1070 results about "Chromatographic column" patented technology

The invention relates to the technical field of deep-sea microorganism nucleic acid detection, in particular to a long-term experimental platform for deep-sea microorganism in-situ nucleic acid detection and a detection method. According to the invention, a water sample is subjected to tangential flow filtration and concentration through the filtration and sampling module, so that a concentrated microorganism sample is obtained. The method comprises the following steps of: transferring a sample into an amplification detection module under reduced pressure, transferring into a lysis purification module for cell lysis, injecting the cracked sample into a chromatographic column, filtering impurities and intercepting DNA by the chromatographic column, then washing by using an eluent to obtain a high-purity DNA sample, loading a suction head through a transfer washing liquid gun, mixing the high-purity DNA sample with an enzyme solution, adding into the amplification detection module for reaction, and detecting the DNA in the amplification detection module. And carrying out fluorescence labeling on the amplified gene, obtaining an amplification curve by using a fluorescence detector, and detecting the in-situ nucleic acid of the deep-sea microorganisms according to the change of the amplification curve. An automatic cleaning assembly is designed in the filtering and sampling module, and the cracking and purifying module is used for sampling and cleaning a cracking chamber and switching pipelines, so that cross contamination caused by deep sea in-situ multiple detection is prevented.

The invention provides a content detection method for a salvia miltiorrhiza medicinal material, a salvia miltiorrhiza clear paste and a musk heart-dredging dropping pill. According to the method, a high performance liquid chromatography method is adopted, octadecylsilane chemically bonded silica is used as a chromatographic column filler, acetonitrile is used as a mobile phase A, 0.02%-0.1% trifluoroacetic acid is used as a mobile phase B, gradient elution is carried out, and rosmarinic acid and salvianolic acid B in the salvia miltiorrhiza medicinal material are synchronously and quantitatively detected. And synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid and salvianolic acid B in the salvia miltiorrhiza clear paste, and synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid, salvianolic acid B, arenobufagin and bufalin in the musk Tongxin dropping pill. The method is used for monitoring the content of specific components, can also judge the transfer rate in the medicine production process, and facilitates traceability in the production link. In addition, the method is relatively low in equipment requirement and suitable for industrial popularization.

The invention provides embedded metal fullerene and a preparation method thereof. The preparation method comprises the following steps: mixing a metal source and graphite powder, and filling a hollow graphite rod with the mixture to prepare an anode; the electrode is installed at the anode end of an electric arc furnace, and on-line activation is conducted through anode and cathode short-circuit current under the inert atmosphere; then carrying out arc discharge under specific air pressure and current, and collecting generated carbon ash; performing ultrasonic extraction by using an organic solvent to obtain a fullerene crude extracting solution; and finally, performing multi-stage separation and purification by high performance liquid chromatography, and performing primary and fine separation by sequentially adopting preparative and semi-preparative chromatographic columns to obtain a high-purity product. According to the method, a complete technical path capable of efficiently and controllably preparing the ultra-high-purity embedded metal fullerene is formed through a synthesis process integrating online activation and accurate atmosphere regulation and control and a multi-stage gradient chromatography purification strategy, and a solid foundation is laid for application of atomic-scale accurate materials in the frontier fields of quantum devices and the like.

The invention provides a therapeutic drug monitoring kit and method and system, a magnetic bead extraction method is combined with LC-MS / MS detection to be applied to human blood drug concentration monitoring, a mixed magnetic bead solution containing phospholipid removal magnetic beads and to-be-detected drug adsorption magnetic beads is utilized to perform adsorption and extraction pretreatment on a to-be-detected drug in a sample, automatic treatment equipment is matched, and the concentration of the to-be-detected drug in the to-be-detected drug in the to-be-detected drug in the to-be-detected drug in the to-be-detected drug in the to-be-detected drug in the to-be-detected drug is detected. The pretreatment efficiency is high, the phospholipid content in the supernate is low, and the matrix effect and the chromatographic column washing pressure are greatly reduced. According to the therapeutic drug monitoring method provided by the invention, a unified pretreatment process is used, simultaneous extraction of multiple drugs is realized, and through a magnetic bead automatic extraction method, the pretreatment step of a sample can be rapidly completed, a therapeutic drug monitoring result can be rapidly obtained, the overall detection time is shortened, and the detection efficiency is improved. Therefore, a reliable laboratory examination basis is provided for individualized treatment.

