62 results about "Capillary column" patented technology

The invention provides a capillary electrophoresis analysis method of serum amino acid. The capillary electrophoresis analysis method comprises the following steps: S1, preparing an operation buffer solution; s2, selection and pretreatment of a quartz capillary column; s3, conditions are analyzed through electrophoresis; s4, drawing a quasi curve; s5, sample derivatization; s6, quantitative analysis. According to the method, a mixed reagent of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin is adopted for the first time, the amino acid migration behavior is cooperatively adjusted, a migration time window is expanded, the separation resolution of amino acids with similar structures is effectively improved, and the separation degree and the atlas definition are remarkably improved. According to the invention, sodium taurocholate is added, pH is regulated and controlled, a weakly alkaline buffer system with moderate conductivity and stable migration behavior is formed, separation and detection of FITC derived amino acids are facilitated, and balance of migration time distribution is optimized. The method is suitable for scenes of clinical sample analysis, disease marker screening and the like, and has good universality, stability and popularization value.

According to the method for detecting the content of the volatile substances in the aquilaria sinensis, provided by the invention, through pretreatment steps such as extraction of an extraction solvent, heating reflux and filtration, a sample is selectively and preliminarily purified, and the matrix effect of subsequent detection and analysis is effectively reduced; an inert capillary column is used for separation, high-purity helium is used as carrier gas, and an optimized heating program and an MRM detection mode are combined; through the synergistic effect of the two components, comprehensive, accurate and high-repeatability qualitative and quantitative analysis of various volatile substances in the aquilaria sinensis, especially nookatone which is easy to leak in a conventional method, is realized, and a reliable technical means is provided for accurate identification and quality evaluation of the aquilaria sinensis.

The present application relates to a controllable preparation method of a colloidal crystal capillary column and its application in biomolecule separation, and specifically comprises the following steps: a plunger and an electroosmotic pump are prepared in situ at one end of a capillary; a buffer solution containing monodisperse colloidal particles is filled in an upper reservoir of an electric field assembly device, and a buffer solution is filled in a lower reservoir; the capillary is filled with the buffer solution, and the end of the capillary containing the electroosmotic pump is inserted into the lower reservoir; the dispersion of the colloidal solution is maintained by applying oscillation to the upper reservoir, an electric field is applied between the two reservoirs to make the colloidal particles move to the electroosmotic pump under the action of an electroosmotic flow, and a three-dimensional colloidal crystal is assembled; and the capillary is supplemented with an ultrasonic force to reduce lattice defects. The present application has the advantages of simple preparation process, controlled directional movement of colloidal particles through an electric field, improved assembly efficiency and quality of the three-dimensional colloidal crystal, and controllable assembly of the colloidal particles under the action of an electric field through regulation and control of the length and surface charge of the electroosmotic pump.

This invention discloses a two-phase liquid-cooled heat dissipation device, comprising a heat absorption module, a heat dissipation module, a delivery pipe section, and a return pipe section. The heat absorption module, delivery pipe section, heat dissipation module, and return pipe section are sequentially connected end-to-end to form a closed-loop cavity. A cooling chamber is provided outside the closed-loop cavity within the heat dissipation module, and the heat dissipation module is provided with a cooling connector. A capillary column is provided inside the closed-loop cavity within the heat absorption module. One end face of the capillary column has a first channel recessed therein, and the other end face of the capillary column has a second channel recessed therein. The opening of the first channel faces the return pipe section, and the opening of the second channel faces the delivery pipe section. The distance between the first channel and the inner wall of the closed-loop cavity is greater than the distance between the second channel and the inner wall of the closed-loop cavity. Liquid returns into the capillary column, and through the unidirectional vapor-liquid action of the capillary column, the working fluid flows unidirectionally within the closed-loop cavity, avoiding mutual disturbance between the vapor and the return liquid, improving the flow efficiency of the working fluid, and enhancing the heat dissipation capacity of the device.

