1901 results about "Chromatography column" patented technology

The invention discloses an organic sample analysis method based on micro gas chromatography and a chromatographic analyzer, particularly relates to the technical field of micro gas chromatography, and is used for solving the problems of unstable separation performance and low complex sample detection precision caused by insufficient uniformity of a stationary phase coating of an existing micro chromatographic column. The method comprises the following steps: constructing a stationary phase distribution initial profile by continuously pre-charging carrier gas, alternately applying segmented temperature gradient, micro-negative pressure and directional pulse flow to remodel a uniform distribution layer, generating a correction factor set of a temperature-resistance coupling relationship by combining a correction mixture and a tracer gas pulse, dynamically adjusting a carrier gas flow velocity and a temperature program to generate a matched operation curve, and finally, carrying out dynamic calibration. High-precision separation detection and quantitative analysis are achieved, stable separation performance is maintained in a miniaturized structure by cooperatively controlling stationary phase distribution optimization and real-time parameter feedback correction, and the detection precision and reproducibility of a wide-boiling-range organic mixture are improved.

The invention belongs to the field of blood product separation, and discloses a high-efficiency chromatography system and method for blood product separation, and the system comprises an intelligent chromatography column module, an automatic sample injection and accurate flow rate control module, a chromatography filler and column design module, a real-time detection and data analysis module, and an intelligent automatic control and management module. By designing an efficient micro-nano filler chromatographic column and matching with a pulsed electric field auxiliary technology and intelligent automatic control, efficient and high-purity separation and purification of target blood product components are realized. The intelligent regulation and control module used in the invention can dynamically regulate chromatography conditions in real time, and the problems of unstable flow velocity and column pressure in the traditional method are thoroughly solved. And meanwhile, a multi-point real-time detection and feedback technology is adopted, so that the separation process is more accurate, transparent and controllable.

The invention discloses an on-load tap-changer oil dissolved gas monitoring device which comprises a variable capacity container, a two-way electromagnetic valve, a switching mechanism, a chromatographic column system, a high-sensitivity detector and a low-sensitivity detector which are sequentially connected, and the top and the bottom of the variable capacity container are connected through a circulating pump to form a gas flow loop. The variable-capacity container is connected with the on-load tap-changer through a connecting pipe, the switching mechanism is connected with at least two quantitative pipes with different capacities, and the switching mechanism is used for equally transferring gas in the variable-capacity container to the quantitative pipes and then sequentially transferring the gas in the quantitative pipes to the chromatographic column system. The invention further discloses a method for monitoring the dissolved gas in the on-load tap-changer oil. According to the monitoring device and the monitoring method for the dissolved gas in the oil of the on-load tap-changer, the detection range of the concentration is improved, a concentration blind area which is not detected and misjudgment of signal saturation can be avoided, and the detection accuracy is improved.

The invention discloses a liquid chromatography-mass spectrometry data peak shape recognition processing method and related equipment, and relates to the field of data processing. The method comprises the following steps: acquiring liquid chromatography-mass spectrometry data; extracting morphological characteristic data of a chromatographic peak based on the extracted ion current chromatogram time sequence; calculating and extracting a signal complexity index of the ion current chromatogram time sequence; adjusting peak shape identification parameters according to the signal complexity index, wherein the peak shape identification parameters comprise a noise threshold value and a peak width range; distinguishing the chromatographic peak into a normal peak or an abnormal peak by using the adjusted peak shape identification parameter; searching a liquid phase method optimization scheme matched with the morphological characteristic data of the abnormal peak in a preset optimization database, wherein the liquid phase method optimization scheme comprises gradient elution time adjustment, mobile phase proportion optimization or chromatographic column replacement suggestion; and sending the liquid phase method optimization scheme to a user. According to the invention, various abnormal peak shapes can be automatically and accurately identified, and the reliability and accuracy of identification are guaranteed.