The invention belongs to the technical field of traditional Chinese medicine detection, and discloses a detection method for a characteristic spectrum of Uighur medicine Kspecific heat extracting tablets and application of the detection method. The detection method provided by the invention comprises the following steps: preparing a test sample solution by taking a 75% methanol solution as a solvent, and determining the test sample solutions prepared from different batches of test samples by adopting ultra-high performance liquid chromatography to obtain a characteristic spectrum; the chromatographic conditions of the ultra-high performance liquid chromatography are as follows: a chromatographic column is a C18 chromatographic column, a mobile phase A is acetonitrile, a mobile phase B is a 0.1 vol% phosphoric acid solution, and the flow velocity is 0.25-0.35 mL / min; the detection wavelength is 0 to 18 minutes, and the wavelength is 327 nm; the time is 18 to 28.5 min, and the wavelength is 254 nm; when the time is 28.5 to 37.6 minutes, the wavelength is 242 nm; after 37.6 to 70 minutes, the wavelength is 210 nm; the sample size is 1 microliter, the column temperature is 20-40 DEG C, and gradient elution is carried out. The invention provides a more scientific identification and quality control method for the Kespecific heat tablets.

The invention belongs to the technical field of pharmaceutical analysis, and relates to a method for detecting the content of povidone K30. According to the method, the content of povidone K30 in the medicinal preparation is detected by adopting a high performance liquid chromatography; detection conditions of the high performance liquid chromatography are as follows: a chromatographic column is a C18-AQ column; a mobile phase is a phosphate solution. The method has the characteristics of high accuracy, strong specificity and the like for detecting the content of povidone K30 in the pharmaceutical preparation, can overcome the interference of other auxiliary materials in the pharmaceutical preparation, and has important application value in development and consistency evaluation of the pharmaceutical preparation.

The invention relates to the field of pharmaceutical analytical chemistry, in particular to a method for determining tandospirone and salt intermediates thereof, high performance liquid chromatography is adopted, and chromatographic conditions include that a chromatographic column with octadecylsilane chemically bonded silica as a filler is adopted, and gradient elution is performed by a mobile phase A and a mobile phase B; wherein the mobile phase A consists of a first water phase and acetonitrile; the mobile phase B is composed of a second water phase and acetonitrile; the first water phase is a water solution containing monopotassium phosphate and sodium hexanesulfonate, and the pH value of the first water phase is 3.0-3.8; the second water phase is an aqueous solution containing monopotassium phosphate and sodium hexanesulfonate, and the pH value of the second water phase is 1.8-2.6. The testing method disclosed by the invention has good specificity, accuracy and repeatability, and can be used for monitoring the quality of the tandospirone raw material medicine.

The invention discloses a construction method of a gout compound decoction fingerprint as well as the fingerprint and application thereof, and belongs to the technical field of analysis and detection. The construction method of the fingerprint spectrum comprises the following steps: taking a test solution prepared from the gout compound decoction; the test solution is subjected to HPLC-SPD detection, so that the fingerprint spectrum of the gout compound decoction is obtained, and the HPLC detection conditions are that a C18 chromatographic column is used, a C18 chromatographic column is used, a C18 chromatographic column is used, a C18 chromatographic column is used, and a C18 chromatographic column is used for detecting the fingerprint spectrum of the gout compound decoction. An aqueous solution containing 0.1%-0.2% of phosphoric acid is used as a mobile phase A, and acetonitrile is used as a mobile phase B for gradient elution; the flow velocity is 0.8-1 mL / min, the column temperature is 25 DEG C, the sample injection volume is 5-10 [mu] L, and a diode array detector is 190-400 nm full-wave band scanning. The chemical components in the gout compound decoction are comprehensively and systematically analyzed, and a basis is provided for quality control and in-depth study of a pharmacodynamic material basis.