The invention belongs to the technical field of gas chromatography detection, and relates to a gas chromatography method for simultaneously determining the content of ethanol and isopropyl myristate. The set conditions of the gas chromatography are as follows: the temperature of an FID detector and a polyethylene glycol 20M capillary column is 240-260 DEG C, the temperature of the detector is 240-260 DEG C, the carrier gas is nitrogen, the flow rate is 0.9-2.5 mL / min, the sample injection amount is 1 mu L, the column temperature is increased by adopting a program, the initial temperature is 80-90 DEG C, the temperature is increased to 180-190 DEG C at the rate of 9-12 DEG C / min, and the temperature is maintained for at least 10 minutes. The method provided by the invention can realize simultaneous detection of ethanol and isopropyl myristate, after the two substances are dissolved by the N, N-dimethylformamide solvent, the detected spectrogram does not have the phenomena of peak overlapping, trailing and the like, and the method has the advantages of high separation efficiency, high selectivity, high sensitivity, high analysis speed and wide application range.

Some embodiments described herein relate to capillary-containing cartridges suitable for use with capillary electrophoresis instruments. Embodiments described herein generally relate to cartridges that include a transfer capillary coupled to a separation capillary. The transfer capillary can be configured to be disposed in sample reservoirs and / or buffer reservoirs. Suction applied through a sheath interface of the transfer capillary and the separation capillary can draw sample / buffer from such reservoirs and bring the sample / buffer into contact with the separation capillary. The separation capillary can be configured for separation of analytes contained within the sample, for example when an electric potential (i.e., voltage) is applied across the separation capillary.

The invention belongs to the technical field of analysis and detection, and particularly relates to a sulfur hexafluoride isotope abundance detection method. The sulfur hexafluoride isotope abundance detection method provided by the invention comprises the following steps: detecting a to-be-detected sample by using a gas chromatograph-mass spectrometer to obtain a total ion flow chromatogram of sulfur hexafluoride; the gas chromatography test conditions are as follows: a DB-5MS capillary column is adopted, the split ratio is (20-80): 1, and the sample size is 1-10 L; the mass spectrum test conditions comprise that the voltage of a multiplier is + 300 to + 600, and the half-peak width is less than 0.6; and carrying out < 32 > SF < 5 + >, < 33 > SF < 5 + > and < 34 > SF < 5 + > ion extraction on the total ion chromatogram of sulfur hexafluoride to respectively obtain the peak area of < 32 > SF < 5 + >, the peak area of < 33 > SF < 5 + > and the peak area of < 34 > SF < 5 + >, and calculating the abundance of < 32 > SF < 5 + >, the abundance of < 33 > SF < 5 + > and the abundance of < 34 > SF < 5 + >. The detection method provided by the invention has the advantages of economical efficiency, high analysis speed and high accuracy.

The invention relates to the field of analytical chemistry, and particularly discloses a method for determining residual solvents N, N-dimethylformamide, dichloromethane, isopropanol, ethyl acetate, methyl tert-butyl ether, ethanol, acetone, tetrahydrofuran and ethylene glycol dimethyl ether in a litamilast raw material by adopting a headspace-gas chromatography method, and a method for determining residual solvents N, N-dimethylformamide, dichloromethane, isopropanol, ethyl acetate, methyl tert-butyl ether, ethanol, acetone, tetrahydrofuran and ethylene glycol dimethyl ether in a litamilast raw material by adopting a headspace-gas chromatography method. The method comprises the following steps of: detecting by using a capillary column with 6 percent of cyanopropyl phenyl-94 percent of dimethyl polysiloxane as a stationary liquid through headspace sample introduction gas chromatography and a flame ionization detector (FID). According to the method disclosed by the invention, nine residual solvents contained in the litamilast raw material can be completely separated in one system, the separation degree is greater than 1.5, the specificity is good, interference from blank solvents and other unknown impurities is avoided, the sensitivity is high, the detection accuracy is high, and the quality of litamilast can be effectively controlled.

The invention discloses a GM806 gas chromatograph system and an operation method, and the system comprises a sample introduction module which is used for collecting a target sample through an automatic sample introduction device and selecting a separation column for accurate sample introduction; the separation module is used for performing component separation on the target sample through a separation column; the detection module is used for detecting the separated sample components, acquiring detection data and calibrating and checking the detection data; and the analysis module is used for analyzing the calibrated and checked detection data and generating an analysis report of the target sample according to an analysis result. The high-efficiency capillary column is used, an optimized temperature control program is combined to realize high-efficiency separation of a complex sample, the separation efficiency and the separation effect are improved, meanwhile, low-concentration component detection is realized by setting the sensitivity of a detector, and reliable detection of all components of a target sample can be comprehensively realized; and the detection efficiency, comprehensiveness, practicability and stability are improved.

