178 results about "Triple quadrupole mass spectrometry" patented technology

The invention relates to a method for detecting the residue amount of terracycline antibiotics in milk and dairy products. The method utilizes an ultra performance liquid chromatography - electrospray tandem triple quadrupole mass spectrometer to determine the residue amount of the terracycline antibiotics. The method is as follows: a sample is extracted from Na2EDTA-McIlvaine buffer solution (pH4.0); proteins are removed by trichloroacetic acids; a columella is extracted through an HLB solid phase and then purified and enriched; the sample is separated by a chromatographic column, with the column temperature of 30 DEG C; gradient elution is performed by utilization of water solution (v/v) which contains 0.1 percent of methanoic acids and acetonitrile as a moving phase; and quantitative detection is performed by adoption of the multi-reaction monitoring means. The detection limit of instruments is between 1.0 and 2.0 mu g/kg; a related coefficient r reaches over 0.999 within the linear range of between 1 and 100 mu g/kg; and the recovery rate is between 81.7 and 100.7 percent (the addition levels are 10 mu g/kg, 50 mu g/kg and 100 mu g/kg). The method has the advantages of quickness, accuracy, high sensitivity and wide application scope.

The invention discloses a method and a sample pretreatment method for detecting a content of fat-soluble vitamins in formula milk powder. The invention firstly discloses the sample pretreatment methodfor detecting the content of the fat-soluble vitamins in the formula milk powder, and the method comprises the following steps of weighing a to-be-detected formula milk powder sample, and adding ascorbic acid, absolute ethyl alcohol and a KOH solution for saponification; adding n-hexane into the solution after saponification, centrifuging after liquid-liquid extraction, and collecting supernatantliquid; and drying the supernatant liquid, re-dissolving and filtering to obtain a to-be-detected solution. The invention also further discloses the method for detecting the content of the fat-soluble vitamins after sample pretreatment through an ultra-high performance liquid chromatography-triple quadrupole mass spectrometry technology. The method disclosed by the invention is easy, rapid, sensitive and accurate, and can meet the detection requirements for the fat-soluble vitamins in the formula milk powder.

The invention relates to a method for detecting residual quantity of norfloxacin antibiotic in milk. The method utilizes an ultra-performance liquid chromatography (UPLC)-electrospray tandem triple quadrupole mass spectrometer to determine the residual quantity of norfloxacin antibiotic. A sample is extracted by Na2 EDTA-Mellvaine buffer solution (pH 4.0), subjected to protein removal by trichloroacetic acid, purified and concentrated by a PEP solid phase extraction columella, separated by adopting a chromatographic column with column temperature of 30 DEG C, subjected to gradient elution by adopting aqueous solution (v/v) containing 0.1% formic acid and acetonitrile as a flowing phase, and then quantitated by adopting a multiple reaction monitoring manner. The instrument detection limit is 1.0-2.0 mug/Kg; and within the linear range of 1-100 mug/Kg, the correlation coefficient r can reach more than 0.999, and the coefficient of recovery is 80%-105% (adding level of 10, 50 and 100 mug/Kg). The method has the advantages of rapidness, accuracy, high sensitivity and wide application scope.

The invention relates to an array triple-quadrupole?mass spectrum system. The array triple-quadrupole?mass spectrum system includes an electrospray ion source, mutually-independent array ion guidance systems, mutually-independent array triple-quadrupole?material selection, dissociation and material selection systems, mutually-independent array ion detection systems, and a shared vacuum system; the electrospray ion source is provided with a plurality of nozzles; the nozzles are respectively connected with the mutually-independent array ion guidance systems, the mutually-independent array triple-quadrupole?material selection, dissociation and material selection systems, and the mutually-independent array ion detection systems sequentially through a plurality of ion sample injection interfaces corresponding to the nozzles. Compared with the prior art, the array triple-quadrupole?mass spectrum system of the invention is capable of performing simultaneous detection analysis on a plurality of polypeptide molecules which have been subjected to liquid chromatogram synchronous elution, polypeptide molecules which have been subjected to isotope labeling or a plurality of characteristic fragment ions of the same polypeptide molecule, and therefore, the analysis flux, sensitivity and dynamic range of a triple-quadrupole?mass spectrometer can be improved manyfold.