The invention relates to the technical field of liquid chromatogram data processing, in particular to a liquid chromatograph state detection and maintenance method which comprises the following steps: establishing a multi-parameter online monitoring system which comprises a normal data set and an abnormal data set; learning the normal data set and the abnormal data set, and collecting real-time monitoring data to be matched with a known fault mode; according to the real-time monitoring data, the control unit draws a pressure curve and calculates a pressure fluctuation value; determining the test period of the chromatographic instrument based on the pressure fluctuation value and the baseline noise peak value, or sending an equipment fluctuation monitoring signal and calculating the difference value between the chromatographic column temperature and the environment temperature: determining the heating power of a constant-temperature box based on the difference value between the chromatographic column temperature and the environment temperature, or sending an equipment fluctuation monitoring signal; and determining the temperature correction coefficient of the chromatographic column according to the equipment vibration frequency. According to the invention, the operation stability and effectiveness of the liquid chromatograph are improved.

The invention discloses a fruit and vegetable exosome extraction method based on ligand fishing. The fruit and vegetable exosome extraction method comprises the following steps: suspending amino-functionalized Fe3O4 (at) SiO2 nanoparticles in a glutaraldehyde solution, and adding activated agglutinin to obtain Fe3O4 (at) SiO2-agglutinin nanoparticles; adding a glutaraldehyde solution into agarose gel to obtain a size exclusion chromatographic column filler; the method comprises the following steps: dispersing Fe3O4 (at) SiO2-lectin nanoparticles in a PBS buffer solution to obtain a uniform suspension, adding the uniform suspension into a size exclusion chromatographic column filler to obtain a uniform slurry, filling the size exclusion chromatographic column with the uniform slurry, and flushing with the buffer solution to form a magnetic bead stationary phase; and loading fruit and vegetable supernatant into a size exclusion chromatographic column, passing through the magnetic bead stationary phase, cleaning residual impurities combined on the exosome-magnetic bead compound by using a buffer solution, and dissociating the exosome from the magnetic beads by using a competitive eluent of the exosome to obtain the high-purity fruit and vegetable exosome. The problem that an existing exosome extraction method is difficult to meet the requirements of high efficiency, simplicity, high purity and high activity at the same time is solved.

The utility model relates to the technical field of ion chromatographs, in particular to a column oven of an ion chromatograph. A column oven of an ion chromatograph comprises a column oven structure and a column oven isothermal body arranged in the column oven structure, a chromatographic column and a temperature control assembly are arranged on the column oven isothermal body, a heat insulation structure matched with the column oven isothermal body is arranged in the column oven structure, and a valve assembly matched with the chromatographic column to form a passage is further arranged in the column oven structure. According to the utility model, by controlling and monitoring the temperature in the column box structure, the temperature can be accurately controlled and maintained in a proper range, so that the temperatures of the chromatographic column, the environment, the liquid and the like are consistent, and the reliability and the accuracy of an analysis test are ensured.

The invention belongs to the field of detection and analysis, and relates to a method for separating and detecting enantiomers in (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride. According to the method, HPLC is adopted for separation and detection, a polysaccharide derivative chiral chromatographic column is selected as a chromatographic column, a mobile phase A is a weak base aqueous solution, and a mobile phase B is acetonitrile and / or methanol. The method is strong in specificity, high in separation degree, high in accuracy, stable, reliable and high in sensitivity, and a simple, accurate, rapid and reliable detection method is provided for control of impurities in a starting material of (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride.

The invention discloses a construction method and an identification method of characteristic chromatograms of a senecio scandens medicinal material as well as decoction pieces, standard decoction and formula granules thereof, and relates to the technical field of traditional Chinese medicine identification. The construction method of the specific chromatogram comprises the following steps: extracting a to-be-detected sample with methanol to obtain a test solution; the method comprises the following steps: dissolving 5-caffeoylquinic acid, chlorogenic acid, caffeic acid, 4-caffeoylquinic acid, rutin, hyperoside, isoquercitrin and 4, 5-dicaffeoylquinic acid with methanol to obtain a reference solution; and a liquid chromatograph is adopted for determination. A chromatographic column of the liquid chromatograph takes phenyl-methyl polysiloxane as a stationary phase, acetonitrile as a mobile phase A and 0.05 vol%-0.3 vol% formic acid aqueous solution as a mobile phase B for gradient elution. The information of the characteristic chromatogram constructed by the method is rich, and the quality of the senecio scandens medicinal material, decoction pieces, standard decoction and formula granules can be quickly and comprehensively reflected.

