19 results about "Hplc ms ms" patented technology

The invention provides a method for detecting N-(2-alanyl)-L-glutamine tetramer impurities in a compound amino acid liquid preparation by adopting a liquid chromatography-mass spectrometry technology, and the conditions of liquid chromatography are as follows: a chromatographic column taking amide bonded silica gel as a filler is adopted, a formic acid aqueous solution with the volume ratio concentration of 0.05%-0.3% is taken as a mobile phase A, a mobile phase B is taken as a mobile phase C, a mobile phase D is taken as a mobile phase C, a mobile phase D is taken as a mobile phase C, and a mobile phase D is taken as a mobile phase C; the method comprises the following steps: by taking a chromatographic column as a mobile phase A and a formic acid acetonitrile solution with the volume ratio concentration of 0.05-0.3% as a mobile phase B, eluting by adopting a gradient elution procedure, and the conditions of mass spectrometry are as follows: the ionization form is ESI < + >, and the detection mass-to-charge ratios are 418.1 / 218.1 and 418.1 / 147.1. The method can be used for effectively separating and detecting two alanyl-glutamine tetramer structure isomer impurities in the alanyl-glutamine liquid preparation.

The application provides a method for improving the sensitivity of liquid chromatography-mass spectrometry in detecting vitamin K1 in serum, which comprises the following steps: preparing a sample solution of vitamin K1 to be detected by using a liquid-liquid extraction method to obtain an initial sample solution; and redissolving the initial sample solution by using an aqueous solution containing at least isopropanol as a redissolving agent to obtain a sample solution to be detected; and adding ammonium fluoride after an LC-MS column to improve the mass spectrometry detection sensitivity of the vitamin K1 sample. By using the technical scheme of the application, isopropanol or isopropanol+methanol is used as a redissolving agent to replace methanol in the prior art as a redissolving agent, the mass spectrometry detection sensitivity of VK1 is improved, the recovery rate is improved, the detection method has good stability, and the clinical detection requirements can be met; meanwhile, the ammonium fluoride in the liquid chromatography can be completely replaced, the system pressure of the liquid chromatograph is reduced, and the service life of the chromatographic column is prolonged.

The utility model belongs to the technical field of liquid chromatography, and discloses a movable liquid chromatography-mass spectrometer experiment table which comprises an experiment table body, a column oven is arranged at the top of the experiment table body, an automatic sampler is arranged at the top of the column oven, a sampling groove is formed in the surface of the automatic sampler, a positioning assembly is arranged in the sampling groove, and the positioning assembly is arranged in the sampling groove. A quaternary pump is arranged at the top of the automatic sampler, a vacuum degasser is arranged at the top of the quaternary pump, a solvent bottle box is arranged at the top of the vacuum degasser, and mounting grooves are formed in four corners of the surface of the solvent bottle box. By means of the arrangement of an automatic sampler and a positioning assembly, in the using process, a worker places a reagent tube into a positioning groove, the reagent tube can extrude an arc-shaped plate, after being extruded, the arc-shaped plate can reset through a spring, and then the arc-shaped plate can clamp the reagent tube; and the efficiency of clamping the reagent tubes with different sizes is improved, and the situation that the reagent tubes fall to the ground is reduced.

The invention provides a liquid chromatography-mass spectrometry combined system and a liquid chromatography-mass spectrograph, and the combined system comprises at least two sets of liquid chromatography groups, at least one flow path distributor and a central control module, each set of liquid chromatography group comprises a sample injector module, a constant flow pump module, a switching valve, a first chromatographic column, a second chromatographic column, a column oven and a liquid phase detection module connected with an outlet of the second chromatographic column; the inlet end of the flow path distributor is selectively communicated with the outlet flow path of each second chromatographic column, and the flow path distributor is used for receiving the eluent from any liquid chromatogram group and selectively guiding the eluent to the mass spectrometer. A high-throughput, continuous and automatic on-line analysis process is realized by utilizing the combined system, the system can effectively improve the utilization rate of the mass spectrometer, simplify or replace tedious off-line pretreatment steps, and realize seamless connection of multi-sample parallel treatment and mass spectrum continuous detection through reasonable flow path design and intelligent control.