The invention relates to the technical field of agricultural product detection, in particular to an agricultural product pesticide residue detection method and system. According to the method, the spatial orientation characteristics of molecular three-dimensional conformation parameters are introduced, a symmetry index set is established, matching calculation is carried out in combination with temperature distribution in chromatographic column operation parameters and the sample injection direction, accurate linkage of structural information and a chromatographic path is achieved, and through coupling analysis of response starting time and chromatographic regulation and control parameters, the accuracy of the chromatographic regulation and control parameters is improved. A detection time window taking a target protein signal as a reference is set, a response enhancement fragment with a significant rising rate is screened out in combination with a signal change trend in the window, and a target signal interval is obtained through weighted fitting, so that the specificity and pertinence of detection data are effectively improved, and the detection accuracy is improved through comparison of peak position time and response data. According to the scheme, accurate labeling of pesticide types in a complex sample is achieved, and the method has high stability and judgment accuracy under the scene that the sample heterogeneity is high and signal interference is complex.

The invention discloses a method for detecting melogabalin besylate and isomer impurities of melogabalin besylate. According to the method, liquid chromatography is adopted, an FXAA reagent and a sample to be tested are subjected to a reaction under the alkaline condition to obtain a solution to be detected, then the solution to be detected is subjected to liquid chromatography separation, the structural formula of the FXAA reagent is # imgabs0 #, R is selected from-CH (CH3) 2,-CH2CH2SCH3 or-C6H5, and the structural formula of the FXAA reagent is as shown in the specification, the structural formula of the FXAA reagent is as shown in the specification, and the structural formula of the FXAA reagent is as shown in the specification, the structural formula of the FXAA reagent is as shown in the specification, the structural formula of the FXAA reagent is as shown in the specification, and the structural formula of the FXAA reagent is as shown in the specification. The test sample comprises melogabalin besylate and isomer impurities thereof, and the liquid chromatography adopts a reversed-phase chromatographic column. According to the method, melogabalin besylate and three isomer impurities thereof can be safely and effectively separated and respectively detected, the detection sensitivity, repeatability and durability are good, and a powerful guarantee is provided for quality control of the medicine.

The invention relates to a method for detecting the content of amino acid in a pesticide through pre-column derivatization liquid chromatography, and relates to the technical field of chemical analys.The method comprises the steps that a pesticide sample to be detected is extracted, and a solution containing amino acid is obtained; then, under the optimized alkaline pH and heating conditions, 4-fluoro-7-nitro-2, 1, 3-benzoxadiazole (NBD-F) is adopted as a derivatization reagent to be subjected to a pre-column derivatization reaction with amino acid, and a stable high-fluorescence NBD-F derivative is formed; injecting the derivative liquid into a high performance liquid chromatography system provided with a phenyl bonded phase chromatographic column, and efficiently separating the NBD-F derivative by utilizing pi-pi interaction and hydrophobic interaction of the phenyl column; and finally, detecting and quantifying through a fluorescence detector. Through the synergistic effect of NBD-F derivation and the phenyl column, the separation selectivity and the detection sensitivity are remarkably improved, and the reaction efficiency and the derivative stability are guaranteed through optimized derivation conditions.

The invention provides a method for detecting free amino acids in camellia oleosa seed oil, and establishes a method for detecting the free amino acids in the camellia oleosa seed oil based on ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS), which comprises the following steps: pre-treating various amino acids in the camellia oleosa seed oil by using a non-derivation method; the problems of complicated operation, impurity interference and the like caused by derivatization are avoided, the extraction solvent is environment-friendly and economical, the extraction efficiency is high, and the pretreatment time is greatly shortened; then selecting a proper chromatographic column and a mobile phase, separating a plurality of free amino acids under the condition of not introducing excessive derivatization agents and ion pair reagents, and controlling the collection time to be 12 minutes. The method for detecting the free amino acids in the camellia oleosa seed oil has the characteristics of no need of derivatization treatment, simplicity and convenience in operation, high detection efficiency and good sensitivity and accuracy, and can effectively separate and detect 14 free amino acids such as alanine, phenylalanine and aspartic acid in the camellia oleosa seed oil.

The invention relates to the field of polymer grading, and discloses a polyethylene grading method, polyethylene obtained through the polyethylene grading method, a system for polyethylene grading and application of the system. According to the polyethylene grading method, on the basis of preparing a high-temperature liquid chromatographic column, two-time flow division is adopted, and the flow ratio of second flow division is controlled, so that accurate and directional grading of a polyethylene raw material is realized, and the purposes of accurate and directional regulation and control of the average molecular weight, the molecular weight distribution curve and the branched structure of polyethylene, especially low-density polyethylene, are realized.

