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

An analytical technique wherein gas chromatography is coupled to tandem mass spectrometry in order to separate, identify, and quantify substances in a sample.

Gas chromatography-mass spectrometer (GC-MS)/MS measuring method for 20 pesticide residues in tobaccos and tobacco products

A gas chromatography-mass spectrometer (GC-MS) / MS measuring method for 20 pesticide residues in tobaccos and tobacco products is characterized by comprising adding acetonitrile and an internal standard substance after a to-be-measured sample is soaked by water, then performing vortex extraction and salting-out layering, adding toluene to perform liquid-liquid extraction, taking supernatant to perform dispersive solid-phase extraction (d-SPE), and using a GC-MS / MS method to perform measurement. The method has the advantages that the water is utilized to soak the sample, and extraction effects of organic solvent acetonitrile added later on on pesticide targets are improved; freezing treatment is performed in advance before anhydrous magnesium sulfate is added, so that thermal degradation of part of the targets caused by severe heat release of anhydrous magnesium sulfate in the dewatering process is avoided; toluene is added in the sample extract liquid after extraction salting-out, the obtained extract liquid has shallower color than when acetonitrile is independently used, and the effects of diluting the extract liquid and partially removing impurities for the extract liquid are achieved actually.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Method for detecting plasticizer content in solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry

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.
Owner:SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI

Method for detecting various phthalic acid ester plasticizers in vegetables, fruits and edible mushrooms at same time

The invention provides a method for detecting various phthalic acid ester plasticizers at the same time. The method includes the steps that firstly, a sample is extracted and purified in an optimized QuEChERS pretreatment mode; secondly, analysis is carried out in a gas chromatography-tandem mass spectrometry mode; finally, accurate qualitative and quantitative analysis is carried out with an isotope internal standard method. The method can be applied to detecting twenty-three phthalic acid ester plasticizers in plant source character foods such as common Chinese cabbages, tomatoes, strawberries, grapes, shiitake mushrooms and agaric at the same time. By means of the method, the plasticizers introduced through external source ways are avoided to the maximum degree, the pretreatment step is simple, consumed time of solid-phase extraction and purification is shortened, and consumed solvents and argent compound losses of the solid-phase extraction and purification are reduced; the method has the advantages of being sensitive, accurate, good in stability, short in consumed time and easy to popularize; the method can be suitable for detecting mass samples at the same time.
Owner:SHANGHAI ACAD OF AGRI SCI

A method for the detection of aromatic amines in mainstream cigarette smoke by gas chromatography-tandem mass spectrometry

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.
Owner:ZHENGZHOU TOBACCO RES INST OF CNTC

Method for measuring phthalic ester in atmospheric particulates

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.
Owner:NANKAI UNIV

Method for determining organochlorine pesticide residues in tobaccos or tobacco products

The invention discloses a method for determining organochlorine pesticide residues in tobaccos or tobacco products. The method comprises the following steps: leaching a wetted tobacco leaf sample with an organic solvent; adding a drying agent to dry extract liquid, and then purifying the extract liquid with a magnetic adsorbent; and finally detecting by an on-line gel permeation chromatography-gas chromatography-tandem mass spectrometry instrument, and building a method for determining organochlorine pesticide residues in tobaccos or tobacco products. According to the method disclosed by the invention, the defects of an existing determination method are overcome; a sample pretreatment method and an instrument detection condition are optimized; compared with the prior art, the method has the advantages that the testing cost is reduced, and has the advantages of simplicity in operation, high purifying capacity, high sensitivity and the like.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Solid-phase extraction-gas chromatography tandem mass spectrometry detection method for pyrazol bactericides in wine

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.
Owner:韩超

Method for simultaneous determination of six residual plant-growth regulators in bean sprout by using gas chromatography-tandem mass spectrometry

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.
Owner:ZHEJIANG ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE

GC-MS/MS (Gas chromatography - tandem mass spectrometry) method for simultaneously analyzing three polycyclic aromatic hydrocarbons and four tobacco-specific nitrosamines in main stream smoke of cigarettes

