58results about How to "Column depression" patented technology

The invention relates to a porous crosslinked polystyrene microsphere which has a surface micropore and internal macropore structure. Particularly, the mean pore size of surface micropores is 18.64-22.82nm, and the mean pore size of internal macropores is 0.75-1.64 micrometers. When the porous crosslinked polystyrene microsphere with the structure serves as chromatographic column filling, the column pressure can be effectively reduced; the internal macropore structure further increases action area between a detected substance and the microsphere; the retention time is prolonged; and substance separation can be better achieved.

The invention discloses a method for preparing surface mesoporous silica core-shell microspheres. The method comprises: selecting monodisperse non-porous silica microspheres with the particle size of 1 to 3 microns, dispersing quaternary ammonium salt B and quaternary ammonium salt A dispersing agents in ethanol water, dispersing the silica microspheres in water, adding a mixed surface active agent solution, regulating a pH value to be 7.5 to 10 by using ammonia water, adding tetraethoxysilane and / or tetramethoxysilane solution, washing, drying, calcining and removing a structure-directing agent, thereby obtaining the surface mesoporous silica core-shell microspheres. By utilizing the quaternary ammonium salt with two different carbon chain lengths as co-structure-directing agent, the core-shell microspheres with a relatively larger radioactive mesoporous structure are prepared; by regulating the proportion of two quaternary ammonium salt structure-directing agents, the mesoporous aperture is controllable in a range of 4 to 20 nm, the obtained radioactive mesoporous structure increases effective specific surface areas of the microspheres, and the application of the microspheres in adsorption, catalysis and separation analysis is improved.

The invention provides molecularly imprinted polymeric microspheres for phenol. The polymeric monomer of the polymeric microspheres is methacrylic acid or 4-vinylpyridine and the specific surface area of the polymeric microspheres is 23.08-62.33m<2> / g. The invention also provides a method for preparing the polymeric microspheres and the use of the polymeric microspheres in collection or detection of phenol compounds. In addition, the invention also provides a chromatographic column and a solid phase extraction cartridge filler. The filler is the molecularly imprinted polymeric microspheres. The molecularly imprinted polymeric microspheres are simple and convenient in preparation, have an adsorption selectivity of 8.25 to 44.55 mg / g, reach a balance within 6 hours and have the advantages of high absorption selectivity and high absorption speed.

A comprehensive utilization process of a glutamic acid crystal mother liquid comprises the following steps: one, leading the glutamic acid crystal mother liquid into a membrane separation system, allowing solid particles, thalli, proteins, polysaccharides and a colloid in the mother liquid to be intercepted by a membrane, and making glutamic acid left in a membrane filtrate; and allowing the membrane filtrate to go to a next step for treatment; two, leading the membrane filtrate into an ion exchange system, adsorbing glutamic acid by an ion exchange resin, when the content of glutamic acid in an ion exchange tail liquid is not more than 0.2%, stopping column-loading, adding an eluting agent, eluting, allowing glutamic acid to go into the eluate, collecting the eluate, and recycling glutamic acid from the eluate. The membrane separation technology and the ion exchange technology are combined, recycling of glutamic acid from the crystal mother liquid is realized, at the same time, a protein feed is prepared from the thalli and the proteins intercepted by the membrane, an organic fertilizer is prepared from the ion exchange tail liquid through slurry-spraying granulation, the whole process allows useful substances in the crystal mother liquid to be totally recycled, comprehensive utilization of the resources is thoroughly achieved, waste is turned into treasure, and significant economic benefits are achieved.

The invention discloses a novel method for preparing macroporous silicon dioxide@porous polymer core-shell microspheres. Non-porous silica microspheres are used as a core, octadecyltrichlorosilane isused for performing the surface hydrophobic modification, PVA and SDS are used as a dispersing agent, monomers GMA, a cross-linking agent EDMA and a pore forming agent are added to prepare the silicondioxide@porous polymer core-shell microspheres with a macroporous structure through an emulsion polymerization process. The preparation method is simple in preparation process, mild in conditions, and easy in mass production; and the surface of the prepared core-shell microspheres is a porous organic polymer which has higher acid and alkali resistance, the application range of core-shell fillersis enlarged, a larger aperture structure can be obtained, and the prepared core-shell microspheres are particularly suitable for the isolated analysis of biological molecules.