The invention relates to a precise separation and online detection integrated system for a multi-component complex system, and belongs to the technical field of analysis and detection. The system comprises an intelligent preprocessing and component sensing unit, a self-adaptive precise separation unit, a multi-modal cooperative detection unit, a zero dead volume-intelligent adaptive interface unit and a multi-algorithm fusion intelligent control and data analysis unit, and the five units form a closed-loop cooperative architecture through real-time data interaction. The system adopts a preprocessing-sensing integrated design, a multi-mode switching type separation architecture, a dynamic intelligent chromatographic column, a four-channel collaborative detection system and multi-algorithm fusion regulation. According to the invention, the problems of separation and detection disjunction, narrow adaptability, weak matrix interference suppression capability, low intelligent degree, poor portability and the like in the prior art are effectively solved, and one-time sample injection accurate separation and high-accuracy detection of trace target components with wide polarity range and similar structures can be realized.

The invention provides a method for detecting a genotoxic impurity TG707 in a macassavir raw material medicine and an intermediate TG7, and relates to the technical field of medicine detection, and the method comprises the step of detecting the genotoxic impurity TG707 in the macassavir raw material medicine or the intermediate TG7 sample by adopting a high performance liquid chromatography and mass spectrometry combined method, the mobile phase A is an ammonium acetate solution, and the mobile phase B is methanol. By adopting a liquid chromatography-mass spectrometry method and utilizing the selectivity of mass spectrum multi-channel monitoring, main components and impurities enter mass spectrum at the same time, the interference of high-concentration main components on the mass spectrum detection sensitivity is avoided, good separation on the mass spectrum is realized, and the sensitivity is relatively high; an ammonium acetate solution and methanol are used as mobile phases, so that the peak pattern and sensitivity of TG707 are ensured. The technical problems that in the prior art, the peak of TG707 on a liquid phase is between two peaks of a main component TG7, and baseline separation is difficult to achieve by replacing a chromatographic column and optimizing the fluidity gradient are solved.

The invention belongs to the technical field of detection methods, and particularly relates to a liquid chromatography detection method for an idedecalciferol intermediate and impurities thereof. According to the liquid chromatography detection method for the eldecalciferol intermediate and the impurities thereof, a liquid chromatography method is combined with an electrospray detector for detection; chromatographic conditions are as follows: an amylose-tri (3-chlorphenyl carbamate) covalently bonded silica gel chromatographic column is adopted; and carrying out gradient elution by taking water as a mobile phase A and acetonitrile as a mobile phase B. The method for detecting the eldecalciferol intermediate and the impurities of the eldecalciferol intermediate is good in specificity, high in sensitivity and accuracy, good in repeatability and stability and high in analysis speed, the content of the eldecalciferol intermediate and the impurities of the eldecalciferol intermediate can be rapidly and accurately detected, and the blank of detection of the eldecalciferol intermediate and the impurities of the eldecalciferol intermediate in the prior art is filled.

The invention discloses a CAD detection method for phosphoric acid and phosphorous acid in an alendronate sodium oral solution, and belongs to the technical field of pharmaceutical analysis. The method comprises the following steps: preparing a reference stock solution and a test solution; then setting high performance liquid chromatography detection conditions; a Shodex VN-504D chromatographic column is adopted, a CAD detector is adopted as a detector, a mixed solution of a mobile phase A and a mobile phase B is adopted as a mobile phase, the mobile phase A is ammonium formate, the mobile phase B is an acetonitrile solution, and gradient elution is performed by adopting the mobile phase; and respectively measuring the reference stock solution and the test solution, injecting into a liquid chromatograph, and recording a chromatogram. A CAD detector is adopted, the detection sensitivity is obviously improved, the quantitative concentration can reach 0.24 mu g / mL, and the detection concentration can reach 0.10 mu g / mL. The method is high in specificity, high in sensitivity, good in durability, rapid, simple, effective and reliable.

