35 results about "Hplc ms ms" patented technology

The invention discloses a method for detecting residues of five kinds of sulfa veterinary medicines in an animal-based functional food. The method comprises the following steps of: (1) extracting a sample: weighing a proper amount of sample, extracting for 2 to 4 times by using acetonitrile as a solvent in a vortex oscillation way, combining acetonitrile solution and placing in a liquid separation funnel for later use; (2) purifying the sample: extracting the acetonitrile solution obtained in the step (1) by using normal hexane, concentrating the acetonitrile solution on the bottom layer and dissolving by using 10 percent acetonitrile water, and filtering; and (3) testing the residual amount of five kinds of sulfa veterinary medicines in the sample by using a high performance liquid chromatography-mass spectrometry-mass spectrometry (HPLC-MS-MS) system. By the test method, the separability of the five kinds of the sulfa veterinary medicine residues in the functional food is high, the sensitivity is high, and the selectivity and the specificity are high; matrix interference and false positive can be eliminated effectively, and the minimum detection concentration is low; furthermore, in a sample treatment process, the degressive amount of acetonitrile is used for extracting, so that the recovery rate of targets is guaranteed, the using amount of organic solvents is reduced, the emission of waste liquid is reduced and the detection cost is saved.

The present invention relates to the determination of the presence of methylmalonic acid in biologic samples including the steps of methylmalonic extraction from the sample; derivatization of methylmalonic acid and use of mass spectrometry with negative mode atmospheric pressure chemical ionization to determine the presence of methymalonic acid through the formation of an ion of mass to charge ratio (m / z) 477. An additional objective of the present invention concerns diagnosis kits for determination of presence and quantification of methylmalonic acid based on the method mentioned before.

The invention relates to a method for detecting a nitrofuran drug in eel. The method comprises the following steps: weighing 4 g of an eel sample, adding 20 ml of a hydrochloric acid solution with concentration being 0.2 mol / L, adding 1 ml of a derivating agent, uniformly shaking with hands, performing a water-bath reaction at the temperature of 60 DEG C for 1 h, taking the sample out and coolingthe sample to room temperature, using a NaOH solution for adjusting the pH value to 7.0-7.5, performing centrifugation for 10 min, taking a half of a supernatant, using 5 ml of methanol and 5 ml of distilled water, activating a solid-phase extraction column; separating the supernatant by a column, using 5 ml of distilled water for leaching, removing a leacheate, using 2 ml of methanol for elutinga solid-phase extraction column, collecting an eluate, drying the material with nitrogen at the temperature of 40 DEG C, using 1 ml of a furan solution for dissolving, filtering the material by a microfiltration membrane, and performing HPLC-MS-MS detection. The method has the advantages of high extraction efficiency, short derivating time, and high sensitivity, precision and accuracy.

The invention discloses a method for detecting chloramphenicol residual in a functional food through HPLC-MS-MS. The method comprises the following steps: weighing a sample, adding deuterated chloramphenicol as an internal standard solution, adding ethyl acetate, ammonium hydroxide and anhydrous sodium sulfate, homogeneously extracting, centrifuging, and transferring the obtained supernatant to a heart-shaped bottle; concentrating the supernatant in the heart-shaped bottle to dryness; dissolving with water, carrying out ultrasonic treatment, adding n-hexane, carrying out vortex mixing, allowing the obtained solution to stand for layering, discarding n-hexane which is the upper layer, adding n-hexane, carrying out vortex mixing, allowing the obtained solution to stand for layering, transferring the obtained water phase to a centrifuge tube, centrifuging, and allowing the centrifuged water phase to go through a filter membrane to obtain a final solution for the determination through HPLC-MS-MS; accurately weighing a chloramphenicol standard substance, carrying out ultrasonic dissolving with chromatographically pure methanol, adding the chromatographically pure methanol to a constant volume, and preparing chloramphenicol standard substance solutions having different concentrations; determining the chloramphenicol standard substance solutions through the HPLC-MS-MS to obtain a standard curve; and calculating according to obtained examination data through the standard curve to obtain the concentration of chloramphenicol in the sample to be measured. The method has the advantages of good accuracy, high precision and good linearity.