The invention relates to the technical field of chromatographic detection and material characteristic analysis, and discloses a multiphase chromatographic analysis system and method.The multiphase chromatographic analysis system comprises a multiphase sample injection module, a multi-field cooperative regulation and control separation column module and a plurality of separation chromatographic columns which are sequentially connected, and the separation chromatographic columns comprise partitions and are installed in a column box in an end-to-end connection mode; a temperature gradient field, an electric field gradient field, a controllable electromagnetic field and a fluid power field; and a multi-modal detection module, a data acquisition and control module and an auxiliary module. Through the brand-new multi-phase sample injection module, the multi-field coordinated regulation and control separation column module and the multi-mode detection module, direct input of detected objects in different phase states can be met, and phase state conversion is carried out according to needs, so that the phase state compatibility of the analysis system to the detected objects is obviously enhanced; and different components can be obviously separated according to different boiling points, migration speeds and magnetic susceptibilities by combining multi-field synergistic separation, so that the chromatogram is more accurate.

The invention belongs to the field of egg by-product processing, and particularly relates to a preparation method and application of eggshell membrane peptides, the preparation method of the eggshell membrane peptides comprises the following steps: S1, drying and crushing cleaned eggshells, and then separating eggshell membranes; s2, putting the eggshell membrane into a steam explosion machine, carrying out pressure maintaining treatment for 1-5 minutes under the pressure of 1.0-1.5 MPa, then instantly releasing the pressure, and collecting a steam explosion sample; s3, adding the eggshell membrane subjected to steam explosion treatment into a sodium hydroxide aqueous solution with the pH value of 7-9 according to the solid-liquid ratio of 1: (20-30), then adding alkaline protease according to the enzyme addition amount of 5000-15000U / g, carrying out enzymolysis for 5-10 hours at the temperature of 35-65 DEG C, then inactivating for 3-5 minutes at the temperature of 100 DEG C, filtering enzymatic hydrolysate, taking filtrate, centrifuging, taking supernate, and freeze-drying to obtain polypeptide; s4, polypeptide obtained in S3 is dissolved in an activation solution to be activated for 8-10 h at the temperature of 4-8 DEG C; and S5, separating the sample activated in the step S4 through a Sephadex G-15 chromatographic column to obtain the activated eggshell membrane peptide. Based on the method, the preparation efficiency is high, and the prepared eggshell membrane peptide is high in antioxidant activity.

The invention relates to a chromatographic instrument temperature control method and system, an intelligent terminal and a storage medium, and relates to the technical field of chromatographic instrument sample separation.The method comprises the steps that the sample type of a preset sample is obtained; analyzing the sample type to determine a window heating rate and a window target temperature; acquiring a chromatographic column initial temperature of a preset chromatographic column; analyzing the initial temperature of the chromatographic column and the target temperature of the window to determine the temperature of the chromatographic column needing to be increased; analyzing the temperature required to be increased and the window heating rate of the chromatographic column so as to determine the heating time of the chromatographic column; and controlling a preset chromatographic column temperature regulation and control device to perform temperature control on the chromatographic column according to the chromatographic column heating time and the window target temperature. The method has the effect of improving the precision of the temperature retention time.

The utility model discloses a chromatographic column filtering device, which relates to the technical field of installation equipment and comprises a chromatographic column main body and a liquid inlet fixed on one side of the chromatographic column main body. Through the arrangement of the vibration mechanism arranged on the back of the filter screen and the cleaning mechanism arranged in the motor box, when the surface of the filter screen is cleaned, the servo motor on the back of the filter screen is started, the servo motor drives the eccentric wheel on one side to rotate, and the eccentric wheel is influenced by centripetal force to drive the servo motor to vibrate; and secondly, a driving motor in a motor box on one side is matched, the driving motor drives a brush head to sweep the surface of the filter screen, and the impurities on the surface of the filter screen are swept down. The filter screen is cleaned in a vibrating and sweeping mode, and the service life of the filter screen is prolonged.