The invention provides a specific chromatogram construction method and application of polygonum-folium isatidis formula granules. The specific chromatogram construction method comprises the following steps: acquiring a specific chromatogram of a to-be-detected substance by adopting a high performance liquid chromatography; the specific chromatographic conditions of the high performance liquid chromatography are provided, octadecylsilane chemically bonded silica is used as a chromatographic column of a filler, the detection wavelength is 305-315 nm, acetonitrile is used as a mobile phase A, a 0.04%-0.06% phosphoric acid aqueous solution is used as a mobile phase B, and elution is carried out according to a specific gradient program. The specificity of the material information corresponding to the characteristic peak in the characteristic spectrum obtained by the construction method is stronger, the related information in the characteristic spectrum represented by the method is more comprehensive, and the overall quality control of the polygonum-folium isatidis can be better realized.

The utility model discloses a system for step-by-step separation and conversion of tar residues, which comprises an ultrasonic cleaning instrument, the liquid outlet end of the ultrasonic cleaning instrument is connected with a solid-liquid separator through a pipeline, the liquid outlet end of an upper liquid layer of the solid-liquid separator is connected with a delivery pump I through a pipeline, and the delivery pump I is connected with the liquid inlet end of a rotary evaporator I through a pipeline. Concentrated organic matters in the rotary evaporator I are conveyed into a vertically arranged chromatographic column through a pipeline, the lower end of the chromatographic column is connected with a sand core funnel, a collecting tank is placed below an outlet of the sand core funnel, the collecting tank is connected with a conveying pump V through a pipeline, and the conveying pump V is connected with a liquid inlet end of the rotary evaporator II through a pipeline. According to the method, high additional organic matters in the tar residues can be effectively extracted by adopting a mode of synergism of ultrasonic-assisted extraction and column chromatography separation, so that resource utilization of the tar residues is realized. The solvent and the eluent selected in the whole process can be recycled through a rotary evaporator, the operation cost is low, and near-zero emission can be realized.

The invention provides a high performance liquid chromatography detection method of a monocrystalline silicon wafer cutting fluid. The monocrystalline silicon wafer cutting fluid is subjected to high performance liquid chromatography detection so as to quantitatively determine components of the monocrystalline silicon wafer cutting fluid. A chromatographic column is Poroshell 120EC-C18, a mobile phase is prepared from acetonitrile and water according to a volume ratio of (68-72): (28-32), the flow velocity of the mobile phase is 0.5-1.0 mL / min, the detection wavelengths are 205-215 nm and 236-240 nm, the column temperature of the chromatographic column is 30-40 DEG C, the sample injection volume is 20-30 [mu] L, and a detector is a DAD detector; the monocrystalline silicon wafer cutting fluid comprises a dispersing agent, a wetting agent and a solvent; the dispersing agent is EO / PO block polyether; the wetting agent is selected from at least one of polyether modified organic silicon and polyethylene glycol; the solvent is water. The problems that in the prior art, the component analysis cost of the cutting fluid is high, and the requirement for operators is high are solved.

The invention discloses a synthesis method of a novel benzosuberone compound, and belongs to the field of organic synthesis. The preparation method comprises the following steps: uniformly stirring methyltriphenylphosphonium bromide in a solvent at room temperature, dropwise adding an n-hexane solution of n-butyllithium in an ice-water bath, stirring a reaction system at room temperature for 30-40 minutes after dropwise adding is completed, then adding an initial raw material phenanthrenequinone 1 in the ice-water bath, transferring the reaction system to 40 DEG C for reaction, and after the reaction is monitored to be complete by a TLC (Thin Layer Chromatography) dot plate, filtering, washing and drying to obtain the phenanthrenequinone 1. And pouring the reaction liquid into a silica gel chromatographic column, and simply filtering by using dichloromethane as an eluent to remove salt and phosphine oxide. And performing rotary evaporation to remove the organic solvent to obtain a crude product, and separating and purifying to obtain a target product 2. The method is short in reaction time and low in reaction cost, provides a practical method for obtaining the seven-membered rigid ring skeleton, and has potential value for synthesis of natural products and bioactive molecules.