The invention discloses a detection method of salbutamol sulfate-related substances. The detection method qualitatively or quantitatively detects the salbutamol sulfate-related substances with high performance liquid chromatography; detection conditions comprise a chromatographic column: octyl-bonded silica gel column, a detection wavelength: 210-400 nm, and mobile phases comprising a mobile phaseA and a mobile phase B, wherein the mobile phase A is an aqueous phase containing a buffer solution and having pH of 1.5-4.0, further having pH of 2.0-3.0; the mobile phase B mainly comprises methanol or acetonitrile; the mobile phases are eluted by gradient elution; and detection steps are as follows: (1) preparing a test substance solution and a reference substance solution; and (2) respectively sampling and detecting the test solution and the reference solution. The detection method of the salbutamol sulfate-related substances adopted by the invention can ensure effective separation of therelated substances.

The invention discloses an integral separating dielectric of polymer and making method, which has regular three-dimensional frame structure constituted by polymer frame and through-out hole, wherein the nanometer grade middle-hole is formed on the surface of the polymer frame and / or in the polymer frame; the through-out hole is between 0. 1um and 10um and the middle hole is between 0nm and 50 nm; the frame size is 0. 2-2um. The invention has regular and sequent dielectric structure to be separated after doing chemical decoration for frame surface, which has huge applying potential in the macromolecular separating and purifying and solid phase extracting domain.

The invention discloses a polymer microsphere and preparation method and application thereof. Polystyrene is used for making a base sphere with the surface comprising a condensed-nuclei aromatic structure in pi-pi interaction with fullerene, and the structure is obtained by substituting a hydrogen atom on a benzene ring contained in the base sphere by chloromethyl and reacting with condensed-nuclei aromatics. The method includes: using a monodispersed polystyrene microsphere as the base sphere, mixing with catalyst SnCl4, adding aliphatic halogenate varsol, slowly dripping chloromethylation reagent while stirring for substitution reaction, allowing the reacted microsphere to react with the condensed-nuclei aromatics, and washing and drying the obtained microsphere to obtain a polymer microsphere with a fullerene separated liquid chromatographic stationary phase serving as a mobile phase. The preparation method of the surface modified polystyrene polymer microsphere only needs two steps, is simple in process, easy to repeat, suitable for massive production of fullerene and has the advantages of high separation efficiency and effectiveness.

The invention relates to high-performance liquid chromatography stationary phases, in particular to a hydrophilic interaction chromatography / ion exchange chromatography mixed stationary phase and preparation and application of the hydrophilic interaction chromatography / ion exchange chromatography mixed stationary phase. The structure of the hydrophilic interaction chromatography / ion exchange chromatography mixed stationary phase is shown as the formula 1, and please see the formula 1 in the specifications, wherein X is -OCH3 or -OCH2CH3, Y1 is F or Cl or Br or I or BF4 or Tf2N or CF3SO3 or SCN or NO2 or NO3, Y2 is -NHCH3 or -N (CH3)2 or -N+ (CH3)3Y1 or -NHCH2CH3 or -N (CH2CH3)2 or -N+ (CH2CH3)3Y1, and n=2 or 3. According to the prepared mixed type stationary phase, raw materials are easy to obtain and the preparation procedure are simple; and the prepared mixed type stationary phase has good retaining performance and separation selectivity for multiple saccharides and has good application and popularization prospects.

The invention provides a 2, 4, 6-trichlorophenol molecular engram microsphere polymer. The invention also provides a method for preparing the 2, 4, 6-trichlorophenol molecular engram microsphere polymer. The invention also provides application of the 2, 4, 6-trichlorophenol molecular engram microsphere polymer in enriching and / or separating 2, 4, 6-trichlorophenol. The invention also provides the application of the 2, 4, 6-trichlorophenol molecular engram microsphere polymer in monitoring and / or processing the 2, 4, 6-trichlorophenol in an environmental water sample. The invention also provides a method for detecting and / or processing the 2, 4, 6-trichlorophenol in a sample through the 2, 4, 6-trichlorophenol molecular engram microsphere polymer. The polymer has simple and convenient preparation, an even grain size, a large specific surface area and pore volume, and high absorption selectivity. The polymer can be used for carrying out the experiment directly in the water environment without excessive other organic agents. The polymer is environmentally friendly and has a high absorption speed.

