, the defects that a current neurotransmitter metabolite test is low in qualitative and quantitative accuracy and high in cost and only a few of substances can be analyzed at the same time are compensated.

The invention provides a method for rapidly detecting multiple antibiotic residues in livestock and poultry manure. The method for rapidly screening and affirming the multiple common antibiotic medicine residues in the livestock and poultry manure is established by using an improved QuEchERs technology as a sample pretreatment technology and a highly-sensitive Waters Acquity UPLC-AB5500 liquid chromatograph-triple quadrupole-linear ion trap tandom mass spectrometer as a detection means. The method has the advantages of short detection cycle, high detection efficiency, good reliability and thelike.

The invention discloses a negative pressure extraction and separation system and separation method for semi-volatile organic matter and non-volatile organic matter in samples. The present invention forms a continuous negative pressure and heating environment around the tested sample through the action of a vacuum pump and a heater. Under this environment, semi-volatile organic compounds and non-volatile organic compounds produce properties similar to volatile organic compounds, gasify to form steam and combine with the sample The matrix is ​​fully separated, and the separated organic matter vapor is transferred from the sample transfer pipeline to the adsorbent for adsorption and enrichment by the suction of the vacuum pump, and then the adsorbent containing the target compound is directly injected into the sample for analysis or thermal analysis, solvent desorption, and then enters the gas chromatography or gas chromatography / mass spectrometer for analysis. The extraction, purification and sample concentration of the present invention are completed simultaneously, greatly reducing the analysis cost and time.

The invention discloses a method and system for measuring the content of gas components in fuel hydrogen, a gas sample is quantitatively sampled through a first quantitative loop, then a first chromatographic column and a first exhaust valve are conducted, the front main components of hydrogen are emptied through the first exhaust valve, and when oxygen and argon are separated from the first chromatographic column, the first chromatographic column is communicated with a second chromatographic column, oxygen and argon are carried into the second chromatographic column, when oxygen and argon completely enter the second chromatographic column, the first chromatographic column is switched to be communicated with the first exhaust valve, and main components after hydrogen are discharged. When nitrogen is separated from the first chromatographic column, the first chromatographic column is switched to be communicated with the second chromatographic column, the nitrogen, methane and carbon monoxide are carried to the second chromatographic column, and the content of the nitrogen, methane and carbon monoxide is detected by the pulse discharge helium ionization detector, so that a gas sample can be prevented from being separated at one time, and the fuel hydrogen content is high; the separated permanent gas is easily separated from the first chromatographic column, so that the detection result is inaccurate, the detection efficiency can be improved as much as possible through twice completion, and the separation time is prevented from being prolonged.

The invention relates to a preparation method of a fluorescent nanoprobe based on a two-dimensional lanthanum metal organic skeleton MOF-La, a prepared probe material and application of the prepared probe in a biosensor. The preparation method comprises the following preparation steps: (1) in an alkali solution, adding 2,2'-thiodiacetic acid or 2,2'-thiodiacetin, La<3+> lanthanum ion inorganic salt, and reacting for 10 to 30 h at the temperature of 120 to 180 DEG C; adding an obtained crystal into an organic solvent, carrying out ultrasonic treatment, performing centrifugation, dispersing into an organic solution of n-butyllithium, and reacting for 15 to 25 h at the temperature of 20 to 30 DEG C under the protection of inert gas, so as to obtain a two-dimensional MOF-La nanomaterial; dispersing the two-dimensional MOF-La nanomaterial in a buffer solution, adding fluorescently-labeled nucleotide chains, and performing centrifugation after reaction at room temperature to obtain the material. The preparation method is simple in preparation conditions, convenient in operation and low in cell toxicity, and the obtained probe has the characteristics of high selectivity and high sensitivity, so that a false positive result is avoided, qualitative performance and quantitative performance are more accurate, and the probe has a good application prospect.

The invention relates to a detection method of annular methylsiloxane in sediment, and aims at solving the problems that for an existing method for detecting methylsiloxane, the detection time is long, and accurate qualitativeness and quantification analysis cannot be achieved when impurities exist. The method comprises the steps that 1, a sample to be detected is pretreated through an oscillation extraction method; 2, GC-MS-MS instrument parameters are set; 3, a standard solution is detected; 4, the sample to be detected is detected. The method for detecting the annular methylsiloxane in the sediment has the advantages that the detection time is short, operation is easy, the pretreatment effect is good, interference can be effectively eliminated, and qualitativeness and quantification to the annular methylsiloxane are accurate.

