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36results about How to "Improve qualitative accuracy" patented technology

Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5

InactiveCN103616458AEstablish and optimize the detection method of MS/MSOptimizing MS/MS Detection MethodComponent separationNitrogen–phosphorus detectorMass Spectrometry-Mass Spectrometry
The invention provides a method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5. The method comprises the following steps: acquiring a sample, extracting the sample, concentrating and purifying the sample and quantitatively detecting by adopting chromatography-tandem mass spectrometry. By optimizing parameters of secondary mass spectrometry conditions, the method is better in selectivity and higher in sensitivity on target compounds in comparison with an existing detection method reported in literature. According to the method, the disadvantage that the selectivity and the sensitivity of a conventional detector in the process of detecting the trace quantity of nitrobenzene compounds in a complex background matrix cannot be ensured at the same time is overcome by virtue of a gas chromatography/tandem mass spectrometry selective reaction monitoring technology, and the qualitative operation is accurate and reliable, so that the method has very remarkable advantages in comparison with conventional GC/ECDs (gas chromatography/election capture detectors), GC/NPDs (gas chromatography/nitrogen-phosphorus detector), GC/LRMS (gas chromatography/low resolution mass spectrometry) detectors or GC/HRMS (gas chromatography/high resolution mass spectrometry) detectors.
Owner:NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA +1

LC-Q-TOF/MS detection technology for 544 pesticide residues in kernel fruit

The invention provides an LC-Q-TOF/MS detection technology for 544 pesticide residues in kernel fruit. In a TOF/MS mode, the LC-Q-TOF/MS detection technology separately determines the retention time of each pesticide standard under designated gas chromatography-mass spectrography conditions, determines the ionization form and chemical formula of a compound under the condition of an ESI source and acquires the accurate mass number of the parent ion of each compound so as to form a TOF/MS database. In a Q-TOF/MS mode, the LC-Q-TOF/MS detection technology separately acquires the fragment ion mass spectrum of each pesticide standard under the condition of three to five different collision energies and introduces acquired information into PCDL software so as to form a Q-TOF/MS database. Through comparison of the retention time, mass spectrometry information and tandem mass spectrometry information of a kernel fruit sample, whether the sample contains pesticide residues or not can be determined; and compounds with high primary scores are subjected to secondary confirmation, and if secondary scores are high, it is confirmed that related pesticide residues are detected. The LC-Q-TOF/MS detection technology provided by the invention has the advantages of fastness, high throughput, high accuracy, high reliability and the like, and can accurately screen pesticides in the kernel fruit.
Owner:CHINESE ACAD OF INSPECTION & QUARANTINE

Method for quantitatively detecting organophosphorus pesticide chlorpyrifos in environmental air

ActiveCN107490647ASet up and optimize HPLCEstablish and optimize the secondary mass spectrometer (MSComponent separationParticulatesChlorpyrifos
The invention provides a method for quantitatively detecting organophosphorus pesticide chlorpyrifos in environmental air, and belongs to the field of detection methods for pesticide residues. The method comprises collection of a sample (comprising a gas phase part and a particulate matter part), pretreatment of the sample and chromatography-tandem mass spectrometry quantitative detection. Compared with reported methods, the detection of the chlorpyrifos in the environmental air is higher in selectivity and higher in sensitivity through the optimization of parameters of a chromatography-mass spectrometry detection method. According to the method, by the use of a multi-reaction monitoring technology of high performance liquid chromatography/tandem mass spectrometry, the shortcoming that a conventional detector cannot have the selectivity and the sensitivity at the same time during detection of a trace chlorpyrifos compound in a complicated background matrix is overcome, and qualitation and quantitation are more accurate and reliable. Therefore, compared with conventional UV-Vis, HPLC/PDA, GC/ECD and GC/NPD, the method provided by the invention has very outstanding advantages.
Owner:NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA

LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables

The invention provides an LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables. In a TOF/MS mode, LC-Q-TOF/MS measures the retention time of each pesticide standard substance under specified chromatographic and mass spectrometric conditions, an ionization form and a chemical formula of each compound under an ESI source are determined, the exact mass number for parent ions of each compound is obtained, and a TOF/MS database is formed. In a Q-TOF/MS mode, fragment ion mass spectra of each pesticide standard substance in 3-5 different collision energies are collected respectively, the collected information is introduced into PCDL software, and a Q-TOF/MS database is formed. Through comparison of the retention time and first-level mass spectrometry and second-level mass spectrometry information of solanaceous fruit vegetable samples, whether the samples contain the pesticide residues is determined, compounds having higher first-level score are subjected to second-level confirmation, and if the second-level score is higher, related pesticide residues are confirmed to be detected out. The method has the advantages of high speed, high throughput, high precision, high reliability and the like, and can accurately screen the pesticides in the solanaceous fruit vegetables.
Owner:CHINESE ACAD OF INSPECTION & QUARANTINE

LC-Q-TOF/MS detection technology for 544 pesticide residues in stem vegetables

The invention provides an LC-Q-TOF/MS detection technology for 544 pesticide residues in stem vegetables. The technology includes the steps of: 1) under a TOF/MS mode in the LC-Q-TOF/MS, respectively measuring retention time of each pesticide reference substance under the certain chromatography-mass spectrometry conditions; 2) determining the ionization formation and chemical formula of the compound with an ESI source to obtain accurate mass number of a parent ion of each compound to form a TOF/MS database; 3) under a Q-TOF/MS mode, respectively collecting fragment ion mass spectrograms under 3-5 different collision energy of each pesticide reference substance, and introducing the collected information to PCDL software to obtain a Q-TOF/MS database; 4)comparing the retention time, primary mass spectrum and secondary mass spectrum of the sample of the stem vegetables to determine whether the pesticide residues exist in the sample or not, and meanwhile, performing secondary determination to the compound having higher primary score, and if secondary score is high, determining existence of the pesticide residues. The technology is quick, high-throughput, high-precision and high-reliability, and can be used for accurately screening the pesticides in the stem vegetables.
Owner:CHINESE ACAD OF INSPECTION & QUARANTINE

Quantitative detection method of trospium chloride in plasma

The invention belongs to the field of detection technology of trospium chloride, and discloses a quantitative detection method of trospium chloride in plasma. The method comprises the following steps:(1) preparation of a standard working solution: respectively diluting a trospium chloride stock solution with a methanol aqueous solution with a volume ratio of 1:1 to obtain a plurality of trospiumchloride working solutions; diluting an internal standard stock solution with the methanol aqueous solution with the volume ratio of 1:1 to obtain an internal standard working solution with a concentration of 10-20 ng.mL-1; (2) pretreatment process of a plasma sample to be tested; (3) preparation of a standard curve: using a chromatographic peak area ratio of trospium chloride and trospium chloride-d8 as a vertical coordinate, using a ratio of the plasma concentration of the trospium chloride to the plasma concentration of the trospium chloride-d8 as an abscissa, performing linear regression by using the weighted least square method to prepare the standard curve so as to obtain a regression equation Y=a+bX; and (4) calculating the plasma concentration of the trospium chloride in the plasmasample to be tested according to the regression equation. According to the quantitative detection method provided by the invention, the liquid chromatography-mass spectrometry / mass spectrometry is adopted to perform measurement, and the sensitivity is high.
Owner:康诚科瑞医药研发(武汉)有限公司

Method for detecting amantadine compounds and triazine herbicides in algae

The invention belongs to the technical field of material analysis, and provides a method for detecting amantadine compounds and triazine herbicides in algae. According to the method, acetonitrile, ethyl acetate, a formic acid-acetonitrile mixed solution with the formic acid volume concentration of 1% or a formic acid-ethyl acetate mixed solution with the formic acid volume concentration of 1% are adopted as an extracting agent, so that amantadine compounds and triazine herbicides in an algae sample can be released; a PSA adsorbent is used as an adsorbent; impurities which have great interference on amantadine compounds and triazine herbicides in an extracting solution can be adsorbed and removed to the greatest extent, qualitative detection is performed by adopting ultrahigh performance liquid chromatography, primary mass spectrometry and secondary mass spectrometry, the qualitative accuracy can be improved, false positive can be eliminated, and the detection accuracy can be improved; the amantadine compounds and the triazine herbicides can be accurately quantified by performing quantitative analysis on the amantadine compounds and the triazine herbicides by using ultrahigh liquid chromatography and primary chromatography, and the method has relatively high detection sensitivity.
Owner:山东省海洋资源与环境研究院