The invention relates to the technical field of food safety detection, in particular to a method for detecting urea in bean sprouts and application thereof.The method comprises the following steps that smashed bean sprouts are subjected to two times of ultrasonic extraction and centrifugation, supernate is combined, and an extracting solution is obtained; fixing the volume and filtering to obtain a to-be-detected solution; detecting the liquid to be detected by using liquid chromatography-tandem mass spectrometry; an extraction solvent for ultrasonic extraction is a 5% formic acid-acetonitrile composite solution; the conditions of the liquid chromatography-tandem mass spectrometry are as follows: the chromatographic conditions are as follows: a chromatographic column is an HILIC column; the sample size is 10 [mu] L; a mobile phase is a mixed solution of a 0.02 mmol / L ammonium acetate buffer salt solution and acetonitrile, and isocratic elution is carried out; the flow rate is 0.3 mL / min; the column temperature is 40 DEG C; mass spectrum conditions are as follows: an electrospray ionization (ESI) positive ion mode, electrospray voltage of 4000 V, sheath gas pressure of 30 psi, auxiliary gas pressure of 5 psi, capillary heating temperature of 300 DEG C and scanning mode of MRM. The method disclosed by the invention is free from substance interference, high in sensitivity, accurate in result, low in cost and high in efficiency, and can be used as a standard detection method.

A catalyst for an acylation reaction, and a preparation method therefor and the use thereof. The preparation method for the catalyst for an acylation reaction comprises the following steps: (1) adding a cation exchange resin to a 0.1-10 mol / L hydrochloric acid solution, performing an ultrasonic treatment for 1-60 min followed by filtration, washing same with water until the filtrate is neutral, and filtering same; and (2) adding the cation exchange resin, which is obtained after the treatment in step (1), to a chromatographic column, adding a 0.01-5 mol / L Lewis acid solution for leaching, filtering same, then washing same with water, and drying same to obtain a catalyst for an acylation reaction. The catalyst for an acylation reaction can efficiently achieve an acylation catalytic reaction of a naphthalene-containing compound and has a good catalytic effect, and the post-treatment is simple.

The invention belongs to the technical field of water treatment brine reuse, and provides an electrochemistry-based brine calcium and magnesium graded extraction process, which comprises the following steps: brine enters a primary electrolysis device for electrochemical reaction, carbon dioxide is introduced, and calcium ions in the brine are precipitated; further entering a primary precipitation separation device, and intercepting and collecting precipitated calcium; then the brine enters a secondary electrolysis device, the density of current applied to an electrode is increased, and magnesium ions in the brine are precipitated; the solution enters a secondary precipitation separation device, and precipitated magnesium is intercepted and recycled; drying the separated calcium and magnesium precipitates to obtain a product; and finally, introducing the reacted effluent into an ion exchange resin chromatographic column to remove untreated calcium and magnesium ions, and applying the obtained hardness-free alkaline water to the hydrogen production industry. By regulating the current density and introducing CO2, calcium and magnesium in various kinds of saline water are respectively precipitated and extracted, and the device is suitable for salt-containing organic wastewater, seawater, seawater desalination concentrated solution, bitter brine and industrial circulating cooling water.

The utility model provides a full-automatic multifunctional pilot platform system and a chromatographic system thereof. The platform system comprises a first input main pipeline with a first input pump and a second input main pipeline with a second input pump, the first input main pipeline is connected with a plurality of input pipelines, and on-off of the first input main pipeline is controlled through corresponding valves; the second input main pipeline is also respectively connected with the plurality of input pipelines, and the on-off of the second input main pipeline is controlled through corresponding valves; the outlet ends of the input pipelines are connected with liquid inlet ports of the corresponding movable installation modules respectively, and the movable installation modules are further provided with a plurality of backflow ports and a plurality of liquid outlet ports. The liquid outlet port is respectively connected with a plurality of collecting pipelines through output pipelines; according to the chromatographic system, an RTF column is mounted in a movable mounting module; during use, two tangential flow chromatographic columns are adopted and operate alternately: one is in a loading mode, and the other is in an elution mode; the multi-functional biological treatment device has the advantages that modularization is achieved, multiple functions are achieved according to different process requirements, and the downstream production process of biological medicine is met.