The invention discloses a method for detecting ethrel. The method includes the following steps: ethrel in a sample is extracted; a detection solution of ethrel derivatives is prepared, the sample is extracted through an analytical reagent, then sulfuric acid is used as a protective agent, heptafluorobutanol and heptafluorobutyric anhydride are used as derivatization reagents to make the ethrel inthe sample derive into the derivatives under the temperature condition of 60-120 DEG C, and then a chromatography reagent is added to obtain the detection solution; a derivative ethrel working solution is prepared; GC-MS/MS chromatographic analysis is conducted; an external standard method is used for quantification, the mass concentration of a target object is used as an abscissa, the corresponding peak area is used as an ordinate, and a standard curve is drawn. The ethrel is stable in the process of derivation, the speed of an esterification reaction is high, the speed of derivation is high,sensitivity is high, qualitative and quantitative detection is accurate, operation is easy, use of hypertoxic reagent diazomethane can be avoided, and the environment is protected.

The invention discloses a rapid instrument analysis method for the residual quantity of hydroxylamine in a reaction solution. The method comprises the following steps: 1, carrying out a derivatizationreaction on the hydroxylamine-containing reaction solution and benzaldehyde to generate benzaldoxime; and 2, determining the content of the benzaldoxime in the above obtained derivatization solutionof the reaction solution through high performance liquid chromatography, and calculating the content of the hydroxylamine in the original reaction solution according to the content of the benzaldoxime. The analysis and detection method provided by the invention has the advantages of simplicity in operation, high accuracy, strong specificity, high sensitivity, fast analysis speed and high efficiency. Compared with the prior art, the method allows determination using a high performance liquid chromatograph to be carried out after the derivatization reaction, and realize accurate qualitative andquantitative determination in order to meet needs in researches and production.

The invention discloses a method for analyzing an electronic cigarette tar component through combination of dynamic pin capture and gas chromatography and mass spectrometry. The method comprises inserting a dynamic capture pin connected with a circular purging apparatus into a head-space bottle, starting the circular purging apparatus, performing heating at 50 DEG C for 30 min, inserting the dynamic capture pin into a GC-MS injection port to perform desorption, and then performing GC-MS qualitative analysis. According to the method, a non-equilibrium continuous adsorption process is adopted, the sample enrichment efficiency can be greatly improved, and volatile components in a sample are extracted from the sample. The dynamic capture pin is used for capture, adsorption and sampling, and after desorption, the sample enters a detector for analysis. The method is suitable for sampling and analyzing a trace amount of an organic target component. The method allows the trace-amount componentto be enriched, and is high in sensitivity, wide in adsorption range, good in reproducibility and easy to operate. After adsorption, the trace-amount component can be sealed and stored. A by-productproduced in an adsorption process is less. The method is accurate in qualitative and quantitative analysis, simple to operate, and relatively long in life.

The invention discloses a small molecular monocarboxylic acid derivatization-liquid chromatography detection method. Chromatographic conditions are as follows: the quantitative detection wavelength is223nm, a chromatographic column is Agilent SB-C18, and the temperature of a column oven is 35 DEG C; acetonitrile and water are used as a mobile phase, and the fixed flow speed is 0.8mL/min; the gradient elution procedure is as follows: the volume ratio of the acetonitrile is 10% at 0 minute, is increased to 70% at 30 minutes and is reduced to 10% at 32 minutes, and the procedure ends at 34 minutes. Several monocarboxylic acid derivatization-liquid chromatography detection methods provided by the invention have qualitative and quantitative accuracy, have the sensitivity which is at least 2 orders of magnitude higher than that in a direct method, can be applied to detection of butyric acid, and have very obvious advantages.

The invention provides a method for determining chlorantraniliprole residues in vegetables. Acetonitrile is used to homogeneously extract chlorantraniliprole residues in a sample, anhydrous magnesiumsulfate is added to remove water, sodium chloride salting-out is carried out, a supernatant is obtained after whirling, oscillation and centrifugation, acetonitrile is added to the supernatant, wateris used for fixing the volume, the mixture is passed through a 0.22[mu]m filter membrane after uniform mixing, then the mixture is detected by a high performance liquid chromatography-tandem mass spectrometer equipped with an electrospray ion source and is monitored by multiple events in sections, then the mixture is quantified by an external standard method, and a standard series working curve isprepared with blank matrix liquid without components to be detected. According to the method, the addition recovery rate is between 97.6% and 117.9%, the average relative standard deviation (RSD) isbetween 1.5% and 6.0%, and when the addition detection limit is 0.001mg/kg, the signal-to-noise ratio of an instrument is greater than 3. Through verification, the method is simple, rapid and reliablein operation, accurate in qualitative and quantitative analysis, high in sensitivity, good in repeatability, and easy to realize analysis of a large batch of samples. The minimum limit value of chlorantraniliprole residues in vegetables in China is 0.01mg/kg, and the method meets this requirement.

The invention discloses a method for determining acrylamide in edible oil. The method comprises the following steps: (1) performing pretreatment; (2) preparing a standard solution; (3) obtaining a liquid chromatogram and a regression equation; (4) performing qualitative analysis; (5) performing quantitative calculation, and quantifying by adopting a stable isotope internal standard method: calculating the concentration of acrylamide by adopting the regression equation in the step (3) according to the areas of chromatographic peaks of an acrylamide quantitative ion pair and a 13C3 acrylamide internal standard quantitative ion pair in a sample. The pretreatment operation is simple and efficient, the automation degree is high, the gel chromatography online purification is achieved, the problem that acrylamide is prone to loss in pretreatment is solved, and the method is good in recovery rate, high in sensitivity and accurate in qualitative and quantitative analysis.