Method for detecting urotropin in cigarette mainstream smoke through gas chromatography-tandem mass spectrum

The invention discloses a method for detecting urotropin in cigarette mainstream smoke through gas chromatography-tandem mass spectrum. The method comprises the steps of gathering mainstream smoke total particulate matter of 20 cigarettes according to the rule of ISO4387:2000, then putting a cambridge filter with the mainstream smoke total particulate matter into a 250mL bread bottle, adding 40 mL of ethanol extract liquor containing triethylamine to oscillate for extracting the cambridge filter for 40 minutes, accurately taking out 20mL of the extract liquor to pass through an activated silica gel columella, washing the columella by using 30ml of dichloromethane firstly, dropping leacheate, then washing the columella by using 40mL of methyl alcohol, collecting the leacheate to concentrate to 1mL, accurately adding 50 microliters of 10mg/L internal standard solution to detect by using GC-MS/MS (Gas Chromatography-Mass Spectrometry/ Mass Spectrometry). According to the method, the GC-MS/MS is used for detecting the urotropin in the cigarette side stream smoke; a multi-reaction monitoring mode is adopted for determining the nature; the method is capable of effectively improving the qualitative accuracy and sensitivity of the method, suitable for the detection of urotropin in various types of cigarette side stream smoke, wide in application and capable of accurately detecting; meanwhile, the method is simple, environment-friendly, and good in practicability.
Owner:CHINA TOBACCO JIANGSU INDAL

Method for detecting urotropin in cigarette mainstream smoke through high performance liquid chromatography-tandem mass spectrum

The invention claims a method for detecting urotropin in cigarette mainstream smoke through high performance liquid chromatography-tandem mass spectrum. The method comprises the steps of gathering mainstream smoke total particulate matter of 20 cigarettes according to the rule of ISO4387:2000, then putting a cambridge filter with the mainstream smoke total particulate matter into a 250mL bread bottle, adding 40 mL of ethanol extract liquor containing triethylamine to oscillate for extracting the cambridge filter for 40 minutes, then filtering through a 0.45 micron filter membrane to detect by using GC-MS / MS (Liquid Chromatography-Mass Spectrometry / Mass Spectrometry). Instrument conditions are as follows: a HILIC (Hydrophilic Interaction Chromatography) is used; the detection temperature is 30 DEG C; the sample size is 2microliter; the flow velocity is 0.25mL per minute; a ratio of a mobile phase V (acetonitrile) to V (5mmol / L ammonium acetate solution) is 75:25; the mobile phase carries out isocratic elution. Mass spectrum conditions are as follows: an ionization mode is electros spray; a scanning mode is positive ion; the atomizing gas is 40 psi; the curtain gas is 10 psi; the auxiliary trim gas is 40 psi; the collision gas is 5 psi; the ion source voltage is 4000-5000V; the ion source temperature is 250-350 DEG C. The method is simple to operate, good in separation effect, accurate to determine the nature, short in sample analysis time and high in detection sensitivity.
Owner:CHINA TOBACCO JIANGSU INDAL

Quantitative detection method of levofloxacin in plasma

The invention belongs to the field of detection technology of levofloxacin, and discloses a quantitative detection method of levofloxacin in plasma. The method comprises the following steps: weighinglevofloxacin reference substance and levofloxacin-d8, diluting the levofloxacin reference substance and the levofloxacin-d8 with methanol and a methanol aqueous solution to obtain a series of levofloxacin working solutions and internal standard working solutions; pretreating a plasma sample by using the internal standard working solutions and a methanol precipitant, and performing LC-MS/MS analysis; preparing a series of correction guide samples and accompanying quality control samples by using blank plasma and the series of levofloxacin working solutions, then respectively performing LC-MS/MSmeasurement, using a chromatographic peak area ratio of the levofloxacin and the internal standard levofloxacin-d8 as a vertical coordinate, using the concentration of levofloxacin in the plasma as an abscissa to make a standard curve, and calculating the concentration of the levofloxacin in the plasma sample. The quantitative detection method disclosed by the invention has the advantages that measurement is performed via precipitation pretreatment and an LC-MS/MS mass spectrometer, so that the operation is quick and simple, the separation effect is good, the qualitative determination is accurate, and the detection sensitivity is high.
Owner:康诚科瑞医药研发(武汉)有限公司

Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5

The invention provides a method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5. The method comprises the following steps: acquiring a sample, extracting the sample, concentrating and purifying the sample and quantitatively detecting by adopting chromatography-tandem mass spectrometry. By optimizing parameters of secondary mass spectrometry conditions, the method is better in selectivity and higher in sensitivity on target compounds in comparison with an existing detection method reported in literature. According to the method, the disadvantage that the selectivity and the sensitivity of a conventional detector in the process of detecting the trace quantity of nitrobenzene compounds in a complex background matrix cannot be ensured at the same time is overcome by virtue of a gas chromatography / tandem mass spectrometry selective reaction monitoring technology, and the qualitative operation is accurate and reliable, so that the method has very remarkable advantages in comparison with conventional GC / ECDs (gas chromatography / election capture detectors), GC / NPDs (gas chromatography / nitrogen-phosphorus detector), GC / LRMS (gas chromatography / low resolution mass spectrometry) detectors or GC / HRMS (gas chromatography / high resolution mass spectrometry) detectors.
Owner:NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA +1

Method for detecting pazopanib drug concentration in human plasma by LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry)

The invention discloses a method for detecting the drug concentration of pazopanib in human plasma through LC-MS / MS combination, and belongs to the technical field of drug concentration analysis. Themethod comprises the following steps: respectively mixing a series of pazopanib working solutions with human blank plasma, performing pre-treating, injecting the mixture into LC-MS / MS for analysis, adding an internal standard working solution mainly prepared from pazopanib-d6 into human plasma to be detected, performing pre-treating, injecting the mixture into LC-MS / MS for analysis, drawing a standard curve by taking the chromatographic peak area ratio of pazopanib to internal standard pazopanib-d6 as an ordinate and the concentration of pazopanib in human blank plasma as an abscissa, and calculating the concentration of pazopanib in the human plasma sample to be detected according to the standard curve, wherein a protein precipitation method is adopted to pretreat a human plasma sample, an electrospray ion source is adopted as an ionization technology, and the detection method is simple and convenient to operate, high in sensitivity, good in reproducibility, high in selectivity, shortin analysis time and suitable for large-batch detection of clinical samples.
Owner:TONGJI HOSPITAL ATTACHED TO TONGJI MEDICAL COLLEGE HUAZHONG SCI TECH

A method for quantitative detection of organophosphorus pesticide chlorpyrifos in ambient air

ActiveCN107490647BMeet analytical monitoring requirementsIncreased monitoring needsComponent separationParticulatesChlorpyrifos
The invention provides a method for quantitatively detecting organophosphorus pesticide chlorpyrifos in environmental air, and belongs to the field of detection methods for pesticide residues. The method comprises collection of a sample (comprising a gas phase part and a particulate matter part), pretreatment of the sample and chromatography-tandem mass spectrometry quantitative detection. Compared with reported methods, the detection of the chlorpyrifos in the environmental air is higher in selectivity and higher in sensitivity through the optimization of parameters of a chromatography-mass spectrometry detection method. According to the method, by the use of a multi-reaction monitoring technology of high performance liquid chromatography / tandem mass spectrometry, the shortcoming that a conventional detector cannot have the selectivity and the sensitivity at the same time during detection of a trace chlorpyrifos compound in a complicated background matrix is overcome, and qualitation and quantitation are more accurate and reliable. Therefore, compared with conventional UV-Vis, HPLC / PDA, GC / ECD and GC / NPD, the method provided by the invention has very outstanding advantages.
Owner:NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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