199 results about "Gas Chromatography/Tandem Mass Spectrometry" patented technology

The invention relates to a method for detecting the plasticizer content in a solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry, and the method combines an isotope internal standard and the headspace solid phase microextraction gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS/MS) analysis for qualitative or quantitative analysis of a dimethyl phthalate plasticizer in a sample. The method mainly comprises the following steps of: a) mixing the solid sample with the isotope internal standard, and conducting extraction with headspace solid phase microextraction equipment; b) carrying out sample analysis; C) performing GC-MS/MS analysis; and d) implementing result treatment and quantitative analysis. The method of the invention is a fast, efficient, sensitive analysis method.

The invention discloses a method for detecting aromatic amine in cigarette mainstream smoke by using a gas chromatography-tandem mass spectrometry. The method is characterized by comprising the following steps of: catching aromatic amine compounds in a particulate matter in the cigarette mainstream smoke by using a Cambridge filter; extracting by using hydrochloric acid solution, washing by usingdichloromethane, reducing by using sodium hydroxide and then extracting by using normal hexane, and performing derivatization by using pentafluoropropionic anhydride and trimethylamine hydrochloride;and concentrating and detecting by using the gas chromatography-tandem mass spectrometer (GC-MS/MS) so as to measure the content of the main aromatic amine compounds in the cigarette mainstream smoke. Compared with the conventional method for analyzing the aromatic amine in the cigarette mainstream smoke, the analysis and measurement method has the advantage of simplifying the pretreatment of a sample along with higher sensitivity, high experimental repetitiveness and recovery rate and applicability to analysis of a large batch of samples.

The invention relates to a method for measuring phthalic ester in atmospheric particulates, belonging to the field of analysis of trace pollutants in the environment. The method uses a quartz filter membrane to collect particulates, takes dichloromethane as extracting solution, uses an ultrasonic extraction method for extraction, carries out nitrogen-blowing concentration and finally uses a gas chromatography and tandem mass spectrometry (GC/MS) for analysis and measurement, thus accurately and fast analyzing the phthalic ester in the atmospheric particulates. The specific sampling and analysis measuring method comprises the following steps: after being baked at high temperature and weighted in a balanced manner, the quartz filter membrane is sampled for 12-48 hours, the sampled and weighted filter membrane is cut into shreds which are placed into a centrifugal tube, 5-30mL of dichloromethane is added, ultrasonic extraction is carried out for 10-30 minutes, the extracting solution is filtered and collected, all the steps are repeated for one time, the extracting solutions are combined and become 3-6mL in concentration by nitrogen blowing, the combined solution is transferred into a concentrating tube for continuously blowing to be below 2mL, an internal label is added, the obtained solution is constant in volume by dichloromethane and is transferred into an automatic sampling bottle, and finally accurate measurement is carried out by using debugged GC/MS. The developed measuring method is simple and fast and has the characteristics of high recovery ratio, low detection limit, high sensitivity, matrix disturbance resistance and the like.

The invention discloses a solid-phase extraction-gas chromatography tandem mass spectrometry detection method for pyrazol bactericides in wine. According to the method disclosed by the invention, five pyrazol bactericides such as penflufen, fluxapyroxad, isopyrazam, rabenzazole and furametpyr in a wine sample can be simultaneously measured. The method comprises the following steps: adding ultrapure water into the wine sample, diluting to obtain a to-be-detected solution; purifying the to-be-detected solution by using an HLB solid-phase extraction column, and separating by using a C18 reversed-phase column; performing qualitative analysis on a target analyte in a multiple-reaction monitoring mode by comparing retention time and ion pair information, and performing external standard quantification. The method has the advantages of high analysis speed, high sensitivity, high reproducibility and high accuracy, and a novel detection method is provided for evaluating the quality of the wine sample.

The invention relates to a determination method for six residual plant-growth regulators in a bean sprout, especially to a method for simultaneous determination of six residual plant-growth regulators in the bean sprout by using gas chromatography-tandem mass spectrometry. Six plant-growth regulators involved in the invention are composed of 4-chlorophenoxyacetic acid, 2,4-dichlorophenoxyacetic acid, naphthylacetic acid, indoleacetic acid, 2,4-D-butyl ester and indolebutyric acid. The method comprises the following steps: 1) sample treatment; 2) determination, wherein gas chromatography-tandem mass spectrometry is employed; 3) drafting of a standard curve; 4) blank test; and 5) result calculation and description. The determination method employs gas chromatography-tandem mass spectrometry for simultaneous determination of the six residual plant-growth regulators in bean sprout; and the method is simple, convenient, rapid, accurate and reliable, and the lower determination limit, recovery rate and precision of the method all accord with requirements.