The invention relates to a method for detecting and / or purifying a protein polymer and application thereof. The method comprises a step of detecting the protein polymer based on HPLC-SEC. The chromatographic conditions are as follows: a chromatographic column is a molecular size exclusion high performance liquid chromatographic column; and a PB buffer solution with the concentration of 50-200mM is used as a mobile phase. The method disclosed by the invention is good in separation degree, simple to operate, short in peak appearance time and short in detection time, and has good method reproducibility and stability.

The invention relates to the technical field of immobilized lipase, in particular to immobilized lipase taking modified nano SiO2 as a carrier as well as a preparation method and application of the immobilized lipase. The immobilized lipase sold in the market is high in price and poor in mechanical strength, the enzyme loss is too large due to shear force or carrier structure damage in the continuous production process, and the transesterification efficiency is poor. In order to solve the technical problems, the invention provides the immobilized lipase taking the modified nano SiO2 as the carrier, the immobilized lipase is obtained by sequentially grafting a modified nano silicon dioxide carrier with an amino silane coupling agent and an epoxy silane coupling agent and loading lipase on the surface of the modified nano silicon dioxide carrier, according to the method, the immobilized lipase forms an enzyme column in a chromatographic column and then serves as a reactor, damage of mechanical stirring to lipase particles is avoided, the ester exchange degree is more effectively controlled by adjusting the flow speed of a substrate, the production cost of an enterprise can be remarkably reduced, and the product quality is improved.

The invention discloses a method for rapidly determining the content of breast milk oligosaccharide in dairy products, which comprises the following steps: sampling and pretreating different types of dairy products according to sample states, carrying out ultrasonic extraction, refrigerated centrifugal degreasing and centrifugal ultrafiltration protein purification on the obtained sample, and reducing the purified sample solution by using sodium borohydride to obtain a sample solution to be detected; reducing the breast milk oligosaccharide standard substance by sodium borohydride to obtain a standard solution to be detected; determining the standard substance solution and the to-be-detected sample solution by adopting ultra-high performance liquid chromatography-tandem mass spectrometry, establishing a standard curve, and carrying out quantitative analysis on the to-be-detected sample solution; the chromatographic conditions are as follows: an ACQUITY UPLC BEH Amide hydrophilic interaction chromatographic column is adopted; the mobile phase A is 20 mmol / L ammonium formate; the mobile phase B is acetonitrile; and gradient elution.

The invention discloses a method for detecting an intermediate acetylglucose of tetraacetyl by an HPLC-CAD (High Performance Liquid Chromatography-Computer Aided Design) method. The method comprises the following steps: (1) preparing a reference substance solution, namely dissolving acetylglucose by adding a diluent, and diluting to prepare the reference substance solution; (2) preparation of a test solution: taking tetraacetyl, adding a diluent solvent, and diluting to prepare the test solution; and (3) detecting the content of acetyl glucose in the test sample by adopting an HPLC-CAD (High Performance Liquid Chromatography-Computer Aided Design) method, and taking octadecylsilane chemically bonded silica as a filler in an adopted chromatographic column. According to the method disclosed by the invention, the intermediate acetyl glucose of the tetraacetyl substance is detected based on an HPLC-CAD (High Performance Liquid Chromatography-Computer Aided Design) method, and CAD parameters, a chromatographic column, a mobile phase, a diluent and a sample concentration are selected, so that the aims of effectively separating and accurately detecting the acetyl glucose in the sample can be fulfilled; the method has the advantages of simplicity, sensitivity, high accuracy, high repeatability, high specificity, good durability, high precision and the like, and has certain guiding significance on carbohydrate compound detection.