The invention discloses a liquid chromatography-mass spectrometry combined metabolite detection method, comprising the following steps: performing first online detection on a sample to be detected; introducing a standard product detection database file; preparing first detection result offline data of the sample to be detected; preparing DP and CE combined gradient information; setting a peak height threshold; deriving DP and CE optimization results; establishing a DP and CE optimization database according to optimized detection results. According to the method, the DPCE optimization conditionanalysis and the time consuming of a conventional project are greatly reduced. The sample collection situation is accurately monitored by using 2-chlorophenylalanine as a general internal standard, and the fluctuating state of an instrument is monitored by using 17 mixed standards as general quality control products. The data analysis and time are greatly reduced, accurate monitoring of the collection process and the instrumental fluctuation is realized, and the experimental efficiency of liquid chromatography-mass spectrometry series detection is improved.

The invention relates to an analysis method for simultaneously detecting six sweetening agents in feng-flavor liquor by high performance liquid chromatography-mass spectrometry. The method comprises the steps of treating a sample in a water bath, fixing the volume, filtering with a 0.22 mu m filter membrane and putting on a machine to analyze; taking a Shin-pack XR-ODSIII C18 column as a separation column and 10% of formic acid-methanol as a mobile phase, carrying out gradient elution, carrying out high performance liquid chromatography separation, scanning in an ESI negative ion mode, and carrying out multi-reaction monitoring mode (MRM) detection. According to the method disclosed by the invention, the measurement time only needs 7 minutes, the detection efficiency is improved, the detection limit and the quantification limit are lower, and the precision of the instrument and the method is high; the method is simple, quick, accurate and reliable; a high-performance liquid phase is adopted in a liquid phase part, so that the detection cost is reduced; the pretreatment of the sample is to heat in the water bath at 60 DEG C, so that not only is the matrix effect caused by alcohol avoided, but also the situation that the aspartame is not stable at high temperature, is prevented.

The invention belongs to a field of foodstuff detection and foodstuff safety, and relates to a method for determining content of natamycin in wine, especially relates to a method which employs a solid phase extraction column for purification and a HPLC-MS / MS method for detection. The method comprises the following steps: (1) activation, (2) adjustment of wine sample pH value, (3) sampling, (4) leaching, (5) elution, (6) drafting of a natamycin standard curve, (7) calculation of the content of natamycin in the wine sample. According to the invention, the method for detecting the content of natamycin in wine is rapid and effective, the detection time is 5 minutes, the detection limit 1mug / l, the quantification limit is 3.34mug / l, and the error is 2-4%. Besides, because the HPLC-MS-MS technology is used, the false positive is effectively eliminated.

The invention relates to a high performance liquid chromatography-mass spectrum-mass spectrum (HPLC-MS-MS) combined detection method for (S)-NNAL and (R)-NNAL in urine. Derivatization and an HPLC-MS-MS method are adopted for determining (S)-NNAL and (R)-NNAL in urine. The HPLC-MS-MS combined detection method comprises the following steps of: determining configuration of (S)-NNAL and (R)-NNAL by adopting a rotation determination and comparison method and taking the configuration as a reference, or determining configuration of (S)-NNAL-(S)-(+)-allpha-methoxy-alpha-trifluoromethyl acetic acid ester and (R)-NNAL-methyl-d3-(S)-(+)-alpha-methoxy-alpha-trifluoromethyl acetic acid ester and taking the configuration as the reference; preparing a mixed standard solution containing rac-NNAL and deuterated rac-NNAL-methyl-d3, then carrying out Mosher derivatization, and then carrying out HPLC-MS-MS analysis on the derivatized mixed standard solution; and finally detecting (S)-NNAL and (R)-NNAL in urine. The HPLC-MS-MS combined detection method provided by the invention has the advantages of low detection limit, good stability, simple pre-treatment, high speed and high accuracy.