The invention relates to the technical field of environment detection and is suitable for measuring erythrocin, chloramphenicol, sulfamethoxazole, sulfadiazine, roxithromycin, cefotiam, pyridazol, norfloxacin, ofloxacin, tetracycline and doxycycline in sewage, surface water and bottom mud. After being sampled, a water sample and a mud sample are pretreated and detected through ultra-high performance liquid chromatography-triple quadrupole mass spectrometry, and qualitative diagnosis is conducted through the characteristic ion pair (m/z) of a target compound, a standard curve is drawn accordingto the response value and the corresponding concentration, and the external standard method is used in quantification, so that the contents of various antibiotics in the sample are obtained. The method is accurate, sensitive and simple, and is suitable for measuring the contents of 11 typical antibiotics in the sewage, the surface water and the mud at the same time.

The invention discloses a determination method of bisphenol S transfer volume in plastic food packaging materials. The determination method of bisphenol S transfer volume in plastic food packaging materials comprises the following steps: firstly, preparing a standard operation solution, a food simulant test solution and a blank test solution; secondly, carrying out liquid chromatogram-tandem triple quadrupole determination on three solutions in the step one by adopting a high performance liquid chromatography-tandem triple quadrupole mass spectrometry instrument; and drawing a standard operation solution regression curve by taking the concentration x of bisphenol S in the standard operation solution as an x-coordinate and taking the correspondingly determined quantitative ion peak area y as a y-coordiate, and calculating the slope a and the intercept b of the regression curve according to the linear equation obtained by the curve: y=ax+b; and thirdly, calculating the concentration of bisphenol S in a food simulant test solution according to the formula c=[(y<module>-y<empty>)-b]/a. The method provided by the invention can accurately measure the transfer volume of bisphenol S in plastic packaging materials, is accurate and reliable in quantification, and is favorable in reproducibility.

The invention relates to the field of drugs, in particular to a detection method for simultaneously determining content of vancomycin and tobramycin in tissue drainage liquid. A method for simultaneously determining content of vancomycin and tobramycin in tissue drainage liquid through an ultrahigh performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-TQD) coupling techniquecomprises the following steps of: 1) preparing reference samples; 2) preparing internal standard solution; 3) preparing sample solution; 4) preparing mobile-phase solution; 5) setting chromatographicconditions; 6) optimizing mass spectrometric conditions; 7) determining the samples; 8) preparing gradient-concentration reference sample solution; 9) preparing a standard curve; and 10) analyzing and computing data. The method has the characteristics that: 1) the method is advanced; 2) the method is rapid and high-efficiency the loss is low; and 3) the clinical application prospect and the effect are good.

The present invention relates to the technical field of detection of heterocyclic amines, in particular to a method for detecting heterocyclic amines in the grease. The method for detecting heterocyclic amines in the grease provided by the present invention comprises the following steps: preprocessing a to-be-detected grease sample to obtain the preprocessed grease; and sequentially using the ultra-high performance liquid chromatography and the triple quadrupole mass spectrometry to perform detection on the preprocessed grease, wherein the preprocessing comprises solvent extraction, degreasingprocessing, and solid phase extraction, and the solvent extraction is organic solvent extraction or alkaline organic solvent extraction. The method provided by the present invention has a simple operation and short time-consumption, and can be used to effectively detect heterocyclic amines in the grease.