The invention relates to a method for screening active ingredients of traditional Chinese medicine by nano mesoporous material immobilized target protein. The method includes filling mesoporous material immobilized protein into a chromatographic column, preparing an immobilized target protein inhibitor screening model, dissolving inhibitor having representative inhibiting effect on the immobilized protein into buffer solution to serve as a mobile phase, introducing samples of substrates with saturation concentration every fixed time, collecting peak appearance fraction, replacing the mobile phase with buffer solution free of inhibitor after fixed times, introducing samples of the substrates with saturation concentration every fixed time, respectively freezing and drying the fraction, dissolving the fraction into water, separating the substrates from a product through the analytical type chromatographic column, recording peak area of the product, drawing an inhibition curve of the immobilized target protein inhibitor, checking the model and adopting the prepared model to dissolve aqueous extract of traditional Chinese medicine to be screened into the buffer solution to serve as the mobile phase. Whether the traditional Chinese medicine has inhibition effect or not and the process and the type of the traditional Chinese medicine can be judged according to the peak area of the product. The method has the advantages of high reliability, online performance and the like.

Disclosed is a method for preparing an organic arsines molecular imprinting monolithic column and application thereof. The method comprises the steps of taking organic arsines veterinary drug carbarsone / nitarsone as template molecules, dissolving the template molecules in a mixed solution of carbinol and dodecanol, adding functional monomers, adding a cross-linking agent and a initiating agent after the mixture is prepolymerized at a low temperature, injecting the mixture into a lower-end-sealed empty column tube of a solid phase extraction column after nitrogen is led, sealing the upper end of the empty column tube of a solid phase extraction column, triggering polymerization at a temperature ranging between 10 DEG C and 30 DEG C for 12 hours to 60 hours, and then obtaining the molecular imprinting monolithic column. The molecular imprinting monolithic column which has good adsorption and enrichment effects on the organic arsines veterinary drug is obtained after the column is eluted from a porogen and the template molecules by a mixed solution of the carbinol and acetic acid. Compared with a traditional mass polymerization method, the method has advantages that the preparation and the postprocessing are simple, recognition is good, cost is low, and the required apparatus and reaction conditions can be acquired easily. The molecular imprinting monolithic column provided by the method can separate, enrich and purify the organic arsines veterinary drug remained in animal origin foods.

The invention discloses a preparation method for a porous polymer microsphere anion filling material. The preparation method comprises the following steps: a chloromethyl group is introduced at first, and then ethene diamine is introduced onto the surfaces of microspheres by using a surface grafting method. According to the invention, monodisperse polystyrene / divinyl benzene microspheres are used as a substrate which reacts with chloromethyl ether for introduction of a chloromethyl functional group and then reacts with ethene diamine via the surface grafting method so as to form the anion filling material. The anion filling material obtained in the invention has the characteristics of controllable microsphere size and controllable varieties of surface function groups; and the preparation method has the characteristics that the method is simple and easily practicable in process, low in cost for raw materials, easy to operate and easy for industrial application.

The invention belongs to the research field of organic polymeric materials, and discloses a preparation method and an application for a hydrophilic organic polymer liquid phase monolithic chromatographic column. The method comprises the following steps of employing monomers of 3-[N,N-dimethyl-[2-(2-enoyloxy)ethyl]butylamin]propane-1-sulfonate as functional monomers, mixing the functional monomers with a cross-linking agent, a pore-forming agent and an initiator, performing a thermocatalytic reaction, and carrying out in-situ polymerization in a quartz capillary to form the polymer liquid phase monolithic chromatographic column. The obtained chromatographic column has larger hydrophilic interaction area than a common hydrophilic chromatographic column. The monolithic chromatographic column is small in usage amount of the organic mobile phase, has little environmental pollution, is simple in preparation process and low in cost, has low column pressure, and is suitable for rapid separation of polar compounds.

The invention relates to the technical field of separation and purification of natural functional ingredients, and particularly discloses a method for purifying a capsaicin monomer by utilizing a reverse-phase resin. The method comprises the following steps: (1) carrying out preliminary purification on a crude capsaicin product obtained by virtue of an aqueous two-phase method by utilizing a macroporous resin; (2) further carrying out purification on the capsaicin by utilizing the novel reverse-phase resin; (3) crystallizing. The method has the beneficial effects that compared with reverse-phase carbon-18 silica gel fillers, the novel reverse-phase resin disclosed by the invention is low in price, low in column pressure and large in adsorption capacity; the whole process is simple and easy to operate and less in investment; meanwhile, a toxic organic solvent is not adopted, so that the production cost is greatly lowered and the purification efficiency is improved. The method is suitable for industrial production.