The invention provides a method for detecting methyl lactate in a sodium lactate solution, a gas chromatography is combined with a headspace sampling technology, and chromatographic conditions are as follows: a chromatographic column is a capillary column taking polyethylene glycol or a compound with similar polarity as a stationary liquid; a sample inlet is 180 DEG C, and headspace sample injection is performed; a flame ionization detector is adopted, and the temperature is 230 DEG C; the carrier gas is nitrogen, the flow velocity is 2.0 ml / min, and the split ratio is 10: 1; the column temperature program is as follows: 35 DEG C is maintained for 3 minutes, the temperature is raised to 90 DEG C at 5 DEG C / min and maintained for 3 minutes, and then the temperature is raised to 200 DEG C at 15 DEG C / min and maintained Headspace conditions are as follows: the balance temperature of a headspace bottle is 90 DEG C, and the time is 30 minutes; a quantitative loop is 100 DEG C; the temperature of the transmission line is 110 DEG C; the circulation time is 40 minutes. The method can accurately and quantitatively detect methyl lactate, is convenient to operate, and has great significance in improving the quality control level of the sodium lactate solution, guaranteeing the application safety of the sodium lactate solution in the fields of medicines and foods and perfecting a quality standard system.

The utility model provides a multifunctional integrated chromatographic analysis device. The multifunctional integrated chromatographic analysis device comprises a sample injection unit, a chromatographic analysis unit and a control unit, wherein the sample injection unit is used for sample injection of probe molecules; the separation unit comprises a capillary column and a temperature control box, and the input end of the capillary column is connected with the output end of the sample introduction unit through a first switching valve; the testing unit comprises a three-way valve, a plurality of sample columns and at least one reference column; the carrier gas unit comprises a carrier gas pipeline and a carrier gas interface, one end of the carrier gas pipeline is connected with the carrier gas interface, and the other end is connected with the output end of the capillary column; the detection unit comprises a first detector and a second detector which are respectively connected with the sample outlet ends of the sample column and the reference column. The analysis device disclosed by the utility model is convenient, simple and efficient to use, can be used for gas chromatography and multi-channel surface energy analysis, and can integrate multi-probe separation and multi-channel surface energy analysis, so that the use flexibility of the analysis device is greatly improved, the test range is expanded, the test process is greatly shortened, and the test efficiency is improved.

Capillary tube assemblies and methods of construction and use are disclosed, including a capillary tube assembly comprising a capillary tube, a plunger, and a grip. The capillary tube has first and second tube ends, a bore, and a longitudinal axis extending between the first and second tube ends. The plunger has a first plunger portion disposed within the bore and a second plunger portion disposed outside of the bore. The plunger is slidably disposed within the bore to be selectively moved toward the first tube end along the longitudinal axis. The grip has first and second grip ends, an opening extending between the first and second grip ends, and a recess in fluid communication with the opening and engaging the second tube end to connect the capillary tube to the grip. The recess has a channel extending between the recess and the second grip end forming a vent.

The invention relates to the technical field of analysis and detection, in particular to a gas chromatography-mass spectrometry detection method for N-methylaniline. The gas chromatography-mass spectrometry detection method for N-methylaniline comprises the following steps: treating a sample to be neutral, and extracting N-methylaniline in the sample by using dichloromethane to obtain a liquid to be detected; aa, separating the to-be-detected liquid through a quartz capillary column, and carrying out gas chromatography-mass spectrometry detection; the conditions of the gas chromatography are as follows: the temperature of a sample inlet is 260-280 DEG C, the initial column temperature is 40-50 DEG C, the conditions are kept for 1-5 minutes, and the temperature is increased to 200-280 DEG C at the speed of 5-30 DEG C / min; the conditions of the mass spectrum are as follows: the temperature of an ion source is 230-250 DEG C, and the temperature of a transmission line is 310 DEG C. By controlling extraction, chromatography and mass spectrometry conditions, N-methylaniline can be effectively separated from a sample, and accurate and efficient qualitative and quantitative analysis can be performed on N-methylaniline.

