109 results about "Triple quadrupole mass spectrometer" 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 provides a liquid chromatography-mass spectrometry method for rapidly detecting the content of beta-agonists. The liquid chromatography-mass spectrometry method comprises the following steps: pretreating a sample, namely, sequentially adding water and an organic extracting solution in the sample for extracting a beta-receptor stimulant; then adding a salting-out agent and a water removing agent to ensure that the organic extracting solution and a water phase demix, centrifuging to obtain a first supernate, adding an adsorbing agent in the first supernate for purification, centrifuging to obtain a second supernate, concentrating, re-dissolving and filtering the second supernate to prepare a sample to be detected; and then detecting the beta-receptor stimulant contained in an animal-derived food by adopting an ultra-high performance liquid chromatography-triple quadrupole mass spectrometer. According to the sample pretreatment method suitable for liquid chromatography-mass spectrometry detection, provided by the invention, interfering molecules are removed through extraction and purification so that high accuracy is achieved in sample detection.

The invention discloses a method for measuring diallyl phthalate migration in food contact materials. The method includes the steps: firstly, preparing a standard working solution, a food stimulant test solution and a blank test solution; secondly, adopting a high performance liquid chromatograph-tandem triple quadrupole mass spectrometer to perform liquid chromatograph-tandem mass spectrum measurement on the three solutions in the first step, drawing a regression curve of the standard working solution by taking concentration x of phthalate in the standard working solution as an abscissa and corresponding measured quantitative ion peak area y as an ordinate, and calculating slope a and intercept b of the regression curve according to a linear equation, of y=ax+b, obtained by the curve; thirdly, according a formula that c=[(y-y)-b]/a, calculating concentration of diallyl phthalate in the food stimulant test solution. By the aid of the method, migration of the diallyl phthalate in the food contact materials can be measured accurately, quantification is accurate and reliable, and reproducibility is good.

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 discloses a method for measuring the content of gingerol in ginger medicinal materials and preparations thereof. By virtue of the separation and analysis technology of ultra-high performance liquid chromatography in series with a triple quadrupole mass spectrometer detector and an ultraviolet detector as well as a one-measurement multi-evaluation method, a pure substance N-vanillyl nonane amide reference substance which does not exist in a sample, has stable properties and is easy to obtain is adopted as an internal reference substance so as to establish a relative correction factor between the component and four gingerol components in the sample, thereby realizing measurement of the contents of the four gingerol components in the ginger medicinal materials and the preparations thereof by virtue of calculation of the correction factor. The method disclosed by the invention is simple in operation, high in sensitivity, accurate and efficient and low in cost, can be used forobjectively and accurately evaluating the quality of the ginger medicinal materials and the preparations thereof, can be used for quality control, can solve the problem that the quality of the medicinal materials and the preparations thereof can not be objectively and reasonably controlled due to the lack of reference substances, and has important significance for controlling quality and ensuringcurative effects.

The invention relates to a method for rapid determination of blood concentration of methotrexate. The method comprises the following steps: firstly, adding a to-be-determined plasma sample into ammonium acetate -formic acid water solution, then, adding methanol solution containing MTX-d3 and eddying for 25s-35s, then, performing centrifugal separation, and then, collecting liquid supernatant, injecting the liquid supernatant into a rapid liquid chromatography system to perform separation analysis, then, injecting into a triple quadrupole mass spectrometer detector for detection, further performing data acquisition and processing through a chromatography software, and obtaining the blood concentration of the methotrexate. The method for rapid determination of blood concentration of methotrexate of the invention is rapid and accurate, highly sensitive, simple to operate and low-cost, and is suitable for clinical routine blood concentration monitoring. Preprocessing of the sample is simple, the amount of needed sample is low, so the method is suitable for clinical routine detection and pharmacokinetic study. An interior label is added in a sample preprocessing process, thus, accuracyof MTX quantification is improved, and specificity is high and sensitivity is high.