The invention relates to the technical field of drug analyzing, in particular to a method for detecting effective components in asthma pellets. A quantitative and qualitative detecting method for theeffective components in the asthma pellets is provided and used for qualifying ten effective components in the asthma pellets and quantifying seven effective components; the separation degree of the components is not lower than 1.5. With the adoption of the method, the seven effective components can be quantified, and the standard recovery rate ranges from 97.29 to 103.78%, so that the method is high in accuracy.

The invention relates to a padding used to do molecule brand solid-phase extraction and it's preparing method. The carrier of the padding is glass bead which has been surface modified. The preparing method of padding is using liquid film method to form a polymeric film layer with molecule brand at the surface of carrier.

The invention relates to a preparing method for ion exchange resin used for simultaneous separation of ten kinds of negative ions including F<->, ClO<2><->, BrO<3><->, Cl<->, NO<2><->, NO<3><->, Br<->, ClO<3><->, H2PO<4><-> and SO<4><2->, a negative ion chromatographic column prepared from the ion exchange resin prepared through the method and application of the negative ion chromatographic column. The preparing method for achieving the ion exchange resin, the negative ion chromatographic column prepared from the ion exchange resin prepared through the method and the application of the negative ion chromatographic column have the advantages that base balls of prepared ion exchange resin are mono-dispersed, the column pressure is low, and the service life is long; the prepared negative ion chromatographic column is convenient to operate, free of gradient elution, low in leacheate price and good in stability; the prepared negative ion chromatographic column can achieve separation of water negative spikes and a fluorinion base line, and quantitative separation of fluorinion is not influenced; the prepared negative ion chromatographic column is high in efficiency, has excellent separation effects and can simultaneously separate the ten kinds of negative ions including F<->, ClO<2><->, BrO<3><->, Cl<->, NO<2><->, NO<3><->, Br<->, ClO<3><->, H2PO<4><-> and SO<4><2->.

The invention discloses a preparation method and application of an amitraz molecular imprinting monolithic column. The preparation method comprises the following steps: by taking amitraz as a template molecule, dissolving the template molecule into a mixed solution of acetonitrile and dodecyl alcohol, adding a functional monomer, pre-polymerizing at a low temperature, further adding a cross-linking agent and an initiator, introducing nitrogen, filling into a chromatographic column hollow tube of which the lower end is already sealed, sealing the upper end of the chromatographic column hollow tube, and initializing polymerization, thereby obtaining the molecular imprinting monolithic column. After the functional monomer, a pore-foaming agent and the template molecule which are not polymerized are washed off from the column by using a mixed solution of methanol and acetic acid, the molecular imprinting monolithic column which has a good adsorption effect and an enrichment effect on amitraz is obtained. Compared with a conventional body polymerization method, the preparation method has the characteristics that the preparation method is simple and convenient, the aftertreatment is simple, the recognition property is good, the cost is low, required instruments and reaction conditions are easy to achieve, and the like. The molecular imprinting monolithic column prepared by using the preparation method is capable of separating and detecting residual amitraz in foods.

The invention provides an establishment method of a scorzonera fingerprint spectrum. The establishment method comprises the following specific steps: preparing a test solution by scorzonera, and carrying out fractionation detection under a certain condition by a high performance liquid chromatograph to obtain the scorzonera fingerprint spectrum. The invention further provides a scorzonera standard fingerprint spectrum obtained by the method. The standard fingerprint spectrum can provide reliable basis for scorzonera identification and internal mass control. The establishment method is simple and convenient to operate, high in stability, good in reproducibility and multiple in characteristic peaks. By utilizing the establishment method, the quality of scorzonera medicinal materials can be comprehensively and accurately evaluated.

The invention provides a method for detecting the content of EDTA-2Na (Ethylene Diamine Tetraacetic Acid-2Na) in sodium hyaluronate. The method comprises the following steps: firstly, degrading a sodium hyaluronate sample by adopting hyaluronidase, and then determining the content of the EDTA-2Na by adopting a conventional ferric trichloride derivation method through high performance liquid chromatography. According to the method, specific hyaluronidase is screened, so that the viscosity of a high-concentration sample can be effectively reduced, the column pressure is reduced, and test equipment is protected; and meanwhile, the produced product does not influence the detection of a detection target, and the detection sensitivity can be improved. A more accurate method is provided for production and detection of sodium hyaluronate, and the method has important significance in improving the quality of sodium hyaluronate.