The invention discloses a method for measuring methyl eugenol in the mainstream smoke of cigarettes. The method comprises the steps of preparation of an internal standard solution, preparation of a standard working solution, preparation of a sample solution, gas chromatography-tandem mass spectrometry, drawing of a standard working curve and calculation of a sample result. According to the method, a C18 solid-phase extraction column is used for purifying sample extract for the first time, a dehydration technology is used for carrying out back-extracting on a target object, and then a gas chromatography-mass spectrometry selective ion monitoring method is used for measuring the methyl eugenol content of the mainstream smoke of the cigarettes; an internal standard method is used for quantification, so that constant column is not required, and errors caused by the reproducibility of the pretreatment method and precision problems of an apparatus can be reduced; a DB-5MS column with the best peak shape and the best separation effects is selected as a separation column, and GC-MS (gas chromatography-mass spectrometry) detection mode capable of simultaneously providing qualitative and quantitative information is adopted, so that the sensitivity of a response signal is improved, and the accuracy of an analysis result is ensured.

The invention relates to a method for determining phthalate ester in soil, belonging to the filed of analysis of trace contaminants in the environment. The method comprises the following steps: taking dichloromethane as an extract, and extracting by an ultrasonic extraction method; carrying out nitrogen blowing concentration; and finally analyzing and determining by gas chromatography tandem mass spectrometry (GC/MS) so as to accurately and quickly analyze phthalate ester in the soil. The specific analytical determination method comprises the following steps: taking a certain amount of naturally air-dried soil in a conical flask, and adding 10-30mL of dichloromethane; ultrasonically extracting for 5-30min, and collecting the extract after filtering; repeating the steps twice, and combining the extract; nitrogen-blowing to 3-6mL, and transferring to a concentration tube and then continuing to blow to below 2mL; adding internal standard, fixing volume with the dichloromethane, and transferring to an automatic sample bottle; and finally, accurately determining with debugged GC-MS. The determination method developed by the invention is simple and fast, and has the characteristics of high recovery rate, low detection limit, high sensitivity, matrix interference resistance and the like.

The invention discloses a method for detecting polyaromatic hydrocarbon and phthalate in a plant extract. The method comprises the following steps of: firstly pretreating the plant extract and secondly detecting polyaromatic hydrocarbon and phthalate in the plant extract through a gas chromatography-tandem mass spectrometry method. The method is simple and convenient to operate, has the advantages of low detection limit and good repeatability, and is applicable to detection of PAHs and PAEs in plant extracts.

The invention relates to a method for detecting four tobacco-specific nitrosamines (TSNAs) in lateral exhaust gas of cigarettes by virtue of gas chromatography-tandem mass spectrometry. The method is characterized by comprising the steps of capturing the lateral exhaust gas of the cigarettes by virtue of a lateral fishtail cover preprocessed by an ascorbic acid solution and a Cambridge filter preprocessed by an ascorbic acid saturated methanol solution, washing the lateral fishtail cover with a hydrochloric acid solution, adding the washed hydrochloric acid solution and an TSNAs internal standard solution into a container in which the Cambridge filter is collected, extracting the Cambridge filter, processing extraction solution by virtue of a solid phase extraction column to obtain an eluate, drying the eluate with nitrogen, redissolving by virtue of dichloromethane to obtain a sample, and analyzing the sample by virtue of the gas chromatography-tandem mass spectrometry (GC-MS/MS). According to the method, the disadvantages of tedious preprocessing process, low detection sensitivity and strong matrix effect in an existing method are overcome, the preprocessing step of the sample is simplified, and the consumption of organic solvents is reduced; the method has the advantages that the detection is accurate, the sensitivity is high, and the repeatability is good.

The invention belongs to the technical field of tobacco analysis and particularly relates to a method of measuring contents of various organic acids in tobacco and tobacco products. The method hereinincludes the steps of mixing well a sample under test, a saponifying agent and an internal standard substance, refluxing at 60-70 DEG C, performing solid-liquid separation, concentrating filtrate under reduced pressure to dryness, and dissolving in water to obtain solution A; adjusting pH of the solution A at 0 DEG C to 1.5-2.5, and adding an extracting agent to carry out extracting; adding a silanized derivative into extract to carry out derivation, and using gas chromatography tandem mass spectrometry to perform detection and analysis. A saponifying-silanization-GC-MS/MS analytic method is established for the first time herein and is suitable for analyzing 53 amino acids in an analysis sample; the target analytes include low molecular weight organic acids, half-volatile organic acids andadvanced fatty acids, and the types are more in quantity and more comprehensive. GC-MS/MS analysis parameter sensitivity is higher; the low contents of organic acids in tobacco and tobacco products can be detected.

The invention relates to a method for determining a content of methanol in insulation oil, which belongs to the technical field of analysis and test. The method mainly utilizes a headspace sample injector to be combined with a gas chromatography tandem mass spectrometry, and adopts an automatic headspace sample injection, so that compared with a manual sample injection way, the method has the characteristics of high accuracy, and higher repeatability, ensures that the sample can be consistently treated before entering the gas chromatography, avoids the interference of other substances in the detection process, and improves the accuracy for determining the content of the methanol; and further, the gas chromatography is used as a mass spectrometry front-end separation system, a sample to be detected is separated by virtue of the gas chromatograph and is then directly led into the mass spectrometry to be detected, so that the complex process for preparing and transferring the sample can be avoided, and the sample can be prevented from being polluted; and moreover, the consistence of the sample feeding amount of the mass spectrometry can be ensured, the mass spectrometry is used as a detector to qualitatively or quantitatively detect the content of the methanol, and finally a detect object can be accurately qualified and quantified.