The present invention discloses a method for alcoholysis of EVA, which relates to the technical field of EVA. The technical solution is as follows: S1 Soak the alkaline anion exchange resin in deionized water for swelling; S2 Wash the alkaline anion exchange resin in deionized water; S3 Pack the washed alkaline anion exchange resin in a chromatography column and wash it with a hydrochloric acid solution; S4 Wash the eluted alkaline anion exchange resin with deionized water until neutral, and then wash it with a sodium hydroxide solution to obtain the activated alkaline anion exchange resin; S5 Pass the EVA solution through the activated alkaline anion exchange resin chromatography column to obtain crude EVOH; S6 The crude EVOH after alcoholysis is washed with water and dried under vacuum, then enters the extrusion equipment, and is granulated and washed to obtain EVOH resin. The present invention solves the problems of introducing metal impurities by the NaOH catalyst, complex post-treatment process and environmental pollution, and reduces the preparation difficulty and cost of EVOH.

The invention discloses a gas chromatographic analysis device and a gas chromatographic analysis method, and relates to the technical field of detection and analysis. The gas chromatographic analysis device comprises a sample injector, a column oven and a detector. The sample injector comprises a plurality of sample injection pipelines; a plurality of chromatographic columns and a conduction device are arranged in the column oven, each chromatographic column is provided with a sample inlet end and a sample outlet end which are oppositely arranged, and the plurality of sample inlet ends are correspondingly communicated with the plurality of sample inlet pipelines; the conduction device comprises a plurality of input ends and an output end, and the plurality of input ends are correspondingly communicated with the plurality of sample outlet ends; the detector is communicated with the output end; the plurality of chromatographic columns are arranged to be chromatographic columns with at least two polarities. Continuous detection and analysis can be realized only by selecting the corresponding sample inlet, so that the long-term use and maintenance cost is reduced, and the risk of simultaneous sample injection of a plurality of chromatographic columns due to improper valve switching is reduced.

The invention discloses a liquid chromatograph, a component separation method, a storage medium and a product, and relates to the technical field of mixture separation, the provided liquid chromatograph comprises a solvent and flow path module, the solvent and flow path module comprises a metering pump and at least one mobile phase liquid storage bottle; the sample separation module comprises a sample injector and a chromatographic column; the component detection module comprises a detector; the component collecting module comprises a plurality of middle collecting bottles and at least one target collecting bottle; the main control module at least comprises a parameter prediction model, and the parameter prediction model is used for outputting separation parameters based on the to-be-separated sample and controlling the solvent and flow path module, the sample separation module, the component detection module and the component collection module. The invention aims to solve the technical problem of how to improve the working efficiency of the liquid chromatograph.

The invention relates to the technical field of pharmaceutical analysis, and particularly discloses a method for detecting related substances of 4-chlorobenzoyl chloride. According to the method, a chromatographic column with 50% of phenyl and 50% of methylpolysiloxane as a stationary liquid is adopted to perform gas chromatographic analysis on a 4-chlorobenzoyl chloride sample, and accurate detection of four related substances, namely methyl parachlorobenzoate, ethyl parachlorobenzoate, o-chlorobenzoyl chloride and m-chlorobenzoyl chloride, in the 4-chlorobenzoyl chloride and the content of the four related substances is realized at the same time. The detection method is high in specificity, low in detection limit and quantitation limit, good in linear relation, high in recovery rate, good in repeatability, good in stability, good in durability, easy and rapid to operate, low in detection cost and accurate and reliable in detection result, and guarantees are provided for monitoring the quality stability and clinical medication safety of rebamipide.

The invention belongs to the technical field of detection of hydroxyl acrylate, and particularly discloses a detection device and method for processing hydroxyl acrylate, which have the advantages that the hydroxyl acrylate can be uniformly and effectively diluted, so that the phenomenon that a sample is not representative in the detection process is avoided, and the detection accuracy is improved. Meanwhile, the diluted sample is filtered when being detected, so that the chromatographic column is prevented from being blocked by insoluble impurities, and the detection accuracy and efficiency are improved.