The invention discloses a coaxial dielectric barrier discharge micro-plasma multi-dimensional element compound detection device which comprises a capillary column assembly and a capillary column interface assembly, the capillary column assembly is provided with a gas transmission channel extending in the axial direction of the capillary column assembly, one end of the capillary column assembly is a capillary gas inlet end, and the other end of the capillary column assembly is connected to the capillary column interface assembly. A conical contraction connector is arranged in the capillary column connector assembly, and the conical contraction connector is gradually transited from the large section to the small section in the gas flowing direction. The plasma discharge cavity is communicated with the capillary column interface assembly and extends along the axial direction; and a first electrode and a second electrode are wound outside the plasma discharge cavity. And a medium tube is arranged between the first electrode and the second electrode. And the first electrode and the second electrode are electrically connected with a high-voltage converter power supply. One end of the plasma discharge cavity away from the capillary column interface assembly is provided with a plasma lighting window; an optical detection assembly is arranged on the outer side of the plasma discharge cavity.

The invention belongs to the field of detection, and particularly relates to a quantitative detection method for benzene in an eltrombopag ethanolamine bulk drug. Comprising the following steps: respectively injecting a test solution and a reference solution into a gas chromatograph by adopting headspace sampling, recording a chromatogram, and carrying out quantitative analysis on the chromatogram by adopting an external standard method; wherein the detection conditions of the chromatography are as follows: a chromatographic column is a capillary column taking 6% of cyanopropyl phenyl-94% of dimethyl polysiloxane as a stationary liquid or a capillary chromatographic column with equivalent efficiency; the column temperature is programmed temperature rise: the initial temperature is 55-65 DEG C, the temperature is maintained for 3 minutes, the temperature is raised to 150 DEG C at the rate of 5 DEG C per minute, then the temperature is raised to 240 DEG C at the rate of 30 DEG C per minute, and the temperature is maintained for 5 minutes; the balance temperature of the headspace bottle is 90-100 DEG C, and the balance time is 20 minutes. The method has the advantages of strong specificity, high sensitivity and high accuracy, and can accurately quantify the benzene content in the preparation process of the eltrombopag ethanolamine bulk drug.

The application provides a method for preparing adamantane, which comprises: isomerizing tetrahydrodicyclopentadiene in the presence of a mesoporous mordenite molecular sieve catalyst with acid sites established by an organic acid, in the presence of an optional organic solvent, and in a hydrogen-containing atmosphere; and calculating the NH3-TPD peak area of the catalyst by integration, wherein the peak area of the weak acid center of the catalyst is greater than or equal to 330, the peak area of the strong acid center of the catalyst is less than or equal to 282, and the specific surface area of the catalyst is greater than or equal to 300 m 2 / g. In the synthesis of adamantane by the method, the isomerization reaction of adamantane is carried out in the presence of the above catalyst, at a reaction temperature of 250 DEG C, a hydrogen pressure of 1 Mpa, and in a 100-ml stainless steel autoclave. The product composition is analyzed by gas chromatography, and the chromatographic column is an HP-5 capillary column with a column length of 30 m. The purity of adamantane can reach more than 99%.

The invention discloses a vapor chamber, and belongs to the technical field of heat dissipation of electronic devices. The vapor chamber comprises a shell assembly, an evaporation capillary structure, a condensation capillary structure and a plurality of capillary column structures, the shell assembly comprises a first inner wall and a second inner wall which are oppositely arranged in the first direction. The evaporation capillary structure is arranged on the first inner wall, a first middle area is arranged in the middle of the evaporation capillary structure, and the first middle area is concavely arranged towards the first inner wall; the condensation capillary structure is arranged on the second inner wall, and the condensation capillary structure and the condensation capillary structure are arranged at intervals; one end of each capillary column structure is connected to the condensation capillary structure, and the other end of each capillary column structure is connected to the evaporation capillary structure. According to the vapor chamber, collaborative optimization of circulation of the liquid working medium and the vapor working medium is achieved, the heat transfer efficiency and the temperature equalizing performance of the vapor chamber are improved, and the efficient heat dissipation requirement of a high-power-density electronic device is met.