The invention provides a method for simultaneously measuring the contents of 7 polyphenol active ingredients in different varieties of osmanthus fragrans through an HPLC-MS-MS method, and belongs to the field of biochemical technology. The method comprises the following steps: performing gradient elution by using a chromatographic column Shim-pack VP-ODS (2.0 x 150mm, 5[mu]m) and using methanol-0.1% formic acid water as a mobile phase, wherein the volume flow rate is 0.2mL.min-1, the column temperature is 30 DEG C, and the sample size is 5 uL; and using an ESI ion source as a mass spectrum, and performing detection in a multi-reaction monitoring anion scanning method, wherein the result indicates that the 7 components have a good linear relationship within a measured concentration range. The precision, the repeatability and the stability are good; and the requirements of methodological investigation are met. The established method is simple, rapid, sensitive and highly specific, and can be used for the simultaneous measurement of 7 polyphenol active ingredients in the osmanthus fragrans, namely, chlorogenic acid, caffeic acid, verbascoside, naringin, rutin, ferulic acid and quercetin.

The invention relates to a method for detecting carbamazepine blood drug concentration by liquid chromatography-mass spectrometry. The method comprises the following specific steps: preparing a carbamazepine stock solution; preparing a calibration product solution; preparing a quality control product solution; pretreating a to-be-detected sample; setting liquid chromatography-mass spectrometry experimental parameters; performing liquid chromatography tandem mass spectrometry analysis on the treated to-be-detected serum sample according to 2microliters of the sample; and finally calculating theconcentration of carbamazepine in the serum sample. The matrixes of the standard substance solution and the quality control substance solution use the animal serum to replace human serum, the detection cost is reduced, and the method for detecting the concentration of carbamazepine in serum is accurate, rapid and high in specificity.

The invention discloses a method for detecting 4-hydroxyl-4-(3-pyridyl) butyric acid in urine. The method comprises the following steps: purifying a urine sample by using an Oasis MCX solid-phase extraction small column; carrying out methyl esterification on carboxyl in the sample and carrying out esterification on alcoholic hydroxyl; then carrying out HPLC-MS-MS (High Performance Liquid Chromatography-Mass Spectrometry-Mass Spectrometry) detection on a derived urine sample so as to calculate the concentrations of (S)-4-hydroxyl-4-(3-pyridyl) butyric acid and (R)-4-hydroxyl-4-(3-pyridyl) butyric acid in the urine sample; and calculating a ratio of the (S)-4-hydroxyl-4-(3-pyridyl) butyric acid to the (R)-4-hydroxyl-4-(3-pyridyl) butyric acid in the urine sample. The method can provide a scientific judgment method for estimating metabolism health conditions to nicotine, nornicotine, NNK (Nicotine-derived Nitrosamine Ketone) and NNAL ((4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol)) by an individual body, and evaluating the exposure degree to substances in smoke, has the advantages of low detection limit, good stability, rapidness and accuracy and the like, and fills the blank of the technical field.

The invention discloses a method for detecting chloramphenicol residual in a functional food through HPLC-MS-MS. The method comprises the following steps: weighing a sample, adding deuterated chloramphenicol as an internal standard solution, adding ethyl acetate, ammonium hydroxide and anhydrous sodium sulfate, homogeneously extracting, centrifuging, and transferring the obtained supernatant to a heart-shaped bottle; concentrating the supernatant in the heart-shaped bottle to dryness; dissolving with water, carrying out ultrasonic treatment, adding n-hexane, carrying out vortex mixing, allowing the obtained solution to stand for layering, discarding n-hexane which is the upper layer, adding n-hexane, carrying out vortex mixing, allowing the obtained solution to stand for layering, transferring the obtained water phase to a centrifuge tube, centrifuging, and allowing the centrifuged water phase to go through a filter membrane to obtain a final solution for the determination through HPLC-MS-MS; accurately weighing a chloramphenicol standard substance, carrying out ultrasonic dissolving with chromatographically pure methanol, adding the chromatographically pure methanol to a constant volume, and preparing chloramphenicol standard substance solutions having different concentrations; determining the chloramphenicol standard substance solutions through the HPLC-MS-MS to obtain a standard curve; and calculating according to obtained examination data through the standard curve to obtain the concentration of chloramphenicol in the sample to be measured. The method has the advantages of good accuracy, high precision and good linearity.