The invention provides a method for measuring tobacco-specific N-nitrosamine in tobacco. The method adopts gas chromatography triple quadrupole mass spectrometry (GC-QQQ-MS/MS) to measure the content of tobacco-specific N-nitrosamine in tobacco and specifically comprises the following steps: 1, preparation of a standard solution; 2, sample pretreatment; 3, qualitative detection of samples; 4, quantitative detection of samples. According to the method for measuring tobacco-specific N-nitrosamine in tobacco, an optimally-selected mixed solvent is used for extraction, so that the sample pretreatment method is optimized; besides, simple and fast measurement is performed on the basis of high chromatographic fractionation capability and good selectivity and sensitivity of the GC-QQQ-MS/MS, so that higher sensitivity, accuracy and precision can be achieved, and the detection efficiency of four kinds of tobacco-specific N-nitrosamine in tobacco can be improved effectively.

The invention provides a method for determining tris (2, 3-dibromopropyl) phosphate content of water, and belongs to the field of organic phosphate flame retardant. The method mainly comprises the following steps: (1) conducting solid-phase extraction on a sample; (2) eluting and collecting the extraction column; (3) concentrating the eluent obtained in the step (2) to a constant volume; and (4) determining the concentrated liquid with a high-performance liquid chromatograph-triple quadrupole mass spectrometer. The method provided by the invention improves determination method of tris (2,3-dibromopropyl) phosphate in water environment; and through ultra performance liquid chromatograph-triple quadrupole mass spectrometry combination, the method for detecting tris (2,3-dibromopropyl) phosphate method has more advantages than other methods. The present invention using ultra performance liquid chromatograph has larger separation speed than gas chromatograph and general high performance liquid chromatograp; triple quadrupole mass spectrometry for SRM scanning realizes higher selectivity, more accurate qualitative diagnosis, and improved sensitivity. Therefore, the method provided by the invention has obvious advantages compared with other gas-phase method and liquid mass chromatography method.

The invention discloses a method for analyzing phenolic compounds in water, used for qualitatively or quantitatively analyzing the phenolic compounds in a water sample. The method comprises the following steps of 1, producing a standard curve; 2, preparing sample liquid to be detected: preprocessing a surface water sample to be detected to acquire the sample liquid to be detected; 3, detecting andanalyzing the sample liquid to be detected by using gas chromatography-low energy electron ionization quadrupole time-of-flight mass spectrometry (GC-le EI-QTOF); and 4, reviewing the sample that isdetected to be positive, namely that includes the phenolic compounds, by using gas chromatography-triple quadrupole mass spectrometry (GC-QQQ). The method provided by the invention is high in resolution, high in sensitivity, and capable of accurately determining the nature of a target, and excluding interferent of which a mass-to-charge ratio is close to that of the target.

In order to provide an analysis method that is capable of determining a glycan structure with high detection sensitivity, a method of the present invention includes the steps of: carrying out triple quadrupole mass spectrometry at various values of CID energy; creating an energy-resolved profile including yield curves representing relationships between (i) a value of the CID energy and (ii) measured amounts of specific types of product ions; preparing a reference profile, and identifying a glycan structure of a test material by comparing the energy-resolved profile with the reference profile.

The invention discloses a method for screening myocardial ischemia resisting pharmacodynamic material basis of yang exhaustion treating decoction. The method comprises the following steps: 1, determining myocardial ischemia resisting endogenous metabolin of the yang exhaustion treating decoction and measuring the peak area; 2, determining in-vivo migration constituents in the yang exhaustion treating decoction and measuring the peak area; 3, performing correlation analysis on the peak area of the myocardial ischemia resisting endogenous metabolin of the yang exhaustion treating decoction and the peak area of the in-vivo migration constituents in the yang exhaustion treating decoction and screening out myocardial ischemia resisting pharmacodynamic material basis of the yang exhaustion treating decoction. The method disclosed by the invention is based on isoproterenol-induced rat myocardial ischemia model; an ultrahigh performance liquid chromatography-quadrupole rod-flight time mass spectrum non-targeted metabonomic technology and a targeted metabonomic technology based on an ultrahigh performance liquid chromatography-triple quadrupole rod mass spectrum are utilized to screen out 12 kinds of myocardial ischemia resisting pharmacodynamic material basis of the yang exhaustion treating decoction; thus, accuracy of the myocardial ischemia resisting pharmacodynamic material basis ofthe yang exhaustion treating decoction is improved, a screening period is shortened, and screening consumption cost is reduced.

