113 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.

The embodiment of the invention provides a uniform temperature plate and a heat dissipation device, the uniform temperature plate comprises an evaporation capillary structure, a condensation capillary structure, a capillary column structure connected between the evaporation capillary structure and the condensation capillary structure, and a heat dissipation structure connected between the evaporation capillary structure and the condensation capillary structure, and the middle thickness of the condensation capillary structure is larger than the peripheral thickness of the condensation capillary structure. And the liquid working medium flows back to the evaporation capillary structure along the capillary column structure. According to the embodiment of the invention, the problem of dry burning or overlarge evaporation thermal resistance of the capillary structure of the vapor chamber in the prior art can be solved, the evaporation thermal resistance is reduced, the circulation heat dissipation efficiency of the phase change working medium is accelerated, dry burning of the capillary structure is prevented, and the heat transfer capacity of the vapor chamber is improved.

The present invention relates to the preparation and application of a micro-cell in-situ microreactor. By subjecting the inner wall of a capillary to silanization treatment and modifying epoxy groups on its surface through free radical polymerization reaction, an open-tubular capillary column is prepared. Then, polyethyleneimine and iodoacetic acid-N-succinimidyl ester are successively modified by covalent bonding to prepare a solid-phase alkylated capillary microreactor. The advantages of the present invention are that proteomic sample processing is carried out in-situ, which is conducive to reducing sample loss caused by multiple transfers during traditional sample processing. Therefore, this solid-phase alkylated open-tubular column is suitable for proteomic pretreatment of trace samples. In addition, this method is tolerant to various surfactants and strong lysis reagents and has good sample compatibility.

The invention discloses a detection method for simultaneously determining ethylene glycol and diethylene glycol in cetirizine hydrochloride drops, which comprises the following steps: step 1, setting chromatographic conditions: heating to 220 DEG C at a rate of 20 DEG C / min by using a capillary column with 6% propylphenyl-94% dimethyl polysiloxane as a stationary liquid, and maintaining for 10 minutes; step 2, solution preparation: preparing a blank solvent, a reference solution and a test solution; step 3, determination: taking the blank solvent, the reference substance solution and the test solution for sample introduction analysis, and recording a chromatogram; step 4, limit: calculating by peak area according to an external standard method, wherein the content of ethylene glycol is not more than 0.062%, and the content of diethylene glycol is not more than 0.025%; the method disclosed by the invention is simple, convenient, rapid, high in accuracy and good in specificity, can be used for simultaneously determining the contents of ethylene glycol and diethylene glycol in the cetirizine hydrochloride drops, and is suitable for quality research and control of the cetirizine hydrochloride drops.

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 discloses a method for detecting related substances of tribromoacetone by gas chromatography, which belongs to the technical field of chemical detection, the related substances of tribromoacetone are detected by gas chromatography, an instrument is a gas chromatograph, a detector is an FID detector, a capillary column taking 100% methylpolysiloxane (MEGA-1) as a stationary liquid is used as a chromatographic column, carrier gas is N2, the flow velocity is 2.0 mL / min, the split ratio is 50: 1, and the detection time is 30 minutes. Temperature programming: the initial temperature is 80 DEG C, and the temperature is raised to 250 DEG C at the rate of 10 DEG C per minute and maintained for 10 minutes; a sample injection mode is as follows: direct sample injection is performed, the temperature of a sample injection port is 260 DEG C, and the temperature of a detector is 280 DEG C; according to the present invention, the sample introduction volume is 0.2 [mu] l, the related substances in the tribromoacetone can be effectively separated, the content of the related substances can be quantitatively detected, the acetone, the bromoacetone, the 1, 3-dibromoacetone and the 1, 1, 3, 3-tetrabromoacetone sequentially appear peaks, and the method has characteristics of simple operation, strong specificity, good repeatability, good intermediate precision and good durability, and can accurately and rapidly determine the content of the various related substances in the tribromoacetone.

The invention belongs to the technical field of medicine detection, and particularly relates to a method for determining enantiomers in a levocarnitine intermediate by gas chromatography. The method for determining the enantiomer in the levocarnitine intermediate by the gas chromatography comprises the following steps: taking a capillary column which takes dimethyl polysiloxane bonded with cyclodextrin as a stationary liquid as a chromatographic column; the method comprises the following steps: dissolving and diluting a test product (R)-4-chloro-3-hydroxy ethyl butyrate by using ethyl acetate, and deriving by adding acetic anhydride and pyridine to prepare a test product solution; and injecting the test solution into a gas chromatograph, recording a chromatogram, and calculating the content of the enantiomer (S)-4-chloro-3-hydroxybutyric acid ethyl ester in the levocarnitine intermediate (R)-4-chloro-3-hydroxybutyric acid ethyl ester according to an area normalization method. The method for determining the enantiomer in the levocarnitine intermediate by the gas chromatography provided by the invention is accurate and fast in detection, and provides a basis for quality control of levocarnitine.