The invention discloses a method for detecting mycotoxin in fermented tea. The method comprises dissolving a fermented tea sample in a polar solution, carrying out salting-out, carrying out centrifugation, carrying out filtration, putting the filtrate in 1290/6460 ultra-high performance liquid chromatography-triple quadrupole mass spectrometer, carrying out analysis through a mobile phase (0.1% formic acid-5 mmol/L ammonium acetate-water)-methanol, wherein the mobile phase A is 0.1% formic acid-5 mmol/L ammonium acetate-water and the mobile phase B is methanol, and carrying out separation through a gradient elution method comprising improving a concentration of the mobile phase B step by step so that the mycotoxin in the fermented tea sample reaches to the base line in short time and then is separated. The method realizes effective extraction and determination of various mycotoxins in fermented tea, can detect a variety of mycotoxins at the same time and has the characteristics of high detection efficiency, low environmental pollution, simple operation and promotion and use easiness.

The invention discloses a method for fast detecting gamma-aminobutyric acid in baijiu. The method is characterized in that an ultra-high performance liquid chromatography serially connected triple quadrupole mass spectrometer is used for detecting the gamma-aminobutyric acid in baijiu; after the rotary evaporation for alcohol removal on a baijiu sample to be tested, an ACQUITY UPLC BEH C18 1.7 mum 2.1*50mm Column liquid chromatography column is used; an acetonitrile (A)+0.1 percent acetic acid water solution (B) is used as a flowing phase to perform isocratic elution; after a sample is subjected to ultra performance liquid chromatography separation, detection is performed through the triple quadrupole mass spectrometer. The method provided by the invention has the advantages that the method is simple; the qualitative and quantitative detection on gamma-aminobutyric acid in the baijiu can be accurately performed; the scientific basis is provided for the accurate judgment and fast detection of the gamma-aminobutyric acid in the baijiu.

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 an analysis method of glucose energy metabolism-related important metabolites in serum samples. According to the analysis method, methanol is adopted for extraction, samples to be detected are subjected to freeze-drying and two-step derivatization, and then are subjected to analysis using a gas chromatography-triple quadrupole mass spectrometer; multi-reaction monitoring mode is adopted for detection, for low-content metabolites, ion pairs with the optimal ion abundance are obtained via optimization and are taken as quantification ion pairs so as to increase sensitivity; for high-content metabolites, ion pairs low in abundance obtained via optimization are selected as quantification ion pairs so as to widen the linear range and realize simultaneous analysis of high and low abundance metabolites. Pretreatment of the analysis method is simple; repeatability is high; sensitivity is high; and linear range is wide.

The invention relates to the technical field of chemical detection. A detection and analysis method of short-chain chlorinated paraffin includes the following steps of firstly, processing a sample, wherein the sample is put in acetonitrile to be shaken after being subjected to ultrasonic extraction through tetrahydrofuran, and a processed extraction solution is obtained after sedimentation and filtration; secondly, conducting quanlitative analysis on the processed extraction solution through a high performance liquid chromatography-tandem triple quadrupole mass spectrometer; thirdly, conducting quantitative analysis on the processed extraction solution through the high performance liquid chromatography-tandem triple quadrupole mass spectrometer. According to the method, by optimizing a traditional detection and analysis method of short-chain chlorinated paraffin, pretreatment extraction is improved under the condition of ensuring consistency of extraction effects, and therefore the extraction solution can be suitable for liquid-phase analysis. In addition, by means of the high performance liquid chromatography-tandem triple quadrupole mass spectrometer and through the combination with the advantages of the phase liquid and mass spectrums, detection and analysis on short-chain chlorinated paraffin are conveniently achieved, and a lower method detection limit is obtained.