The invention belongs to the technical field of chromatographic separation materials, and discloses a preparation method and application of a GM-8 nanosheet material. The preparation method of the material comprises the following steps: respectively dissolving Cu (NO3) 2.3 H2O and 1, 3, 6, 8-tetra (4-carboxybenzene) pyrene in an organic solvent, mixing, transferring into a reaction bottle, adding trifluoroacetic acid and pyridine, and uniformly mixing and stirring to obtain a reaction mixture; and heating the reaction mixture to react for 7-9 hours to obtain a blue precipitate, cooling the blue precipitate to room temperature, and washing and drying the blue precipitate to obtain the ultra-stable microporous GM-8 nanosheet material. The nanosheet GM-8 is used as a gas chromatography stationary phase, high-efficiency separation and trace detection of xylene isomers can be realized, and the chromatographic column still keeps excellent separation capacity after being stored in an environment with air humidity of 65-90% for 31 months. The capillary gas chromatographic column can realize high-efficiency separation of disubstituted benzene isomers such as xylene, the separation degree of m-xylene / p-xylene is up to 18.2, and a new solution is provided for high-efficiency separation of isomers with similar properties.

The invention discloses a compound monitoring method and system based on chromatographic column analysis and a medium, and relates to the technical field of chromatographic detection.The method comprises the steps that a complex matrix sample is taken, and first chromatographic column response distribution of the complex matrix sample is collected through a diode array detector; enhancement strategy optimization is carried out according to adjustable action parameters of the diode array detector, and the diode array detector collects second chromatographic column response distribution of the complex matrix sample under a first enhancement strategy; identifying a difference chromatographic column response distribution of the first chromatographic column response distribution and the second chromatographic column response distribution, and constructing a high-dimensional feature fusion fingerprint; and performing similarity measurement based on the high-dimensional feature fusion fingerprints and a pre-constructed compound feature fingerprint database to obtain a compound detection result. The technical problem of low detection accuracy caused by insufficient chromatographic response information of the compound under a complex matrix condition in the prior art is solved, and the technical effect of improving the detection accuracy of the compound is achieved.

The utility model provides automatic medium-pressure preparation and separation equipment and an automatic separation and preparation system. The automatic medium-pressure preparation and separation equipment comprises a workbench; the sample loading, liquid adding and needle cleaning module, the column packing module, the fraction collecting module, the carrying mechanism and the pump valve module are arranged on the workbench; the mobile phase cache module, the sample loading liquid adding and needle cleaning module which are arranged independent of the workbench are used for sucking sample liquid and cleaning a sample loading needle; chromatographic columns and / or sample loading columns are installed on the column loading module through a carrying mechanism, samples are separated, and the chromatographic columns and / or the sample loading columns of various specifications can be arranged in the column loading module; the fraction collection module is used for collecting fractions; the carrying mechanism is used for transferring materials on the sample loading, liquid adding and needle cleaning module, the column packing module and the fraction collecting module; the mobile phase cache module caches the required mobile phase; and the pump valve module is respectively communicated with the sample loading, liquid adding and needle cleaning module, the column packing module, the fraction collecting module and the mobile phase caching module and is used for providing power for liquid transmission among the modules. According to the invention, automation and unmanned operation of the whole process of medium-pressure preparation and separation are realized.

The invention provides a modular combined type column oven capable of rapidly replacing a chromatographic column, and relates to the technical field of column ovens. A ring frame is rotationally connected to the inner side face of the containing cylinder, a pushing motor is installed on the outer side face of the containing cylinder, a threaded rotating rod is installed on a motor shaft of the pushing motor, a supporting guide rod is welded to the inner side face of the containing cylinder, a pushing frame is slidably connected to the outer side face of the supporting guide rod, and a supporting plate is welded to the inner side face of the containing cylinder. A conversion motor is installed on the lower side face of the supporting plate, and a driving gear is installed on a motor shaft of the conversion motor. Through the arrangement of a driving gear, a ring frame, a threaded rotating rod and a push frame, automatic quick replacement work of different experimental chromatographic columns in the column oven is realized, and the situation that hands of experimenters are scalded when touching the column oven is avoided; the problem that according to a traditional column oven, an experimenter needs to frequently replace chromatographic columns of different experimental objects in the mode that the hands penetrate into a heating box body, and consequently the hands of the experimenter are scalded when touching a heat source is solved.