To provide a technology for improving the accuracy of compound identification in liquid chromatograph mass spectrometers, including single quadrupole mass spectrometers. [Solution] In the analytical apparatus 100, the sample contains a target compound produced by the derivatization of a short-chain fatty acid or organic acid, which is the target compound in the analyte. The central control unit 5 causes the mass spectrometry unit 2 to measure the m / z intensity of the fragments while performing insource collision-induced dissociation on the sample during a given holding time in the liquid chromatograph, and also to measure the m / z intensity of the fragments on the sample during the same given holding time without performing insource collision-induced dissociation.

A method for identifying and / or verifying at least one analyte peak in a chromatogram of a sample for said analyte from a liquid chromatography mass spectrometer device, said method comprising: a) determining a chromatogram of the sample by acquiring a plurality of data points for quantifier signal intensities and / or qualifier signal intensities, over time; and, in case the sample comprises an internal standard, optionally acquiring a plurality of data points for internal standard quantifier signal intensities and / or internal standard qualifier signal intensities, over time; b) determining for at least a fraction of the data points acquired in step a), a ratio type; c) comparing the ratios determined in step b) to a reference; and d) identifying and / or verifying at least one analyte peak in a chromatogram based on comparison step c).

This invention provides a DNA modification detection method using gel electrophoresis coupled with liquid chromatography-mass spectrometry (LC-MS / MS), comprising the following steps: separating a DNA sample to be tested by gel electrophoresis to obtain a gel strip containing the target DNA, wherein the electrophoresis buffer used in the gel electrophoresis method does not contain EDTA; enzymatically digesting the target DNA in the gel strip into single deoxynucleosides / deoxynucleotides by in-gel DNA digestion to obtain enzymatic digestion products; and detecting the enzymatic digestion products by liquid chromatography-mass spectrometry to obtain the results of DNA chemical modifications (including epigenetic modifications and DNA damage adducts). The detection method of this invention can accurately quantify the chemical modification information in different DNA components separated by gel electrophoresis.

The application provides a liquid chromatography-mass spectrometry method capable of efficiently detecting deoxynivalenol (DON) acetylated derivative: 3-acetyldeoxynivalenol (3-Ac-DON). The detection method detects 3-Ac-DON in a negative ion mode, and compared with a conventional positive ion detection scheme, the detection limit of the method is 8 ppb (10 ppb according to the national standard), and the sensitivity is higher; by using high-resolution mass spectrometry and an optimized negative ion system, the anti-matrix interference ability and the qualitative accuracy are significantly improved, and meanwhile, the method has good linearity and precision, and is suitable for accurate detection of 3-Ac-DON in various samples. The detection time of the application is 10 min, the retention time of 3-Ac-DON is 8.41 min, the detection limit is 8 ng / ml, the quantification limit is 20 ng / ml, the linear range is 20-2000 ng / ml, the correlation coefficient R 2 =0.9995, and the relative standard deviation RSD is 1.25%.

The invention relates to the technical field of biological detection, in particular to a method for synchronously determining full-chain-length perfluoro and polyfluoroalkyl compounds in a biological matrix by two-dimensional liquid chromatography-mass spectrometry, which comprises the following steps: pretreatment: removing impurities from the biological matrix by extraction and low-temperature freezing to obtain a supernatant, and carrying out nitrogen blow-drying and redissolving to obtain a supernatant; a to-be-detected sample is obtained; two-dimensional liquid chromatography-mass spectrometry: separating out a part of ultra-short chain PFAS with strong polarity in a sample to be detected through one-dimensional liquid chromatography, trapping the rest target PFAS (mainly medium-long chain PFAS) by a trapping column, supplementing liquid to the target PFAS, separating the trapped target PFAS by two-dimensional liquid chromatography, and carrying out qualitative and quantitative analysis through mass spectrometry. Through the two-dimensional liquid chromatography-mass spectrometry detection method, the synchronous detection process of 43 kinds of PFAS from ultrashort chain to long chain is realized, and stable and reliable analysis results are obtained.