The invention relates to the technical field of traditional Chinese medicine detection, in particular to a method for determining the content of various components in blumea balsamifera oil. According to the method, a gas chromatography-mass spectrometry (GC-MS) technology is adopted, and chromatographic conditions are as follows: a chromatographic column is an SH-Stabilwax (30m * 0.32 mm, and the film thickness is 0.25 [mu] m) capillary column; the temperature of a sample inlet is 230 DEG C; the split ratio is 10: 1; the sample size is 1 microliter; the mass spectrum conditions are as follows: the ion source temperature is 200 DEG C; the interface temperature is 230 DEG C; the ionization mode is electron impact ion (EI); the detection voltage is 0.2 KV; the solvent is delayed for 2 minutes; the mass number scanning range is 30 to 400 amu; and SIM mode. According to the method disclosed by the invention, the contents of alpha-pinene, camphene, beta-pinene, limonene, p-cymene, camphor, alpha-coumarin, linalool, bornyl acetate, beta-caryophyllene, myrtenal, alpha-caryophyllene, L-borneol, perillaldehyde, caryophyllene oxide, guaiacol, beta-eudesmol and xanthoxylin in the blumea balsamifera oil can be simultaneously determined; the method provided by the invention has good precision, repeatability and stability, and the quality consistency of the blumea balsamifera oil can be quickly, accurately and effectively evaluated through detection of multiple components.

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.

The invention discloses a method for detecting NDMA in a famotidine injection by adopting gas chromatography-mass spectrometry. The method comprises the following steps: detecting a to-be-detected sample of the famotidine injection by adopting gas chromatography-mass spectrometry; the parameter conditions of the gas chromatography are as follows: a capillary column taking polyethylene glycol (or similar polarity) as a stationary liquid is taken as a chromatographic column; the temperature of a sample inlet is 190-210 DEG C; the heating procedure is as follows: the initial temperature is 54-66 DEG C, and the temperature is kept for 0.5-1.5 minutes; the temperature is raised to 235-245 DEG C at the temperature raising rate of 15-25 DEG C / min, and the temperature is kept for 0 min; the parameter conditions of the mass spectrum are as follows: the acquisition type is SRM; the ion source is EI; the solvent delay is 0 min; the temperature of the transmission line is 235-245 DEG C; and the temperature of the ion source is 245-255 DEG C. The method is simple to operate, high in detection speed, low in detection limit and high in reliability.

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 provides a gas phase detection method for simultaneously determining six chlorine-based disinfectant byproducts in serum. The gas phase detection method comprises the following steps: S1, liquid-liquid extraction-acidification methanol derivatization pretreatment; s2, instrument detection: S21, chromatographic conditions: a 6890N gas chromatograph and a DB-1701 capillary column are adopted, the temperature of a sample inlet is 200-250 DEG C, and the temperature of a detector is 280-320 DEG C; s22, carrying gas and flow velocity; s23, temperature programming conditions are set; according to the method, by optimizing detection conditions, the recovery rate of the HAAs is increased, and the detection limit of the method is reduced, and the method is proper in sensitivity, small in sample usage amount, simple and convenient to operate and capable of being widely applied to detection of the HAAs in clinical large-scale queues and serum.

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 method for determining the residual quantity of petroleum ether in an isonicotinamide benzonate bulk drug by using capillary gas chromatography, and belongs to the technical field of drug analysis. According to the method, an external standard method is adopted for quantification, a 6% cyanopropyl phenyl-94% dimethyl polysiloxane capillary column is used as a chromatographic column, and an FID detector is adopted for detection; the residual quantity of the petroleum ether is the total residual quantity of normal hexane, 2-methylpentane and 3-methylpentane in the petroleum ether. The method disclosed by the invention is good in specificity, good in linearity, reliable in accuracy and high in sensitivity; the gas chromatographic method can be used for rapidly, effectively, accurately and reliably separating and detecting the residual amount of petroleum ether in the isopropylamine bulk drug, and is beneficial to improving the product quality of the isopropylamine bulk drug and improving the medication safety of a patient.