The present invention discloses a method for preparing a capillary chromatographic column based on a metal-organic framework material for chiral separation, comprising the following steps: slowly adding a monohydrated copper acetate aqueous solution to a gel-like ligand product aqueous solution for reaction to obtain a metal-organic framework material solution; passing the metal-organic framework material solution through a capillary column pre-anchored with the obtained ligand for 0.5 to 2 hours, closing the column, allowing the column to stand for reaction, and rinsing with ultrapure water to obtain the capillary chromatographic column based on the metal-organic framework material for chiral separation. The capillary chromatographic column prepared by the present invention has good thermal and chemical stability, maintains structural integrity under high temperature, partial acid and alkaline conditions, and long-term storage conditions, and maintains good stability after 100 runs.

The invention provides a method for detecting six isomers of trinitrotoluene, a separation method in the detection method is a gas chromatographic method, a quantitative detector in the detection method is a mass spectrometric detector, and a qualitative method in the detection method is standard sample verification. A chromatographic column in the gas chromatography is a capillary column; the temperature rise mode of a column oven in the gas chromatography is a programmed temperature rise mode. The rapid detection method for the six isomers of trinitrotoluene has the characteristics of good peak presentation, high resolution, strong repeatability and simple and rapid operation, can realize separation and content determination of the six isomers of trinitrotoluene in one step, saves the test cost, is convenient to popularize and has wide application prospects. And effective guarantee is provided for synthesis process monitoring and product quality control of TNT.

The invention mainly relates to the technical field of gas chromatography detection, in particular to a method for detecting an alkane plasticizer in a silicone adhesive. One purpose of the invention is to provide a method for detecting an alkane plasticizer in a silicone adhesive. The method comprises the following steps: a, pretreating a sample; b, preparing a standard sample; c, detection of a standard sample and a test sample: a gas chromatograph is used for detection, and chromatographic conditions comprise that a chromatographic column is a 100% polydimethylsiloxane capillary column (preferably 30 m * 0.32 mm * 0.25 m); the carrier gas is nitrogen; the gas flow is 5 mL / min. The method for detecting the alkane plasticizer in the silicone adhesive has the advantages of rapidness, high sensitivity, excellent quantitative accuracy and wide applicability, and is of great significance to guarantee of product quality and safety compliance.

The invention discloses a method for measuring refrigerant ratio by gas chromatography, and belongs to the technical field of refrigerant gas chromatographic analysis. According to the technical scheme, a sampling steel cylinder is used for sampling, a double-valve type steel cylinder or a single-valve type steel cylinder is used for preparing a standard sample, a gas chromatographic method is used for determining the content of R404 series and R507 series refrigerants in a matching mode, chromatographic columns are aluminum oxide capillary columns, detectors are hydrogen flame ionization detectors, and the gas chromatographic method is used for determining the content of R404 series refrigerants and R507 series refrigerants in a matching mode. The used carrier gas is high-purity nitrogen. According to the invention, the defects existing in the existing use standard detection are overcome, and the same gas chromatograph can detect R404 series refrigerants and analyze R507 series refrigerants on the basis of setting parameters, so that accurate detection is realized.

The utility model relates to a gas chromatography detection system for analyzing trace impurity hydrocarbon in ultrapure ammonia. Comprising an ultrapure ammonia gas quantitative sampling unit, and the ultrapure ammonia gas quantitative sampling unit is connected with a detection unit through a C1-C3 pre-separation unit; the detection unit comprises a DID detector, an inlet of the DID detector is connected with a fourth interface of a switching valve VIII, a first interface of the switching valve VIII is connected with a third carrier gas pipeline, a second interface of the switching valve VIII is connected with a second emptying pipeline, and a third interface of the switching valve VIII is connected with C1-C3 pre-separation units through a special capillary column; the device has the characteristics of simple structure, reasonable design, simplicity in operation, high detection sensitivity of the system, capability of ensuring that all components do not interfere with each other to generate peaks and capability of preventing main components from polluting a chromatographic column and a detector.