This invention relates to a mass spectrometer and a liquid chromatography-mass spectrometry (LC-MS) system. The mass spectrometer includes an ion source, a first mass analyzer, a collision cell, a second mass analyzer, an ion detector, and a power supply unit. An ion transport section is provided between the ion source and the first mass analyzer in the ion transport direction. The power supply unit is designed to apply a DC voltage to the ion transport section to screen out non-target substances passing through it. The power supply unit is also designed to apply a radio frequency (RF) voltage to the ion transport section to facilitate ion transport. The LC-MS system includes the aforementioned mass spectrometer. By incorporating an ion transport section in the mass spectrometer and applying a DC voltage to it, non-target substances can be screened out, reducing contamination of downstream systems by these substances.

The invention belongs to the technical field of grain detection, and particularly relates to a grain detection method and device based on liquid chromatography-mass spectrometry, the grain detection device comprises a sample pretreatment module and a sample detection analysis module, the sample pretreatment module comprises a grain treatment device, and the sample detection analysis module comprises a sample detection analysis module. The sample detection and analysis module comprises a liquid chromatograph and a mass spectrometer and is used for testing and analyzing fungaltoxin contained in the sample; through the cleaning liquid supply system, cleaning liquid containing sterilization and disinfection components is fed into the crushing bin, crushed grain materials attached to all parts in the crushing bin and fungaltoxin components possibly attached to all the parts in the crushing bin are removed, the experiment efficiency of grain samples is improved, meanwhile, the interior of the crushing bin is fully sterilized and purified, and the experiment efficiency is improved. And the situation that residual grain crushed aggregates and fungal components are mixed into the next grain sample to affect the accuracy degree of the experiment is avoided.

The invention belongs to the technical field of analysis, and provides a liquid chromatography-mass spectrometry analysis method for polyethylene glycol series auxiliary material components and key quality attributes thereof. In particular to a high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) method for analyzing and identifying a polyethylene glycol component in an auxiliary material and a preparation and simultaneously evaluating four key quality attributes of polyethylene glycol, and the polyethylene glycol auxiliary material and a preparation sample thereof are analyzed by adopting the HPLC-HRMS analysis method. The polyethylene glycol component is identified based on high-resolution mass spectrum information and a linear relation between retention time and polymerization degree, and four key quality attributes of polyethylene glycol are evaluated based on a component identification result and an established mathematical calculation formula. According to the method, comprehensive, rapid and accurate analysis and identification of polyethylene glycol components in polyethylene glycol series auxiliary materials and preparations can be realized, simultaneous evaluation of four key quality attributes is realized, and the quality control efficiency and level of the polyethylene glycol auxiliary materials and the preparations thereof are effectively improved.

The invention relates to a liquid chromatography-mass spectrometry system including: a pretreatment module configured to pretreat a test sample; a liquid chromatography module configured to elute the pretreated test sample; a mass spectrometry module configured to perform mass spectrometry on the eluted test sample; a waste gas treatment module in fluid communication with at least one of the pretreatment module, the liquid chromatography module and the mass spectrometry module and configured to perform liquefaction and absorption of volatile waste gas in gas to be treated that is generated by the module(s) in fluid communication with the waste gas treatment module; and a control module configured to generate a waste gas treatment instruction based on waste gas-related information and to control the waste gas treatment module to initiate waste gas treatment on the gas to be treated in response to the waste gas treatment instruction.