The invention discloses a GC-MS / MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing three polycyclic aromatic hydrocarbons and four tobacco-specific nitrosamines in main stream smoke of cigarettes. The method comprises the following steps of: taking out a Cambridge filter disc catching granule phase objects of main stream smoke of cigarettes, adding ethyl acetate and an internal standard, carrying out vibrating extraction, carrying out dispersive solid-phase extraction (d-SPE) on extracting liquid, then, carrying out nitrogen-blowing concentration on supernatant, and measuring by using GC-MS / MS. The method provided by the invention overcomes the problems that a sample treatment method can separately detect the two substances in the prior art and the pretreatment is tedious; and a sample pretreatment method and an instrument detection condition are optimized aiming at the granule phase objects of main stream smoke of cigarettes. The method provided by the invention has the advantages that two target objects with large polar phase differences are extracted at the same time by 10mL of ethyl acetate, and the extraction efficiency is high; and compared with the national standard method, the method has the advantages that the consumption of an organic solvent is reduced by a several times to tens of times, and the method has the characteristics of accurate operation, high sensitivity and good repeatability.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Method for measuring methyl eugenol in mainstream smoke of cigarettes

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.
Owner:CHINA TOBACCO JIANGSU INDAL

GC-MS (Gas Chromatography-Mass Spectrometer)/MS (Mass Spectrometer) method for simultaneously analyzing four tobacco-specific nitrosamines (TSNAs) in main stream smoke of cigarette

ActiveCN103293245AReduce usageReduce the number of usageComponent separationPretreatment methodOrganic solvent
The invention discloses a GC-MS / MS (Gas Chromatography-Mass Spectrometer) / MS (Mass Spectrometer) method for simultaneously analyzing four tobacco-specific nitrosamines (TSNAs) in main stream smoke of a cigarette. The method is characterized by comprising the steps of: adding ethyl acetate and an internal standard substance after taking out a Cambridge filter on which main stream smoke particulate phase substances are captured; getting an extract liquor after vibrating extraction and carrying out dispersive solid-phase extraction (d-SPE) on the extract liquor; then getting the supernatant liquor and carrying out nitrogen flushing concentration on the supernatant liquor; and measuring by a GC-MS / MS method. According to method disclosed by the invention, the shortcoming of complex treatment an existing method is overcome, and the pretreatment method of a sample and the instrument detection conditions are optimized aiming at the main stream smoke particulate phase substances in the cigarette. Compared with the prior art, the method disclosed by the invention has the following good effects that four TSNAs are simultaneously extracted by using ethyl acetate in pretreatment of the sample, so the good extraction efficiency is realized. Compared with the national standard method, the method disclosed by the invention has the effect that the use amount of organic solvent can be reduced by tens of times (260ml of dichloromethane is needed for measuring the TSNAs according to the national standard), and has the advantages of accuracy in operation, high sensitivity and good repeatability.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Method for determining phthalate ester in soil

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.
Owner:NANKAI UNIV

GC-MS/MS (gas chromatography-mass spectrometer/mass spectrometer) technique-based method for analyzing migration volume from photoinitiator to MPPO (modified polyphenylene oxide) in printing packaging paper

The invention discloses a GC-MS / MS (gas chromatography-mass spectrometer / mass spectrometer) technique-based method for analyzing the migration volume from a photoinitiator to MPPO (modified polyphenylene oxide) in printing packaging paper. The method is characterized in that a photoinitiator target released by a sample under a simulated condition is adsorbed by MPPO, and a solvent is extracted from the MPPO by acetonitrile, and supernate is concentrated and then is filtered so as to determine the specific migration volume of the photoinitiator in a printing packaging material by the GC-MS / MS method. The method can be rapidly and accurately used for detecting the specific migration volume of the photoinitiator in the printing packaging material, has an accurate determination result, is good in repeatability, is simple in pretreatment process, and is low in detection and analysis cost.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Method for detecting polyaromatic hydrocarbons (PAHs) and phthalic acid esters (PAEs) in plant extract

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.
Owner:陕西出入境检验检疫局检验检疫技术中心

Method for detecting four tobacco-specific nitrosamines (TSNAs) in lateral exhaust gas of cigarettes by virtue of gas chromatography-tandem mass spectrometry

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.
Owner:ZHENGZHOU TOBACCO RES INST OF CNTC

Method of measuring contents of various organic acids in tobacco and tobacco products.