The invention discloses a method for simultaneously detecting 37 phenolic substances in a plant based on HPLC (High Performance Liquid Chromatography). HPLC-PDA (Personal Digital Assistant) is adopted for separation and detection; the detection conditions are as follows: the chromatographic column is a PFP chromatographic column; the detection wavelengths are 280 nm, 330 nm and 360 nm; the flow velocity is 0.5 to 0.8 mL / min; the sample size is 8-12 [mu] L; the column temperature is 28-32 DEG C; the mobile phase A is an aqueous solution containing 0.3% by mass of formic acid, and the mobile phase B is methanol; the elution gradient is 0-10 min, and the elution gradient is 5-10% B; in 10-16 min, 10%-25% of B is obtained; after 16 to 25 minutes, 25 to 40 percent of B is obtained; 25 to 50 minutes, 40 to 60 percent of B is adopted; and 60-67% of B is carried out in 50-55 min. The method is suitable for plant sample detection, is especially suitable for sea-buckthorn sample detection, can be applied to multiple fields of food analysis, plant research, component development and the like, and has wide application value.

The invention belongs to the technical field of medicine detection, and particularly relates to a method for detecting a nitroso compound in a raw material medicine in a riptacaine emulsifiable paste, which comprises the following steps: preparing a test sample: taking the riptacaine emulsifiable paste, adding a 5mol / L sodium hydroxide solution, uniformly mixing, then adding a 5mol / L hydrochloric acid solution, and uniformly mixing; diluting with a solvent with the pH value of 7.20 + / -0.02, and then centrifugally filtering to obtain a test sample; wherein the solvent is a mixed solvent composed of monopotassium phosphate and acetonitrile; liquid chromatography separation: the tested sample is separated by liquid chromatography, and a mobile phase A is a 0.2% formic acid solution; the mobile phase B is methanol; the chromatographic column is SB-C18, 2.1 * 100 mm, 1.7 [mu] m; and mass spectrum detection: detecting the substance separated by the liquid chromatography by using a mass spectrometer to obtain the content of the nitroso compound. The detection method is efficient, sensitive and excellent in reproducibility.

The invention discloses an analysis method for determining multiple components of white spirit by high performance liquid chromatography-tandem mass spectrometry, and relates to the technical field of white spirit analysis and detection, and the analysis method comprises the following steps: firstly, preparing an ethyl carbamate precursor substance standard stock solution and a mixed standard intermediate solution, and diluting the mixed standard intermediate solution step by step to obtain a mixed standard working solution; then determining chromatographic and mass spectrometry conditions, wherein BEH Ami chromatographic column is adopted as the chromatographic condition, and 0.1% formic acid water-acetonitrile is adopted as a mobile phase for gradient elution; a mass spectrum condition adopts a multi-reaction monitoring mode under an electrospray positive ion mode; drawing a quantitative calibration curve; finally, preparing a to-be-detected sample for content determination. According to the analysis method for determining the multiple components of the Baijiu through the high performance liquid chromatography-tandem mass spectrometry, through chromatographic condition optimization and mass spectrometry parameter innovation, the detection efficiency is improved, peak area data of urea, citrulline and arginine can be synchronously obtained through single sample injection, the analysis time is short, and quantification is accurate.

The invention mainly relates to a method for determining related substances of doxofylline injection, using high performance liquid chromatography, using octadecylsilane bonded silica gel as a filler; mobile phase A is a phosphoric acid aqueous solution with a pH of 1.5-3.5, and mobile phase B is acetonitrile, and gradient elution is performed. The detection method can completely separate impurities 1-9 in doxofylline injection, with a separation degree greater than 1.5, good system applicability, and the method has high specificity, accuracy and reproducibility, etc., is easy to operate, has no damage to the chromatographic column, and can be used for analysis, detection and quality control of doxofylline injection in industrial production.

The invention discloses a method for detecting the content of effective components in a nerofloxacin malate capsule, and relates to the technical field of medicine detection and analysis, and the detection method comprises the following step: detecting the content of the effective components in the nerofloxacin malate capsule by adopting a high performance liquid chromatography. The invention provides the method for detecting the content of the effective components in the nerofloxacin malic acid capsule for the first time, and the inventor finds that the interference of non-effective components such as impurities and auxiliary materials in the nerofloxacin malic acid capsule can be effectively avoided by selecting a specific chromatographic column and a specific mobile phase for isocratic elution; the accuracy of detecting the content of the effective components in the nerofloxacin malic acid capsule is improved, the accurate quantification of the content of the nerofloxacin malic acid capsule is realized, and the blank in the prior art is filled.