The invention provides a method for detecting polar phenol type chlorinated/brominated disinfection by-products in water. The method comprises steps as follows: 1) standard working solutions of 13 polar phenol type chlorinated/brominated disinfection by-products required to be detected are prepared; 2) a to-be-detected water sample is acidized, salted out, subjected to continuous liquid-liquid extraction, separated, concentrated, filtered and pretreated in other modes; 3) analysis is performed by means of a UPLC/ESI-tqMS (ultra-high performance liquid chromatography/electrospray ionization-triple quadrupole mass spectrometer): mass spectrum parameters, liquid chromatography parameters and gradient elution process parameters of the UPLC/ESI-tqMS are established; 4) a calibration curve is drawn and the concentration is calculated after a chromatographic peak of a chromatogram sample is preliminarily determined to be identical to that of a known standard substance and the chromatogram sample and the known standard substance are the same substance. The detection method is high in sensitivity, precision and accuracy, can achieve the purpose of rapidly and efficiently measuring the 13 polar phenol type chlorinated/brominated disinfection by-products in the water, particularly can rapidly and efficiently detect a trace quantity of polar phenol type chlorinated/brominated disinfection by-products in the water, and has relatively high practical value.

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 embodiments of the present invention provide an online pretreatment device for hair sample injection. The device is used for transferring hair samples during a pre-treatment process. The online pretreatment device for hair sample injection includes an image detector, a mass spectrometer, an objective lens and a sample cabin assembly; the sample cabin assembly includes a sample cavity and a plate drawer disposed within the sample cavity; the plate drawer slidably enters and withdraws from the sample cavity, the objective lens is connected between the mass spectrometer and the sample cabin assembly; and an image under the objective lens is shot through an image sensor and is transmitted to an external device. The online pretreatment device for hair sample injection of the invention adopted, the rapid qualitative and quantitative measurement of drugs or metabolic components thereof in hairs can be realized; samples are directly injected into a time of flight mass spectrometer; the time of flight mass spectrometer is connected in series with a triple-quadrupole mass spectrometer for quantification; and therefore, the online pretreatment device has the advantages of improved sensitivity and high detection speed.

The invention discloses a method for detecting concentration of infliximab in serum by high-performance liquid chromatography tandem mass spectrometry and application thereof. The method specificallycomprises the following steps of preparation of standard products, enzymatic digestion reaction, high-performance liquid chromatography separation, tandem mass spectrometry detection, and detection ofinfliximab in serum. The invention also discloses application of the method for detecting concentration of infliximab in serum by high-performance liquid chromatography tandem mass spectrometry. Theinvention uses acetonitrile for protein precipitation, and uses chromatographic tandem triple quadrupole mass spectrometer for detection after the extraction, which is simple in pretreatment steps, can effectively remove serum matrix interference, and has good specificity. In addition, the detection is performed by high performance liquid chromatography tandem mass spectrometer, and infliximab inserum is qualitatively and accurately quantified at the same time, thereby having short detection time, high throughput, high detection sensitivity, good specificity and low cost.

The invention relates to a method for measuring contents of multiple mycotoxins in fresh and raw milk samples. The method comprises the following steps: S1, extracting extracts of the mycotoxins from the fresh and raw milk samples; S2, carrying out liquid chromatographic separation on the extracts of the mycotoxins, so as to obtain elution fractions; S3, carrying out mass spectrum identification on the elution fractions by using a triple-quadrupole mass spectrometer, so as to determine the types and contents of the mycotoxins. After the method is adopted, the fourteen mycotoxins are fully extracted; compared with a single-quadrupole mass spectrometer, the triple-quadrupole mass spectrometer adopted by the method is higher in accuracy, so that a target compound is better separated from interference impurities; therefore, reliable and accurate data can be provided.

The invention discloses a detection method of gelatin medicinal materials. According to the detection method, trypsin is adopted for enzyme digestion of the gelatin medicinal material, so that specific polypeptide is released from collagen; then a liquid chromatography triple quadrupole mass spectrometer is adopted for detection, and if it is detected that the sample is corresponded to the specific polypeptide retentiontime, the parent ions and the daughter ions, determining that the species source of the gelatin medicinal material sample is consistent with the species corresponding to the specific polypeptide; and determining the adulteration proportion of the doped sample according to the peak area ratio of the specific polypeptide. The method has the advantages of strong specificity, high sensitivity, simple operation and the like, and can be used for identification and quality control of the gelatin medicinal materials.