This invention belongs to the field of detection, specifically relating to a liquid chromatography-mass spectrometry (LC-MS) analytical method for detecting ethylamine content in sodium chloride, an industrial byproduct. The method includes the following steps: sample pretreatment: adding extraction reagent to the sample, mixing, agitating and sonicating, and filtering; preparing a standard solution; and detection by LC-MS. The method of this invention is highly specific, sensitive, accurate, and reliable, meeting the requirements for detecting ethylamine content in sodium chloride, an industrial byproduct.

This invention belongs to the field of analytical chemistry and biomedical detection, and discloses a method for detecting nucleotides in biological samples based on liquid chromatography-mass spectrometry (LC-MS). The method includes: pretreatment of the biological sample by homogenization with a weakly basic ammonium acetate buffer, protein precipitation with organic solvent, vacuum concentration, and reconstitution; separation using an alkali-resistant C18 column and a weakly basic mobile phase with gradient elution; and detection by multiple reaction monitoring (MRM) in negative ion mode using an electrospray ionization source. This invention can simultaneously detect more than 40 target substances, covering bases, nucleosides, deoxynucleosides, and their phosphorylated forms and modified metabolites, with a limit of quantitation at the ng / pg / mL level. It exhibits strong resistance to matrix interference and excellent chromatographic separation. This method is rapid, highly sensitive, and stable, suitable for high-throughput and precise detection of nucleotides in biological samples, providing a powerful tool for disease biomarker screening and related basic research.

This invention relates to a liquid chromatography-mass spectrometry (LC-MS) system, comprising: a pretreatment module for pretreating a sample; a liquid chromatography module for eluting and separating the pretreated sample; a mass spectrometry module for mass spectrometry analysis of the eluted sample; and a waste gas treatment module, comprising: a suction component connected to at least one of the pretreatment module, the liquid chromatography module, and the mass spectrometry module for suctioning the gas to be treated generated by the connected modules; a waste gas treatment component disposed downstream of the suction component for liquefying and absorbing volatile waste gases in the suction gas, the waste gas treatment component including a first waste gas absorption component and a second waste gas absorption component, the second waste gas absorption component being disposed downstream of the first waste gas absorption component; and a waste liquid discharge component for discharging waste liquid. This invention enables a miniaturized waste gas treatment module.

The application discloses a kind of 210 kinds of pesticides in surface water simultaneously determination method based on solid phase extraction and liquid chromatography-mass spectrometry, it is related to water quality detection technical field.The present application comprises the following steps: S1, sample pretreatment: using hydrophilic-lipophilic copolymer (HLB) solid phase extraction column to surface water sample enrichment purification, after elution, concentration, constant volume, add internal standard mixed standard, filter and measure;S2, analysis and detection: using ultra-high performance liquid chromatography-triple quadrupole mass spectrometry, in multiple reaction monitoring mode, the sample after step S1 is handled and is detected;S3, internal standard method quantitative.The present application is through system optimization pretreatment method and chromatographic condition, using ultra-high performance liquid chromatography / triple quadrupole tandem mass spectrometry method, establishes 210 kinds of pesticides in surface water simultaneously detection analysis method, realizes to surface water in multiple pesticides simultaneously, fast determination and accurate quantification, method repeatability, precision is good, and have good accuracy.

The invention belongs to the technical field of detection and analysis, and particularly relates to a detection method and application of nicotine and metabolites thereof based on laser microdissection and liquid chromatography-mass spectrometry. A biological tissue target area sample is accurately obtained through laser microdissection with optimized parameters, and detection is completed by adopting a specific chromatographic column, a mobile phase, gradient elution and multi-reaction monitoring mass spectrum conditions after extraction pretreatment with 80% methanol water containing 0.1% formic acid. Methodology verification shows that the linear relation is good, and the precision and the accuracy both meet biological sample analysis requirements. The method is accurate in sampling, high in anti-interference capacity and suitable for quantifying trace target objects in complex tissues such as brain tissues and kidneys, and reliable technical support is provided for nicotine related research, public health monitoring and smoking cessation effect evaluation.