39 results about "Capillary column" patented technology

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 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.

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 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 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 present application relates to the technical field of drug screening, in particular to an effective mobility ratio screening method based on affinity capillary electrochromatography and application. A target protein is fixed by a MOF material, and a capillary electrochromatography column is prepared by in-situ growth method; a to-be-tested substance is passed through the column, and screening is realized according to the affinity between the to-be-screened component and the protein; the present application adopts effective mobility ratio as a quantitative screening strategy, and the binding affinity between the to-be-screened component and the target protein is directly and quantitatively represented by calculating the effective mobility ratio of the drug in the column containing the fixed phase and the empty capillary column, so that efficient, stable and sensitive screening of multiple active ingredients in a complex system is realized, the stability and reusability of the affinity capillary electrochromatography platform are improved, the drug screening strategy is improved, and the present application is expected to become an effective and reliable strategy for screening of thrombin inhibitors in natural products.

The invention provides a method for detecting the content of methanol in liquid essence, and belongs to the field of pharmaceutical analysis. According to the method, a capillary column method is adopted, dimethyl polysiloxane is taken as a stationary phase, headspace sampling is carried out, and the content of methanol is calculated by peak area according to an external standard method. Compared with the prior art, the method has the advantages of high specificity, good reproducibility, high sensitivity and the like.

This invention belongs to the field of analytical detection technology, specifically relating to a method for detecting the abundance of sulfur hexafluoride isotopes. The method for detecting the abundance of sulfur hexafluoride isotopes provided by this invention includes the following steps: gas chromatography-mass spectrometry (GC-MS) is used to detect the sample to obtain a total ion current chromatogram of sulfur hexafluoride; the GC-MS test conditions include: DB-5MS capillary column, split ratio of 20~80:1, and injection volume of 1~10µL; the mass spectrometry test conditions include: multiplier voltage +300~+600, and half-maximum width at half maximum (HWHM) below 0.6; the total ion current chromatogram of sulfur hexafluoride is then analyzed... 32 SF5 + , 33 SF5 + and 34 SF5 + Extract ions and obtain 32 SF5 + , 33 SF5 + and 34 SF5 + The peak area was calculated. 32 SF5 + , 33 SF5 + and 34 SF5 + The abundance of [the substance / method / method]. The detection method provided by this invention has the advantages of being economical, having a fast analysis speed, and high accuracy.

The invention provides a chromatography-mass spectrometry / mass spectrometry rapid detection method for heliotropin in essential oil for cleaning. The chromatography-mass spectrometry / mass spectrometry rapid detection method for heliotropin in essential oil for cleaning comprises the following steps: S1, sample pretreatment: carrying out ultrasonic extraction on an essential oil sample by using a mixed solvent of normal hexane and ethyl acetate to obtain an extracting solution; purifying the extracting solution through a silica gel solid-phase extraction column, leaching with n-hexane, eluting with ethyl acetate, and collecting the eluent; and S2, gas chromatography-tandem mass spectrometry analysis: carrying out GC-MS / MS analysis on the eluent obtained in the step S1, with a chromatographic column being a weakly polar or non-polar capillary column and mass spectrometry adopting a multi-reaction monitoring mode, and carrying out qualitative and quantitative detection on heliotropin by an internal standard method. The chromatography-mass spectrometry / mass spectrometry rapid detection method for heliotropin in essential oil for cleaning provided by the invention has the advantages of simple and convenient treatment steps, good sensitivity, high accuracy and short analysis time.

This invention provides a capillary electrophoresis analysis method for serum amino acids, comprising the following steps: S1 preparation of running buffer; S2 selection and pretreatment of a quartz capillary column; S3 electrophoresis analysis conditions; S4 plotting a quasi-curve; S5 sample derivatization; and S6 quantitative analysis. This method is the first to employ... α‑ Cyclodextrin, β‑ Cyclodextrin and c‑ The cyclodextrin mixture synergistically regulates amino acid migration behavior, expands the migration time window, effectively improves the separation resolution of structurally similar amino acids, and significantly enhances separation efficiency and chromatographic clarity. The addition of sodium taurocholate, along with pH adjustment, forms a weakly alkaline buffer system with moderate conductivity and stable migration behavior, which is beneficial for the separation and detection of FITC-derived amino acids and optimizes the uniformity of migration time distribution. This invention is applicable to clinical sample analysis, disease biomarker screening, and other scenarios, possessing good versatility, stability, and promotional value.

The invention provides a chromatographic analysis method of methyl mercaptan. The chromatographic analysis method comprises the following steps: providing a liquid methyl mercaptan sample under the pressure of 1-3 MPa; a liquid methyl mercaptan sample is conveyed into a gas chromatograph through a high-pressure liquid sample injection valve and is separated and detected through two analysis paths, wherein the first analysis path comprises that the vaporized sample sequentially enters a first chromatographic column and a second chromatographic column for limiting flow to be separated; the second analysis path comprises the following steps: intercepting fractions flowing out of the first chromatographic column from the vaporized sample entering the first chromatographic column according to a preset time window through a center cutting technology in a microflow plate center cutting system, and then cutting the fractions into a third chromatographic column for re-separation; the first chromatographic column is a non-polar capillary column or a weak-polar capillary column, the second chromatographic column is an empty white chromatographic column, and the third chromatographic column is a polar or medium-polar capillary column. The invention provides complete off-line analysis for high-purity liquid methyl mercaptan samples from sample stabilization to efficient quantitative and qualitative analysis and separation of impurities.