The invention discloses a quantitative detection method for tobacco components. The quantitative detection method comprises the following steps: extracting a tobacco sample to obtain extract liquor; performing component analysis on the extracting solution by adopting high-resolution liquid chromatography-mass spectrometry to obtain a spectrogram of the tobacco sample; the high-resolution liquid chromatography mass spectrometry adopts two ion sources of an ESI source and an APCI source for detection, and the two ion sources both adopt reversed-phase chromatographic columns for detection; in detection, under the ESI source condition, positive and negative ion modes are adopted for scanning respectively, and under the APCI source condition, a positive ion mode is adopted for scanning. According to the quantitative detection method, two different ion sources are adopted, and high coverage and detection precision are both considered; corresponding chromatographic columns are adopted for liquid phase separation, separation of tobacco metabolism components with different properties in a complex natural tobacco matrix is facilitated, and the separation efficiency and the coverage degree are improved; by combining the ultrahigh resolution and high precision of the high-resolution liquid chromatography-mass spectrometry, the to-be-detected substance and the interfering substance are effectively distinguished, and the detection accuracy of various samples is improved.

The invention discloses a primary separation method and system of a liquid chromatography system.The method comprises the steps that a sample is pretreated according to physicochemical properties of a target sample, and a high-purity enriched sample is obtained; optimizing the composition proportion of the mobile phase according to the composition characteristics of the high-purity enriched sample to obtain the optimized mobile phase composition; selecting an optimal chromatographic column type according to the optimized mobile phase composition, and carrying out dynamic temperature control separation through a dynamic temperature control technology to obtain a high-selectivity separation condition; performing real-time detection on the separated chromatographic peak according to a high-selectivity separation condition to obtain a high-signal-to-noise-ratio detection signal; and evaluating the preliminary separation effect according to the high signal-to-noise ratio detection signal. By utilizing the embodiment of the invention, the enrichment efficiency and the separation selectivity of the sample can be improved, and the accuracy and the reliability of integral separation are further improved.

The invention provides a method for analyzing and identifying chemical components of a calculus-eliminating prescription, which comprises the following steps: S1, preparing a test solution: performing ultrasonic treatment on a calculus-eliminating prescription extract by using methanol, centrifuging, taking supernate, diluting, filtering, and taking subsequent filtrate to obtain the test solution; s2, analyzing the test sample solution by adopting UHPLC-QE-MS (Ultra High Performance Liquid Chromatography-Quantitative Enhanced-Mass Spectrometry), wherein the detection conditions of the UHPLC-QE-MS are as follows: a chromatographic column is an octadecylsilane chemically bonded silica chromatographic column; the column temperature is 20-40 DEG C; the flow rate is 0.1 to 0.5 ml / min; the mobile phase A is 0.03-0.20% v / v formic acid aqueous solution, the mobile phase B is acetonitrile, gradient elution is carried out, and the gradient elution procedure is 0-1 min, 5% B-> 5% B; in 1-14 minutes, 5% B is changed into 60% B; and after 14-15 minutes, 60% B is converted into 95% B. The detection method disclosed by the invention can identify 68 compounds in the calculus eliminating sample at one time, and is rapid, simple, convenient, high in sensitivity and good in specificity.

The invention discloses a method for determining bedaquiline fumarate clean verification target residues, and relates to the technical field of instrument analysis of chemical pharmacy. The method comprises the following steps: preparing a sample wiping solution; determining the content of bedaquiline fumarate in the sample wiping solution by adopting a liquid chromatography; chromatographic conditions are as follows: a chromatographic column is a VP-ODS C18 column; mobile phases: a potassium hexafluorophosphate aqueous solution and acetonitrile, wherein the concentration of the potassium hexafluorophosphate aqueous solution is 0.01-0.03 mol / L; the elution mode is isocratic elution; the flow rate is 1 ml / min to 2 ml / min; the column temperature is 28-32 DEG C; the method has good specificity and sensitivity for determination of bedaquiline fumarate cleaning verification target residues, is simple and convenient to operate, rapid in determination, simple and easy to implement, and overcomes the defects that TOC, chemical titration methods, conductivity methods, pH methods and the like which are commonly used at present do not have specificity.