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.
Owner:ZHENGZHOU TOBACCO RES INST OF CNTC

Method for determining content of methanol in insulation oil

InactiveCN107515260AAvoid makingAvoid the cumbersome process of transferringComponent separationGas phaseMass Spectrometry-Mass Spectrometry
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.
Owner:CHONGQING UNIV

Soft-shelled turtle fatty acid analysis method

The invention relates to the field of aquatic organisms and analysis chemistry, in particular to a method for separating and authenticating the components of fatty acid in the body of a soft-shelled turtle by combining GC-MS (gas chromatography-mass spectrometry) with a retention index. Fatty acid methyl esters are prepared by separating the adipose tissue of the soft-shelled turtle, and extracting and deriving the fatty acid from the separated adipose tissue. The method for separating and authenticating the fatty acid comprises the following steps: dissolving fatty acid methyl esters of the soft-shelled turtle in hexane and analyzing by using GC-MS to fulfill the aim of separating; calculating the retention index of fatty acid methyl esters according to the retention time of different fatty acid methyl esters; searching a mass spectrometry library, and meanwhile, carrying out nature determination by combining the retention index, and calculating the relative content of each fatty acid methyl ester by an area normalization method so as to fulfill the aim of analyzing the components of fatty acid of the soft-shell turtle accurately and quickly. The method has the advantages that the components of fatty acid in the soft-shell turtle can be authenticated accurately by fully utilizing the method of searching the mass spectrometry library and nature determination by combining the retention index; particularly, the operation is simple and convenient, and the method has the advantage that the result is accurate compared with the method of searching the mass spectrometry library.
Owner:NANCHANG UNIV

Chiral analysis method for nicotine in tealeaves

The invention discloses a chiral analysis method for nicotine in tealeaves. The chiral analysis method is characterized by comprising the following steps: drying, crushing and sieving a tealeaf sample, adding extraction liquid for extraction and filtration, performing multidimensional gas chromatography-tandem mass spectrometry analysis after automatic solid-phase micro-extraction, and quantitatively detecting the proportion of S-(-)-nicotine and R-(+)-nicotine in the tealeaves by adopting a peak area normalization method. According to the analysis method, the sample can be simply and rapidly treated, the method is low in detection limit and high in sensitivity and accuracy, and the chiral analysis requirement of the nicotine in the tealeaf sample can be met.
Owner:CHINA TOBACCO GUANGXI IND

Measurement method for non-fat organic acids in tobacco and tobacco product

The invention relates to a measurement method for non-fat organic acids in tobacco and a tobacco product and belongs to the technical field of analysis of acidic components in the tobacco and the tobacco product. The measurement method provided by the invention comprises the steps of extracting a to-be-measured sample, and taking extract liquid for derivative reaction to obtain to-be-measured liquid; taking the to-be-liquid, and carrying out gas chromatography-tandem mass spectrometry, wherein a gas chromatography condition comprises the following heating program of keeping 40-60 degrees centigrade for 1-3 min, heating to 140-160 degrees according to 3-10 degrees centigrade / min, heating to 190-210 degrees centigrade according to 5-10 degrees centigrade / min, heating to 270-290 degrees centigrade according to 20-30 degrees centigrade / min, and keeping warm for 15-25 min. According to the measurement method provided by the invention, various non-fat organic acids can be effectively separated, sensitivity is high, and the measurement method can be used for measuring content of the organic acids such as 3-hydroxypropionic acid, m-toluic acid, 4-oxononanoic acid, 2-hydroxybenzoic acid andcinnamic acid.
Owner:ZHENGZHOU TOBACCO RES INST OF CNTC

Analytical method for quantitatively measuring super-multi-target aroma components in tobacco

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.
Owner:ZHENGZHOU TOBACCO RES INST OF CNTC

GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing dinitroaniline pesticide residue in tobacco and tobacco product

The invention relates to a GC-MS / MS (gas chromatography-tandem mass spectrometry) method for analyzing dinitroaniline pesticide residue in tobacco and a tobacco product, which is characterized by comprising the following steps: drenching a sample with water, and adding acetonitrile and an internal standard substance; performing vortex extraction and salting-out stratification, and performing secondary salting-out and liquid-liquid extraction with a sodium chloride water solution and n-hexane; and taking the n-hexane supernatant, and determining according to a GC-MS / MS method. The method provided by the invention simplifies the existing sample treatment method, provides a cleaner on-machine solution, and reduces the maintenance of instruments in the operating process. The sample pretreatment process of the method provided by the invention omits a purification step of substrate d-SPE (dispersive solid phase extraction); and instead, the acetonitrile extracting solution is taken, and liquid-liquid extraction and secondary salting-out are performed by using the n-hexane and the sodium chloride water solution, so that the polar coextraction substrate in the supernatant is greatly reduced. By using GC-MS / MS having high sensitivity and high interference rejection, the detection limit of a target substance can be greatly reduced, and the advantages of high sensitivity and favorable repetitiveness are achieved.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Method for simultaneously detecting phenol, NNK and benzo-[a]-pyrene in main stream smoke of cigar by using gas chromatography-tandem mass spectrum