This invention relates to the field of thermal management technology, specifically to a method for manufacturing a harmonica-shaped vapor chamber. The method first provides a copper-aluminum composite billet, which is extruded into a harmonica-shaped shell and microchannels. Then, a differentiated capillary column array is deposited on the inner wall of the microchannels using selective laser melting. Next, copper powder slurry is sintered to form a porous substrate layer. Following this, a dendritic fractal microchannel network is constructed using electrochemical etching, and a nanocomposite coating is deposited. Finally, the shell is laser-welded to seal it. After vacuuming, a nanofluidic working fluid containing carbon nanotubes is filled in, and the process is completed by heat treatment. This method integrates additive manufacturing, micromachining, and surface modification technologies, aiming to manufacture a vapor chamber with high-efficiency thermal transport performance. The integrated manufacturing of the harmonica-shaped shell through copper-aluminum composite material extrusion completely eliminates peripheral welding joints in traditional processes, improving airtightness by over 95%, while maintaining high thermal conductivity and achieving a 35% weight reduction.

The invention provides a multifunctional integrated chromatographic analysis device and an analysis method. The analysis device comprises a sample injection unit, a detection 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 is convenient, simple and efficient to use, can be used for gas chromatography and multi-channel surface energy analysis, can integrate multi-probe separation and multi-channel surface energy analysis, greatly improves the use flexibility of the analysis device, expands the test range, greatly shortens the test process, and improves the test efficiency.

The invention discloses a GC fingerprint spectrum detection method for traditional Chinese medicine, and belongs to the field of traditional Chinese medicine detection. The traditional Chinese medicine is prepared from nine medicinal materials including pericarpium citri reticulatae, thunberg fritillary bulb, selfheal, oroxylum indicum, platycodon grandiflorum, radix scrophulariae, semen coicis, biond magnolia flower and divaricate saposhnikovia root, and is used for treating the child adenoid hypertrophy, and the method comprises the following steps: preparing a test solution, adopting an HP-5 capillary column, performing analysis under the chromatographic conditions that the split ratio is 30: 1, temperature programming is performed, the temperature of a sample inlet is 290 DEG C, and the temperature of a detector is 300 DEG C, and recording a chromatogram for 075 min. A standard fingerprint spectrum containing 19 common peaks is established by measuring a plurality of batches of samples, the attribution of each peak is defined, and five characteristic components such as eucalyptol and beta-bisabolol are identified. The method is good in stability and high in reproducibility, the constructed fingerprint spectrum is high in characteristic, the method can be used for quality consistency evaluation and production process control of traditional Chinese medicine, and safety and effectiveness of clinical medication are guaranteed.

The invention relates to a method for preparing a colloidal crystal capillary column and application of the colloidal crystal capillary column in peptide fragment and protein separation, and the method specifically comprises the following steps: (1) drawing one end of a capillary into a spray needle, inserting the spray needle into a protective sleeve, and tightly connecting the end, far away from the spray needle, of the capillary with a conical outlet in the lower part of a conical liquid storage tank; (2) fixing the conical liquid storage tank above the centrifugal tube, and placing the capillary tube connected with the conical liquid storage tank in the centrifugal tube; and (3) uniformly dispersing the colloidal particles in the solvent, adding the colloidal dispersion liquid into the conical liquid storage tank, arranging a conical liquid storage tank upper cover at the opening end of the upper part of the conical liquid storage tank, applying centrifugal force to the centrifugal tube, and enabling the colloidal particles to enter the capillary tube from the conical liquid storage tank under the centrifugal action to assemble the three-dimensional colloidal crystal capillary column. The preparation flux of the colloidal crystal capillary column is improved, and the colloidal crystal capillary column has a good application prospect in the aspect of separation and characterization of biomolecules.

The application discloses a method for detecting the content of quinclorac in grain, and belongs to the technical field of food safety detection. The detection method comprises the following steps: (1) crushing a sample to be detected, adding anhydrous ethanol to perform ultrasonic extraction, and centrifuging to obtain an extraction liquid; (2) concentrating the extraction liquid to less than 1 mL; (3) adding a purifying agent to the concentrated liquid, vortexing, and centrifuging to obtain a purified extraction liquid; (4) detecting the purified extraction liquid by adopting an Rxi-5Sil MS or VF-1701ms capillary column in combination with GC-NCI-MS selected ion mode, and quantitatively calculating the content of quinclorac by adopting an internal standard method. The method is simple in operation, green and environment-friendly, accurate in qualitative and quantitative determination, and high in sensitivity, can be used for determining quinclorac in grain, and meets the detection requirements.

The invention discloses a method for detecting a residual solvent in an istradefylline bulk drug, which comprises the following steps: taking the istradefylline bulk drug, preparing a test solution, injecting the test solution into a gas chromatograph, adopting a capillary column with 6% cyanopropylphenyl-94% methylsiloxane as a stationary phase, carrying out programmed temperature rise, setting the temperature of a sample inlet to be 195-205 DEG C, and detecting the residual solvent in the istradefylline bulk drug. The temperature of a flame ionization detector (FID) is 245-255 DEG C, the column temperature is 38-42 DEG C, the column pressure is 98-102 kPa, the split ratio is 10: 1, the sample size is 1 [mu] L, and the peak area is calculated according to an external standard method. According to the technical scheme, by adopting the chromatographic conditions, the separation degree between the solvents is larger than 1.5, operation is easy, specificity is good, sensitivity is high, and the residual solvents in the istradefylline raw material medicine can be effectively separated.