The invention discloses a liquid chromatography tandem mass spectrometry quantification method used for simultaneous detection of a plurality of effective components in gelsemium elegans. According tothe liquid chromatography tandem mass spectrometry quantification method, a gelsemine methanol solution, a koumine methanol solution, a gelsenicine methanol solution, and a koumidine methanol solution are taken as reference sample solutions, a gelsemium elegans extracted solution is taken as a sample solution to be measured, a high performance liquid chromatography triple quadrupole mass spectrometer is adopted for detection, and the contents of the plurality of effective components in the sample solution to be measured are calculated based on detection results. The liquid chromatography tandem mass spectrometry quantification method is stable and reliable, is simple, is high in efficiency, sensitivity, and accuracy, possesses wide practicability, and can be used for detection and quantitative analysis of any components or derivative products from gelsemium elegans.

The invention relates to a method for testing tetracycline antibiotic residue in cattle pulmonary surfactant extract. The method adopts ultrahigh-performance liquid chromatography-tandem mass spectrometry for testing and includes following steps: providing an ultrahigh-performance liquid chromatograph, a triple quadrupole mass spectrometer, the cattle pulmonary surfactant extract and a reference sample; determining chromatographic conditions and mass spectrometric conditions; performing liquid preparation, testing and result processing. By using the method, 11 antibiotics including tetracycline, chlorotetracycline, terramycin, doxycycline, metacycline, minocycline, beta-doxycycline, epitetracycline, epichlorotetracycline, anhydrotetracycline and epianhydrotetracycline and known impuritiescan be tested at the same time. Linear range, sensitivity, precision and recovery rate of the method all meet analysis requirements.

The invention relates to a method for measuring the residual quantity of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food, which comprises the following steps: pretreatment: crushing a sample to be measured, adding ethyl acetate, performing vortex oscillation for extraction, and then centrifuging; sucking the supernate, adding ethylenediamine-N-propyl silanized silica gel, graphitized carbon black, C18 and anhydrous magnesium sulfate for purification, carrying out vortex mixing, centrifuging, taking the supernate, and filtering a membrane to obtain an extracting solution; detecting the extracting solution by a gas chromatography-triple quadrupole mass spectrometer, and quantifying by a matrix matching external standard method. According to the method, the linear relation of the target compound in the range of 0.01-0.10 mg/kg is good, and correlation coefficients are all larger than 0.99. The average recovery rate of a blank sample at low, medium and high addition levels is 81.5%-109.4%, the relative standard deviation (n = 6) is 2.8%-9.0%, and the limit of quantitation of the method is 0.01 mg/kg. The method is simple, rapid and sensitive to operate, and can meet the detection requirements of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food.

The invention discloses a real-time direct analysis method for rapidly determining free formaldehyde in water-soaked products. The method comprises the following steps: enabling 2,4-dinitrophenylhydrazone as a reaction reagent to react with formaldehyde, taking an appropriate amount of reaction liquid to be dripped on a screen so as to be naturally dried in air to obtain a product, placing the product between a real-time direct analysis mass spectrum ion source gas outlet and a triple quadrupole mass spectrometer ion inlet, and determining, wherein DART ion source conditions are as follows: a negative ion mode is adopted and an ion source temperature is 300 DEG C, and triple quadrupole mass spectrometer conditions are as follows: the mass analyzer voltage is 3000V, and the mass-to-charge ratio of parent ions to quantitative ions to qualitative ions is 209 to 151 to 133 in a second-grade scanning mode; and by comparing second-grade mass spectrograms of a sample and a control sample, analyzing the free formaldehyde in the water-soaked products and quantifying by adopting an external standard method. The real-time direct analysis method provided by the invention has the advantages that the complex pretreatment and chromatographic separation process is not needed, the detection limit is up to 1ppm, and the detection method is sensitive, simple and convenient, and can be used for rapidly detecting the free formaldehyde in the water-soaked products.