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.
Owner:ZHENGZHOU TOBACCO RES INST OF CNTC

GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and tobacco product

The invention relates to a GC-MS / MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and a tobacco product, which is characterized by comprising the following steps: drenching a sample with water, and adding acetonitrile and an internal standard substance; performing vortex extraction and salting-out stratification, and performing secondary salting-out and liquid-liquid extraction with a sodium chloride water solution and n-hexane; and taking the n-hexane supernatant, and determining according to a GC-MS / MS method. The method provided by the invention simplifies the existing sample treatment method, provides a cleaner on-machine solution, and reduces the maintenance of instruments in the operating process. The sample pretreatment process of the method provided by the invention employs the step of drenching the sample with water in the existing method to improve the extraction effect of the acetonitrile on a pesticide target substance, and simultaneously omits the step of putting into a refrigerator before adding into a salting-out package. Inspection discovers that most of pyrethroid pesticides are thermostable, so that the pyrethroid pesticides can not be degraded due to heat release caused by the combination of anhydrous magnesium sulfate and water, thus saving the operating time herein.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke

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.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT

Method for quantitative analysis of main pyrazine flavor substances in cigarette mainstream smoke

ActiveCN105842374AGood effectSolve the impact of factors such as serious interference analysisComponent separationResponse sensitivityTetramethyl pyrazine
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.
Owner:CHINA TOBACCO JIANGSU INDAL

Method for comprehensively detecting N-nitrosamine content in meat products

The invention discloses a method for comprehensively detecting N-nitrosamine content in meat products. The method comprises the following steps: weighting crushed meat products; adding acetonitrile, normal hexane and anhydrous magnesium sulfate; whirling, ultrasonically extracting, centrifuging, pouring out supernate, remaining acetonitrile and abandoning normal hexane layer; adopting acetonitrile for repeatedly extracting the meat product for 1-3 times; merging the extracting solution; reducing pressure, steaming till being almost dry; using the acetonitrile for keeping the constant volume; using C18 / PSA powder for purifying the constant volume solution; collecting the supernate, thereby acquiring a to-be-detected sample; using a gas chromatogram series mass spectrometer for detecting the to-be-detected sample, preparing a standard solution and drawing a curve and then calculating a result. The method has the advantages of less time consumption, less interference, strong specificity, high sensitivity, simplicity and convenience in operation, low equipment cost and high accuracy and precision.
Owner:广西壮族自治区食品药品检验所

Pretreatment and quantitative analysis method for rapid determination of pesticide residue in tea

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.
Owner:厦门鹭珈聚芯生物科技有限公司

Solid-phase membrane extraction and gas chromatography-tandem mass spectrometry detection method of organic chlorine compounds in water body

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.
Owner:MARINE FISHERIES RES INST OF ZHEJIANG

GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes

The invention discloses a GC-MS / MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes. The method is characterized by comprising the following steps of: taking out a Cambridge filter disc catching granule phase objects of main stream smoke of cigarettes, adding ethyl acetate and an internal standard, carrying out vibrating extraction, carrying out dispersive solid-phase extraction (d-SPE) on extracting liquid, then, carrying out nitrogen-blowing concentration on supernatant, and measuring by using GC-MS / MS. The method provided by the invention overcomes the deficiency that the existing pretreatment is tedious. A sample pretreatment method and an instrument detection condition are optimized, aiming at the granule phase objects of main stream smoke of cigarettes; the matrix disperse solid phase extraction (d-SPE) is selected to be used as a purification measure in purifying treatment; compared with a national standard method solid phase extract phase, the operation is simple, and the price is low; and the method provided by the invention has the advantages of accurate operation, high sensitivity and good repeatability.
Owner:CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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