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 belongs to the technical field of medicine detection, and particularly relates to a method for detecting and analyzing dimethyl sulfate in potassium sulfate serving as a raw material of a sodium potassium magnesium sulfate concentrated solution, the method adopts gas chromatography, and the chromatographic conditions are as follows: a chromatographic column is a capillary column of a non-polar stationary phase; the temperature programming control is as follows: the initial temperature of the column temperature is controlled to be 40-60 DEG C, the holding time is 2-5 minutes, the temperature is raised to 120-140 DEG C at the rate of 5-20 DEG C / min, then the temperature is raised to 230-280 DEG C at the rate of 15-25 DEG C / min, and the holding time is 5-15 minutes; the temperature of a sample inlet is 240-280 DEG C; the temperature of a detector is 250-350 DEG C. The method provided by the invention can detect the content of dimethyl sulfate in potassium sulfate, does not appear in the existing detection method, and can make up the technical blank in the field. The analysis method provided by the invention is good in specificity, high in repeatability, low in detection limit and high in accuracy.

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 discloses a gas chromatograph-mass spectrometer extended low-temperature column oven device which comprises a gas chromatographic column oven, a low-temperature column oven body and a low-temperature column oven cover, an inner container is arranged in the gas chromatographic column oven, the gas chromatograph-mass spectrometer extended low-temperature column oven device further comprises sliding rails, a chromatographic column hanging frame and a lifting structure, a pair of sliding rails is arranged on the opposite side faces of the inner container, and the lifting structure is arranged on the sliding rails. Box body sliding blocks are arranged on the two sides of the low-temperature column oven body respectively, box cover sliding blocks are arranged on the two sides of the low-temperature column oven cover respectively, and the box body sliding blocks and the box cover sliding blocks located on the same side are aligned and then jointly inserted into the sliding rails on the same side and can slide along the sliding rails; the chromatographic column hanger is rotatably mounted on the lifting structure; a heating disc and a fan are mounted in the gas chromatographic column oven; and the heating disc is positioned between the low-temperature column oven and the fan and faces the low-temperature column oven. According to the device, the chromatographic separation of permanent gas and low-boiling-point compounds by a single capillary column is realized, the rapid switching of common test and an extended low-temperature column oven is realized, and the variable adjustment of the distance between the chromatographic column and a protective sieve plate is realized.

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 invention discloses a method for determining the purity of tert-butyl-(S)-[2-(2-cyano-4,4-difluoropyrrolidine-1-yl)-2-oxyethyl] carbamate, which comprises a capillary column with (5%-phenyl)-95% methyl polysiloxane copolymer as a stationary liquid as a gas chromatography column, and a temperature program is used to calculate the purity of tert-butyl-(S)-[2-(2-cyano-4,4-difluoropyrrolidine-1-yl)-2-oxyethyl] carbamate by a peak area normalization method after injection. The invention adopts a gas chromatography program temperature method to detect the purity of Boc-Fapi-a, which can avoid the influence of weak UV response signals and different response intensities of each impurity component, makes up for the technical gap of the current lack of an effective chromatographic detection method for the substance, realizes convenient quality control, and meets the detection requirements.

The invention discloses a method for detecting the content of hydrazine in a bile acid product, which adopts a gas chromatographic method to detect the content of hydrazine in the bile acid product, and the chromatographic conditions are as follows: a gas chromatograph adopts Shimadzu GC-2030; a chromatographic column is an SH-Wax capillary column, and the chromatographic column is 60.0 m * 0.25 mm * 0.5 [mu] m; the carrier gas is high-purity nitrogen; the flow velocity is 2.0 ml / min; the split ratio is 1: 1; the detector is a hydrogen flame ionization detector; the temperature of the detector is 220 DEG C; the temperature of a sample inlet is 200 DEG C; the headspace sampling amount is 5ml; the temperature rising procedure of the chromatographic column is as follows: from 80 DEG C, raising the temperature to 100 DEG C at the rate of raising the temperature by 10 DEG C per minute, retaining for 20 minutes, raising the temperature to 220 DEG C at the rate of raising the temperature by 20 DEG C per minute, and retaining for 17 minutes; the headspace temperature and time are set as follows: the box body temperature is 80 DEG C, the flow path temperature is 90 DEG C, the transmission line temperature is 100 DEG C, the circulation time is 65 minutes, and the sample preheating time is 60 minutes. The method can rapidly, accurately and effectively separate and measure the hydrazine content in the bile acid product, improves the detection efficiency, greatly reduces the detection cost, and is simple in operation process and strong in specificity.

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.