The invention discloses a detection method of ochratoxin A in cereals. The detection method comprises steps as follows: a cereal sample is dissolved in an acetonitrile solution, a mixed solution is centrifuged, a supernatant is collected and injected to an amine solid phase extraction column for elution, an eluent is collected and blow-dried, residues are obtained and re-dissolved in a methanol solution, filtering is performed, filtrate is a sample purification liquid, the sample purification liquid is subjected to HPLC-MS-MS (high performance liquid chromatography-tandem mass spectrometry) detection, a detection result is substituted into a curve of a formula 1 for comparison, and the content of ochratoxin A in the sample is obtained. The detection method solves the problem of high cost caused by adoption of an immunoaffinity column for detection of ochratoxin A in the prior art, has the characteristics of being simple, fast, sensitive and accurate, and is applicable to detection of massive samples, and an accurate analysis method can be provided for quality security risk assessment of agricultural products.

The invention discloses a method for detecting NNAL (4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol) and NNA in cut tobacco and cigarette smoke. The method comprises the steps: preparing a mixed standard solution containing NNAL, NNA and NNA-methyl-d3, and respectively establishing standard solution working curves of NNAL and NNA by adopting an internal standard method; and then adding an NNA-methyl-d3 solution in a sample, adding an extraction solution, oscillating at a room temperature, collecting supernate, and performing HPLC-MS-MS (High Performance Liquid Chromatography-Mass Spectrometry) detection. The method has the advantages of low detection limit, good stability, rapidness and accuracy, and the like; a detection result is influenced by a subjective judgment factor a little, and thus the method is easy to popularize and apply.

The invention discloses a liquid chromatogram-mass spectrum combined analysis method and device and a control system and method of the liquid chromatogram-mass spectrum combined analysis device. The analysis method comprises the following steps: carrying out one-dimensional liquid chromatography separation on a biological sample to be detected to obtain a one-dimensional eluent, carrying out two-dimensional liquid chromatography separation on the one-dimensional eluent, carrying out series on-line mass spectrometry, and directly carrying out series on-line enzymolysis and on-line trapping on the one-dimensional eluent, and carrying out series on-line two-dimensional liquid chromatography separation on the captured enzymolysis components. According to the method, on-line enzymolysis and 2D-MS are realized for a biological sample needing enzymolysis, the method has universality for the biological sample, the analysis efficiency can be effectively improved, the original analysis time of two weeks is shortened to less than two hours, the analysis cost is greatly reduced, and the method can be used for detection and analysis in industrialization and has wide application prospects. And guidance can be provided for scientifically developing antibody drug research and development.

The invention belongs to the technical field of contaminant determination and discloses a method for determining perfluorooctanesulfonic acid and perfluorohexanesulfonic acid in edible parts of crops. The method comprises the main steps: freezing, drying and crushing the edible parts of the crops so as to obtain a sample, adding an internal standard substance into the sample, carrying out uniform mixing, then, adding a disassociation agent into the mixture for a disassociation reaction, then, adding tetrabutylammonium bisulfate and a sodium carbonate buffer solution into the reaction solution, carrying out uniform mixing thoroughly, then, adding methyl tert-butyl ether into the mixture for ultrasonic extraction, so as to obtain an extract; subjecting the extract to solid-phase extraction purification by graphite carbon black loaded WAX columellae so as to obtain sample detection liquid, and determining the sample detection liquid by adopting an HPLC-MS-MS method. According to the method disclosed by the invention, the recovery rate is high, the accuracy is good, the sensitivity is high, and the method is resistant to interference of complicated matrixes; meanwhile, the method is applicable to the determination on perfluorooctanesulfonic acid and perfluorohexanesulfonic acid in cereals, root vegetables, leaf vegetables and fruit vegetables.