The invention relates to a method for analyzing isomalto-oligosaccharide and isomeride thereof in yoghourt. The method comprises the following steps: applying an ultra-high performance liquid chromatography-ion mobility-triple quadrupole mass spectrometry tandem time-of-flight mass spectrometry technology; using an HMSE mode for collecting a sample; using primary and secondary ion fragments for quantification; determining the nature by using the retention time and the ion drift time; accurately analyzing maltose, maltotriose, isomaltose, panose and isomaltotriose in the yoghourt from multipledimensions; establishing the UPLC-IMS-QTof method for isomalto-oligosaccharide in yoghourt, the blank in the field is filled, a more efficient and accurate analysis method is provided for workers in the industry, and technical support is provided for detecting the oligosaccharide content of yoghourt on the market.

A triple quadrupole mass spectrometer provided with: a calibration information storage section for storing mass calibration information showing the relationship between the mass-to-charge ratio and a calibration value, with a CID gas pressure as a parameter, for each measurement mode of an MS/MS analysis including a dissociating operation using a collision cell; and a controller for calibrating the mass-to-charge ratio of the ion to be detected by a detector, by reading, from the calibration information storage section, the mass calibration information corresponding to the measurement mode to be performed and a specified CID gas pressure and by driving each the front and rear quadrupoles and using that information.

The invention discloses a method for rapidly determining acrylamide in vegetable oil by QuEChERS-LC-MS/MS. The method comprises: extracting acrylamide in the oil sample by acetonitrile; and after freezing and degreasing, purifying the supernatant by MgSO4, C18, PSA and GCB adsorbents, separating by a C18 chromatographic column, carrying out gradient elution by adopting a methanol -0.1% formic acidaqueous solution mobile phase, detecting by adopting a triple quadrupole mass spectrometry electrospray multi-reaction monitoring mode (MRM), and quantifying by adopting an internal standard method.The acrylamide has a good linear relationship in a concentration range of 1-500 ng/mL, and the correlation coefficient is greater than 0.997. The detection limit of the method is 2 [mu]g/kg, and the quantification limit is 5 [mu]g/kg. The adding standard recovery rate is 96.4%-108%, and the relative standard deviation is less than 7.74%. The method has the advantages of simple and efficient pretreatment operation, direct on-machine determination without concentration, good recovery rate, high sensitivity, and accurate qualitative and quantitative determination.

The invention belongs to the technical field of organic pollutant analysis, and discloses a solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method foronline determination of hydroxyl polycyclic aromatic hydrocarbon in urine. The method comprises the following steps: adding an isotope internal standard into urine, and then adding beta-glucuronidase-aryl sulfatase; carrying out enzymolysis on a constant-temperature shaking table, adding an organic solvent to precipitate protein after enzymolysis, carrying out refrigerated centrifugation, transferring the centrifuged supernatant, carrying out online solid-phase extraction through automatic valve switching, and then carrying out quantitative determination through liquid chromatography triple quadrupole mass spectrometry; and carrying out data processing and quantitative calculation to obtain the content of the hydroxyl polycyclic aromatic hydrocarbon in the urine. According to the invention, rapid and accurate detection of hydroxyl polycyclic aromatic hydrocarbon metabolites in human urine is realized, and an effective method is provided for human exposure health risk assessment of polycyclic aromatic hydrocarbon.

The invention relates to a method for determining paclitaxel or paclitaxel, in particular to a method for quantitatively analyzing paclitaxel or paclitaxel by adopting a high-performance liquid chromatography-triple quadrupole mass spectrometry combination technology. The method comprises the steps of using a mobile phase containing ammonium formate and formic acid in a high-performance liquid chromatograph, adopting an MRM mode to determine formate added quasi-molecular ion peaks and daughter ion peaks of the paclitaxel or paclitaxel in an ESI (-) or APCI (-) ionization mode.