The application discloses a detection method of related substances in (3S, 5S)-3-Boc-amino-5-methylpiperidine. The related substances are detected by using a gas chromatography method. The detection method provided by the application solves the interference problem of other impurities possibly introduced in the process. The application researches and screens gas phase lining pipes of different materials, capillary columns of different stationary liquids, different sample injection procedures, sample injection bottle materials and sample dispensing droppers, provides an optimized detection method, and proposes solutions to the problems of poor reproducibility, adsorption and leaching in the detection process, so that the accuracy of the detection result is ensured.

The invention discloses a method for detecting related substances of sulfolane, which comprises the following steps: by taking nitroterephthalic acid modified polyethylene glycol as a capillary column of a stationary liquid and a methanol solution containing 2, 6-butylated hydroxytoluene as a solvent, directly injecting a sample through temperature programming and carrying out gas chromatography detection; the contents of isopropyl sulfolane ether and 2-butadiene sulfone are calculated by using an external standard method, and the contents of other single impurities are calculated by using a peak area normalization method. According to the method, 2, 6-butylated hydroxytoluene is added into the solvent, degradation of a 2-cyclobutene peak can be effectively inhibited, and the problems that in the sulfolane capillary column gas chromatography, the accuracy and linearity of 2-cyclobutene sulfone are poor, and the solution stability is poor are successfully solved. The method provided by the invention can be applied to factory-in detection of sulfolane, additional modification of a gas chromatograph is not needed, and additional training related to a packed column does not need to be carried out on analysts, so that the implementation period of the method is shortened, and the implementation and detection cost of the method is reduced.

Invention Title: A Method for Detecting Ethylene Glycol and Diethylene Glycol in Aripiprazole Oral Solution Abstract: This invention provides a method for detecting ethylene glycol and diethylene glycol in aripiprazole oral solution, applicable to the field of drug oral preparation detection technology, especially in the field of pharmaceutical quality control, requiring gas chromatography detection methods to monitor pharmaceutical excipients and byproducts. This analytical method overcomes the limitations of ethylene glycol and diethylene glycol, which lack ultraviolet absorption methods. The sample solution is injected into the injection port via a microsyringe, and instantly vaporized in a high-temperature vaporization chamber, increasing sensitivity and accuracy, and solving the problems of low detection efficiency and low precision. Separation and detection efficiency are improved by optimizing column temperature and other conditions. This invention uses high-performance gas chromatography (HPLC) with a 100% bonded cross-linked polyethylene glycol (PEG) capillary column, a flame ionization detector, nitrogen as the carrier gas, and an organic solvent as the diluent. It uses a conventional chromatographic column, an automated injection method, and reduces costs. Gradient temperature elution is employed for separation and detection. This invention relates to a method for the detection of ethylene glycol and diethylene glycol in aripiprazole oral solution. This method has good separation, high specificity, high precision, and good repeatability, and meets the requirements for methodological research on the determination of ethylene glycol and diethylene glycol in aripiprazole oral solution.

The invention provides a water-gas dual-purpose halogenated olefin sensor, and relates to the technical field of analytical chemistry instruments, the water-gas dual-purpose halogenated olefin sensor comprises a carrier gas pipeline, a clustered membrane in-situ extraction sampling device, a cold trap dehydration device, a gas sample pipeline and a photoionization detector, the clustered membrane in-situ extraction sampling device is connected with the cold trap dehydration device through a conveying pipeline; the clustered membrane in-situ extraction sampling device comprises a container and a membrane sampling device, a liquid sample is contained in the container, the membrane sampling device comprises a clustered membrane, and halogenated olefin in water is extracted into a gas phase; the cold trap dehydration device is used for dehumidifying the gas conveyed in the conveying pipeline to obtain a low-humidity halogenated olefin-containing gas sample, and the low-humidity halogenated olefin-containing gas sample is sent into the photoionization detector for detection through the capillary column; and the gas sample pipeline is directly connected with the ionization detector. The water-gas dual-purpose halogenated olefin sensor disclosed by the invention is high in sensitivity, solves the problems of humidity interference, poor membrane stability and the like, and is suitable for detecting halogenated olefin in underground water.