The invention provides a method for establishing a fingerprint of leech. The method comprises the following specific steps: preparing the leech into a test solution; and performing separation detection through a high performance liquid chromatograph under certain conditions to obtain the fingerprint of the leech. The invention also provides a standard fingerprint of the leech, which is obtained through the method. The fingerprint can provide a reliable basis for leech identification and internal quality control. The method is simple and convenient to operate, high in stability, high in repeatability and large in quantity of characteristic peaks, and is capable of comprehensively and accurately evaluating the quality of leech medicine.

The invention discloses a liquid chromatography-tandem mass spectrometry detection method for emodin and aloe-emodin in mouse urine, which comprises the following steps of S1, unfreezing the collectedurine, and recovering to room temperature, S2, taking the urine obtained in the step 1, and adding deionized water for mixing, S3, adding an internal standard into the mixed solution, S4, filtering the mixed solution, and S5, taking the filtered mixed solution for determination by a liquid chromatography-mass spectrometer, the liquid chromatography mobile phase being a water-acetonitrile system,the liquid chromatography column being a C18 reversed-phase liquid chromatography column, and the flow velocity of the liquid chromatography column being not greater than 0.5 mL / min. The method has the advantages of high sensitivity, simple operation, high stability and reliable result.

The invention relates to a porous crosslinked polystyrene microsphere which has a surface micropore and internal macropore structure. Particularly, the mean pore size of surface micropores is 18.64-22.82nm, and the mean pore size of internal macropores is 0.75-1.64 micrometers. When the porous crosslinked polystyrene microsphere with the structure serves as chromatographic column filling, the column pressure can be effectively reduced; the internal macropore structure further increases action area between a detected substance and the microsphere; the retention time is prolonged; and substance separation can be better achieved.

The invention relates to the chemical technical field of mesoporous material preparation and analysis, in particular to a hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing and a preparation method thereof. The hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing is characterized in that: hydroxyl connected with silicon atoms on the original hybrid ordered mesoporous silica gel is substituted by aminopropyl. The stuffing has regular and smooth spherical appearance; frameworks of the silicon gel are doped with ethylene radical which has weak hydrophobicity, therefore, the stuffing can not generate silicon gel dissolution phenomenon when being used in flow phase with high aqueous phase proportion and can bear larger pH range (1-11); furthermore, mesoporous pore paths are distributed sequentially, therefore, the mass transfer can be accelerated, and the column pressure is reduced; and the invention is suitable for fast segregation analysis under high aqueous phase proportion.

The invention discloses silicon-based anion exchange resin and a preparation method thereof, and relates to the technical field of anion exchange resin. The resin is obtained by chloromethylation andre-amination reaction of silicon-based white balls, and has a trimethylamine type quaternary ammonium salt functional group; the total exchange capacity of the resin is 0.8-1.0 meq / g; the particle size of the resin is 75-150 [mu]m. The porosity is 47 to 48 percent; the water absorption swelling rate is 0%; the particle size of the obtained resin is consistent with that of silicon dioxide and ranges from 75 micrometers to 150 micrometers. According to the invention, the resin is rich in pore structure, so that the problem that traditional resin is too slow in dynamics is solved, and meanwhilethe problems of too large column pressure, poor resin mechanical performance and the like caused by too high water absorption swelling rate of organic resin are solved.

The invention discloses a surface-modified polystyrene polymer microsphere, a preparation method and an application thereof. It uses polystyrene as the base ball, and the surface contains a brominated benzene ring structure with π-π interaction with fullerene. This structure is obtained by replacing the hydrogen atom on the benzene ring contained in the base ball with a bromine atom. The steps are as follows: : Use monodisperse polystyrene microspheres with a particle size of 10-40 μm as the base ball, mix with the catalyst, add an aliphatic halogenated hydrocarbon solvent, and slowly add a brominating agent dropwise under stirring conditions for substitution reaction; the taken out The microspheres are washed and dried to obtain a polymer microsphere, which is used as a liquid chromatography stationary phase for separating fullerenes whose mobile phase is toluene or o-xylene. The surface-modified polystyrene polymer microspheres provided by the invention only need one step for preparation, are simple in process and easy to repeat, are suitable for large-scale production of fullerenes, and have the characteristics of high separation efficiency and good effect.