The invention relates to a liquid chromatography-mass spectrometry detection method of cephalosporin antibiotics. The method is characterized by comprising the following steps: (1), performing samplepretreatment; to be specific, removing suspended matters from a certain number of water sample through a centrifuge, carrying out suction filtration, and regulating the pH value of the water sample; (2), performing sample extraction; to be specific, leaching an extraction column for activation, then adding a chelating agent into the water sample and fully mixing the substances, enabling the watersample to pass through an extraction column, then flushing the sample-passing extraction column, then performing drying and eluting, collecting eluent and blowing the eluent to be nearly dry to obtainresidues; and (3), performing mass spectrum detection; to be specific, dissolving the residues to obtain a to-be-detected solution, and detecting the to-be-detected solution under certain gradient elution conditions and mass spectrum detection conditions. Compared with the prior art, the method has the advantages of simple operation, strong specificity, high accuracy, good tolerance, high instrument sensitivity and the like.

The invention provides a method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry. The method comprises: S01, adding an extraction agent to a sample to be detected, and carrying out ultrasonic extraction under an ice bath condition; S02, carrying out centrifuging, and separating supernatant and precipitate; S03, adding an extracting agent into the precipitate, and carrying out repeated centrifuging; and S04, combining the supernatant obtained by each centrifugation, carrying out purifying, and carrying out high performance liquid chromatography-mass spectrometry detection. The trimethylamine is detected by utilizing the established method; the content of trimethylamine in an actual sample is converted according to the matrix inhibition ratio of trimethylamine in food. The method is simple to operate, economical and practical; the standard curve of trimethylamine obtained in a range of 0 to 200ng / mL has the linear correlation R being 0.9994, the detection limit being 11.2 microgramme / kg, the low detection limit reaching ppb level, the high sensitivity; and the method can be used for accurately detecting trimethylamine in food.

The invention discloses a method for detecting content of essence in a rice product in the technical field of agricultural product detection. The method specifically comprises the steps of sample pretreatment, extraction, centrifugation, mixing, purification, filtration, HPLC-MS-MS quantitative determination, and the like, wherein the pH value of a water phase in a liquid chromatographic mobile phase is 2.7. Compared with the traditional liquid chromatographic method, the gas chromatographic method and the like, the method disclosed by the invention is fast, simple and convenient, the extraction and purification steps are few, a large amount of manpower and material resources can be saved, fewer samples and organic extraction solvents can be consumed in the pretreatment process, a better purification effect is achieved, the recovery rate of the method is high, the detection limit is lower, and peaking of 2-acetyl pyrazine in an ion chromatogram is more perfect.

The invention relates to an LCMS detection method for potential genotoxic impurities in irbesartan. The method comprises the following steps: injecting a blank solution, a reference solution and a test solution into a liquid chromatograph-mass spectrometer, and recording a chromatogram. The LCMS detection method for the potential genotoxic impurities in the irbesartan, provided by the invention, is implemented through a high performance liquid chromatography-mass spectrometry method, and can be used for sensitively and accurately detecting the potential genotoxic impurities in the irbesartan; and the system specificity, the detection limit and the quantitation limit, the linearity and the range, the solution stability, the precision, the accuracy and the durability are verified by referring to the related content of the Chinese pharmacopoeia, and all the aspects meet the requirements.

The invention relates to the technical field of acetonitrile purification, more specifically, the invention relates to an improved acetonitrile purification process for ultra-high liquid chromatography-mass spectrometry. The invention provides an acetonitrile purification process, through the operation of oxidation, rectification and adsorption, drying, reflux rectification and filtration of industrial acetonitrile, and related parameters such as temperature and flow are controlled, high-purity finished products can be obtained to ensure continuous production, Its transmittance of ultraviolet light at 200-260nm is greater than or equal to 95%, removes water and impurities in industrial acetonitrile, and meets the requirements of ultra-high liquid chromatography-mass spectrometry; and by controlling process parameters and equipment, the finished product can be improved. The yield reaches more than 95%, and the purification efficiency is improved; in addition, the present invention replaces the adsorption column by using an adsorption rectification tower, which can increase the regeneration efficiency and reduce environmental pollution while improving the purity.