The invention belongs to the technical field of medicines, and particularly relates to a method for determining the content of triethylamine in a vaccine adjuvant MPLA and homologues thereof. According to the detection method, a vaccine adjuvant MPLA and / or a homologue are / is taken as a sample to be detected, and gas chromatography is adopted for detection; according to the gas chromatography, a capillary column coated with a non-polar stationary phase is used as a chromatographic column, a mixture of an organic solvent and an inorganic polar solvent is used as an analysis solution, and detection is carried out in a gradient heating mode. According to the method disclosed by the invention, the content of triethylamine in the vaccine adjuvant MPLA or homologues thereof can be efficiently, accurately and conveniently measured. The optimal stationary phase and diluent composition and the optimal determination condition are selected through screening, and a rapid method is provided for accurately completing the method for detecting the content of the triethylamine in the MPLA or the homologues of the MPLA. The method is high in accuracy, convenient to operate, high in efficiency and suitable for being widely popularized and used.

The invention relates to the technical field of chemical analysis and detection, and discloses a method for detecting pivalaldehyde in amamecycline and tosilate thereof by gas chromatography, the gas chromatography is adopted, and the gas chromatography conditions are as follows: a detector is an FID (Flame Ionization Detector), a chromatographic column is a capillary column which takes 5% phenyl-95% methylpolysiloxane as a stationary liquid, temperature programming is adopted, and the detection time is 30 minutes; the initial temperature is 35-45 DEG C, the temperature is maintained for 5 minutes, the temperature is raised to 110 DEG C at the rate of 10 DEG C per minute, then the temperature is raised to 240-280 DEG C at the rate of 40 DEG C per minute, and the temperature is maintained for 5-9 minutes; the invention establishes a simple method capable of detecting pivalaldehyde, so as to detect the levels of pivalaldehyde impurities in the ombalicycline and tosilate thereof, and the method is very important for ensuring the controllability of the product quality.

The invention discloses a method for detecting free fatty acid in ganoderma lucidum spore oil or a preparation thereof and application thereof, the method comprises the following steps: loading the content of the ganoderma lucidum spore oil or the preparation thereof to be detected into a small solid-phase extraction column with silica gel as a filler, eluting with a solvent, collecting eluent, carrying out saponification reaction and methyl esterification reaction after nitrogen blowing, extracting with an organic solvent, and concentrating to obtain the free fatty acid in the ganoderma lucidum spore oil or the preparation thereof. Obtaining a test solution; performing gas chromatography detection on the test solution; a filling material of a capillary column for gas chromatography detection is polyethylene glycol or modified polyethylene glycol, and a heating procedure is as follows: the initial temperature is 110-130 DEG C, the temperature is maintained for 3-5 minutes, the temperature is raised to 240-250 DEG C at the rate of 8-12 DEG C / min, and the temperature is maintained for 2-4 minutes. The detection method disclosed by the invention is low in cost, short in time consumption, high in analysis efficiency, high in sensitivity and high in accuracy, can be used for sensitively monitoring the tiny quality change of the ganoderma lucidum spore oil or the preparation thereof in the initial storage stage, and has important practical application value for product quality control and stability evaluation of the ganoderma lucidum spore oil or the preparation thereof.

The embodiment of the application discloses a gas chromatographic column and a preparation method and application thereof.The method comprises the following steps: (1) treating the inner wall of a quartz capillary column with acid to hydroxylize the surface; (2) depositing silica on the inner wall of the quartz capillary column to increase the surface roughness; (3) inertly treating the inner wall of the quartz capillary column; and (4) coating a stationary phase solution on the inner wall of the quartz capillary column to form a uniform film layer.The gas chromatographic column has high wettability, thermodynamic stability, chemical stability, ultrahigh inertness, stable detection signal and high product success rate.Under the scheme, various types of chromatographic columns are developed, and various impurities can be jointly detected, the purity analysis of compounds is improved, and the gas chromatographic column is mainly widely applied to the analysis and detection of fire extinguishing agents in fluorine chemical industry and other industries.