The invention, which belongs to the technical field of tobacco component detection, relates to an analytical method for quantitatively measuring super-multi-target aroma components in tobacco. The method comprises the following steps that: a tobacco sample is immersed in an acidic buffer solution and extraction is performed by an organic solvent; a multi-walled carbon nanotube is used as a reversesolid phase-dispersed adsorbent and vortexing and centrifugation are performed to purify the sample; and then simultaneous detection of 345 kinds of aroma component in tobacco is realized by combining gas chromatography-tandem mass spectrometry. The method has advantages of simple and rapid operation, high flux, low cost, low solvent dosage, good environmental friendly effect, wide range of analytical compounds, high accuracy, high precision, high sensitivity and high repeatability and can satisfy the demand of rapid detection and analysis of aroma component in tobacco.

The invention discloses a method for simultaneously detecting phenol, NNK and benzo-[a]-pyrene in main stream smoke of a cigar by using gas chromatography-tandem mass spectrum. The method is characterized by comprising the following steps: gathering phenol, NNK and benzo-[a]-pyrene in the main stream smoke of the cigar by using a Cambridge filter; extracting the Cambridge filter by using an extracting solution; detecting the extracting solution by adopting gas chromatography-tandem mass spectrum (GC-MS/MS); and measuring the content of phenol, NNK and benzo-[a]-pyrene in the main stream smoke of the cigar. In comparison with an existing assay method for independently assaying phenol, NNK and benzo-[a]-pyrene in the main stream smoke of the cigar, the analysis and assay method disclosed by the invention has the advantages of simplifying the pretreatment of a sample, improving the detection sensitivity, also increasing the analysis and assay flux and being suitable for rapid analysis of large-batch samples.

The invention discloses a determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke and belongs to the technical field of tobacco chemical inspection. The determination method comprises the steps that graphitized carbon black, N-propyl ethylenediamine bonded silica gel, anhydrous magnesium sulfate and a sodium chloride adsorbing agent are added into a sample extracting solution, centrifugation and filtration are carried out after dispersive solid-phase extraction, and a to-be-tested solution is obtained; the to-be-tested solution is taken for gas chromatography-tandem mass spectrum analysis, the content of volatile N-nitrosamine in the to-be-tested solution is obtained with reference to a standard curve, and the content of volatile N-nitrosamine in a sample is obtained through calculation. The method is high in detection sensitivity, good in accuracy and repeatability and easy, fast and efficient to operate, the relative recovery rate is between 82.4% and 112.4%, and the intra-day precision and inter-day precision are smaller than 9.1% and 8.2% respectively.

The invention discloses a method for quantitative analysis of main pyrazine flavor substances in cigarette mainstream smoke and relates to a method for gas chromatography-tandem mass spectrometer-based determination of eight main pyrazine flavor substances such as 2-methylpyrazine, 2, 5-dimethylpyrazine, 2, 6-dimethylpyrazine, 2-methoxypyrazine, 2, 3, 5-trimethylpyrazine, 2-ethyl-3-methylpyrazine, 2, 3, 5, 6-tetramethylpyrazine and 2-acetylpyrazine in cigarette mainstream smoke. The method comprises internal standard solution, standard work solution and sample solution preparation, gas chromatography-tandem mass spectrometry analysis and determination result calculation. The improved detection method can be operated simply, has response sensitivity and quantitative analysis accuracy, effectively reduces complex sample matrix-caused interference and is suitable for quantitative analysis of a trace quantity of a target object in a complex flue gas matrix.

The invention discloses a pretreatment and quantitative analysis method for rapid determination of pesticide residue in tea. The method comprises the following steps: 1) extraction: soaking the tea in water, adding acetonitrile for extraction of pesticide residues, then adding sodium acetate for salting out, so as to separate an organic phase and a water phase and obtain an acetonitrile layer of a tea extract; 2) purification: step 1) adding activated carbon, N-Propylethylenediamine and magnesium sulfate in the tea extract for purification, so as to obtain a supernatant namely a liquid to be tested in the fast determination of pesticide residues in tea; and 3) using a standard curve method to conduct quantitative analysis by gas chromatography-tandem mass spectrometry. In the pretreatment process, the extract contains considerably reduced tea matrix; the purifying effect is good, and the recovery rate of pesticide is basically not affected, so as to greatly improve the pretreatment effect; and the gas chromatography-tandem mass spectrometry is combined for separation detection of the pesticide. The method greatly improves the separation efficiency of pesticide, reaches high detection sensitivity and accuracy and good reproducibility.

The invention discloses a solid-phase membrane extraction and gas chromatography-tandem mass spectrometry detection method of organic chlorine compounds in a water body. A C18 solid-phase extraction membrane is used for achieving enrichment of the organic chlorine compounds in the water body. A gas chromatography-tandem mass spectrometry detection method is used for detection. The method is few in operation step, high in sensitivity and good in reproducibility and can be used for measuring the content of the organic chlorine compounds in the water body.