The invention discloses a first detection method of a high boiling point solvents fragrance samples before using gas chromatography mass spectrometry prior. Certain steps: weight 10~50g high boiling point solvents fragrance samples and out it into a 30 to 80 degreeC three-mouth flask; puts 600~1500ml/min ventilation velocity of inert gas flow and nitrogen flow and brings out the flavor components effectively, receives solvent absorption in -25~-15 degreeC, receives the self-enrichment samples by direct injection GC-MS detection. The invention method can analyze the essence of effective qualitative and quantitative composition accurately and improve the recovery efficiency, shorten recovery time, reduce the loss of effective ingredients, eliminate impurity effectively in the course of processing.

The invention relates to an analysis method of acrylic resins and in particular relates to an analysis method of acrylic resin monomers in acrylic resin-containing mixtures. The analysis method is capable of determining the natures of the acrylic resin monomers and quantifying the acrylic resin monomers; the difficulty that the acrylic resin monomers only can be selectively quantified by nuclear magnetism is avoided; the analysis method is simple and convenient to operate without excessive precision operation requirements, wide in application range and suitable for all types of acrylic resins or acrylic resin-containing mixtures.

The invention relates to a method for determining aniline in soil and sediment. The method comprises the following steps: 1, pretreating: weighing 2 g of soil or sediment to be determined, putting thesoil or sediment into a headspace bottle, adding sodium chloride with the mass of more than 4 g, adding a pure water solution with the pH value of more than 11, adding an internal standard substance1,2-dichlorobenzene-d4, tightening a bottle cap, and putting the bottle into a sample introduction disc for determination; 2, carrying out solid-phase micro-extraction: uniformly mixing before extraction, and extracting by using a solid-phase micro-extraction fiber head; and 3, determining by using a gas chromatography-mass spectrometer. A solid-phase microextraction process is adopted, so that asoil or sediment sample does not need to be pretreated, and manpower, time, reagents and the like are saved; the solid-phase microextraction process is adopted, the detection limit can be lower without a concentration step, the split ratio is set to be 20, and a larger split ratio can be set if the soil with higher concentration is measured; and gas chromatography-mass spectrometry determination is adopted, and simultaneous determination of selective ion scanning and full scanning is adopted, so qualitative and quantitative determination of aniline is more accurate.

The invention discloses a method for determining the content of 1,3-propanesultone, belongs to the field of analysis and detection and in particular discloses a method for determining the content of the 1,3-propanesultone by using gas chromatography-mass spectrometry. The method comprises the following steps: putting a proper amount of uniform sample into a glass centrifugal pipe; adding n-hexane and uniformly mixing by vortex; carrying out ultrasonic extraction at a room temperature and centrifuging at a high speed; taking supernatant liquid and repeatedly extracting and combining the supernatant liquid; making the volume constant until the volume is 50mL; centrifuging at a high speed; metering 2mL at a middle scale of a solution to be detected by using a pipette; filtering with a filtering membrane, and carrying out gas chromatography-mass spectrometry analysis; quantifying with an external standard method. The method disclosed by the invention is simple and rapid, and accurate in qualitative and quantitative properties; the interference of sample matrix is effectively avoided and detection requirements can be met.

According to a method for rapidly determining various pesticide residues in ecological textile based on a liquid chromatography-triple quadrupole-tandem mass spectrometry technology, provided by the invention, an improved QuEchERs technology is used as a pretreatment means, and a high-sensitivity liquid chromatography-triple quadrupole-linear acceleration ion trap tandem mass spectrometer is used as a detection means, a rapid screening and confirmation technology for simultaneously detecting various common pesticide residues such as organophosphorus, pyrethroid and carbamate insecticides, bactericides and herbicides in the ecological textile matrix is established, and the method has the advantages of multiple detection types, low detection limit, short detection period, high detection efficiency and the like.

The invention relates to an ultra-high performance liquid chromatography-high-resolution quadrupole flight time mass spectrometry method for extracting lipids in freeze-dried food based on an ultrasonic single solvent, which is characterized in that the lipids in the freeze-dried food are extracted by using an ultrasonic-assisted single solvent, and then positive and negative ions are quickly scanned by using ultra-high performance liquid chromatography-high-resolution quadrupole flight time mass spectrometry within 34 min to realize rapid qualitative and quantitative analysis of the lipids. The method is fast and simple to operate, the extraction is not affected by protein, the extraction time is short, the toxicity of the solvent is small, the repeatability is good, the recovery rate ofvarious lipids is high, and the purpose of high coverage of the lipids is achieved.