50 results about "Electrochromatography" patented technology

The invention relates to methods for isolating an analyte of interest in a sample suspected of containing the analyte of interest using two-dimensional planar electrochromatography. The methods comprise treating at least a portion of the sample with a mobility modifier capable of modifying the mobility of the analyte of interest after the second dimension of planar electrochromatography. Kits and compositions are also disclosed.

The invention provides a polydopamine-assisted method for fixing a covalent organic framework material, and an application thereof. First, a dopamine water solution is prepared; the pH value is regulated to weakly alkaline, and an oxidation treatment is carried out; a carrier with a clean surface is added under room temperature, and the surface of the carrier is modified with a polydopamine coating; the modified carrier is placed in a mixed solution of binary boric acid and 2,3,6,7,10,11-hexahydroxyl triphenyl; one boric acid group is subjected to a reaction with o-phenyldihydroxyl site provided by the polydopamine coating, and another boric acid group participates in COFs framework formation, such that COFs crystal is formed on site and fixed on the surface of the carrier. The preparation process provided by the invention is simple. With the wide adaptability of polydopamine modification, synthesis and fixing of COFs on the surfaces of various substrates can be realized. The method is applied in preparing open tubular electrochromatography columns. Prepared open tubular column based on COF-5 has good separation effect upon electrically neutral benzene-series substances in an electrochromatography mode.

The invention provides a novel reversed phase electrochromatography silica-based monolithic column, that is, an alkylamine silica capillary monolithic column which can realize the separation and the analysis of most of organic compounds containing neutral, acidic and alkaline compounds on the premise of meeting the simple chromatographic conditions. The alkylamine silica capillary monolithic column can effectively improve the symmetry of chromatographic peaks in particular to the alkaline organic compounds. The alkylamine silica capillary monolithic column of the invention comprises a capillary and a fixed phase, in the structural formula of the fixed phase: Si represents the silica capillary monolithic column, R represents normal chain alkyl and R1 represents hydrogen or the normal chain alkyl. The invention further provides a preparation method of the alkylamine silica capillary monolithic column, and the specific synthesis steps are as follows: the silica capillary monolithic column is firstly prepared, then the silica capillary monolithic column containing epoxy is prepared and the alkylamine silica capillary monolithic column is finally obtained by connecting alkylamine. The invention further provides the application of the alkylamine silica capillary monolithic column in neutral, acidic and alkaline organic compounds.

A method for separating a sample comprising a plurality of compounds includes loading a sample onto a planar stationary phase, said sample comprising a plurality of compounds to be separated; and, while retaining the sample on the planar stationary phase, subjecting the sample to planar electrochromatographic separation in a selected direction using a first mobile phase; and subjecting the sample to a chromatographically-based separation in a direction other than that of the direction used for planar electrochromatographic separation using a second mobile phase. Separation is optionally followed by direct detection of analytes using mass spectrometry (MS). These three dimensions of separation are orthogonal to one another, providing for improved resolution of the analytes.

The invention discloses a method for preparing an electrochromatography monolithic column of silicon dioxide-titanium dioxide monolithic materials, as well as application thereof. The titanium dioxide-silicon dioxide forms a mesopore molecular sieve under the action of a supramolecular template of which the mechanical strength is good, and pore diameter is easy to control according to requirement. A uniform capillary electrochromatography column with high specific surface area is prepared by one-step method. The method has the advantages that the mesopore molecular sieve which is prepared by using the supramolecular template as a structure-directing agent and has a specific pore structure, extremely high specific surface area and uniform adjustable pore diameter has the advantages of simple preparation method, good repeatability and high separation efficiency, and is suitable for the separation and enrichment of phosphorylated polypeptide, wherein titanium dioxide and silicon dioxide molecules are combined with silicon hydroxyl on the surface of the inner wall of a capillary through chemical bonds; a framework structure and the pore diameter of nanometer pores can be conveniently controlled by changing the categories and proportion of the supramolecular template; and surface properties and the chemical environment of a pore cavity are regulated so as to provide a specific molecular field.

The invention provides a raw material formula of the anti-phase ion exchange electricity chromatographic column: ionic compound monomer; neutral compound monomer; initiator; the hole-making. According to the above raw material formula, the neutral compound monomer and the ionic compound monomer carries on the polyreaction in the capillary vessel, joins the hole-making and the initiator in the polyreaction, then prepares the anti-pjase ion exchange electricity chromatographic column. The invention has solved the mutual solubility question which between the ionic compound monomer and the neutral monomer, may satisfies the continuously sharp separation request of the neutrality, acidity and alkaline matter; the pillar has good insightful performance, is suitable to the high concentrated buffer salt system; when preparing, no longer need to burn the plug on the two ends of the pillar, also has avoided the difficulty of filling up the pillar.

The invention discloses a combination press capillary tube electrochromatography equipment, it is composed of the sequential linked high pressure pump, mixing valve, injection valve, capillary chromatographic column, detector and high voltage power pack parallel connect with capillary chromatographic column and supplies high voltage for capillary chromatographic column, much more it includes diverter and electric insulator, this invention makes to control the sample volume, increase the flexibility of the system, has promoting and optimizing effect for establishing analysis method.

The invention relates to a method for producing electrolytic manganese metal. The method comprises the following steps: respectively ball-milling high-phosphorus high-iron manganese ore and iron pyrite into powder, and mixing the powder according to a proportion for sulfating roasting; leaching the mixture treated by means of sulfating roasting with water as a leaching agent to obtain manganese sulfate solution; removing impurities from the manganese sulfate solution to obtain manganese sulfate electrolyte; adding an electrolysis additive into the manganese sulfate electrolyte, and simultaneously adding an ammonium salt as a buffering agent into the solution; putting the electrolyte into an electrolytic cell, providing direct current and keeping the temperature constant to play an electrochromatography effect so as to separate out manganese metal on a cathode; passivating, water-washing, drying and removing the manganese metal that is separated out, and thus obtaining an electrolytic manganese metal product. The method disclosed by the invention has a short technological process, low energy consumption and small environmental pollution, so the method is suitable for development and application of high-iron high-phosphorus lean manganese ores and the like.

The invention relates to a sample injection method of a micro fluidic chip system, in particular to a large-volume sample injection method and a special chip adopted in a micro fluidic chip, wherein, two or more than two shunt channels are arranged between a chip separation channel and a mobile phase inlet inside a micro fluidic chip system adopting fixed stationary phase; large-volume sample injection of the micro fluidic chip system is realized through controlling the switching and cutoff of the fluid inside the system. The method is suitable for large-volume sample injection inside a micro fluidic chip in electrochromatography mode, compression electrochromatography mode and liquid phase chromatogram. Moreover, the method has the advantages that: sample injection of large-volume sample inside a micro fluidic chip can be realized; the invention overcomes the gradient delay effect of the system, and is particularly suitable for gradient separation; moreover, the invention has the characteristics of simple strucuture, convenient operation, small dead volume, small pre-column effect and good sample injection repeatability, etc.

The invention discloses an iminazole type ionic liquid reversed phase electrochromatography organic monolithic column. A monolithic stationary phase is a porous continuous bed formed by in situ polymerization of neutral compound and ionic compound monomer; the neutral compound is methacrylic acid dodecyl ester and dimethyl crylic acid ethyl diester, the ionic compound monomer is 1-allyl-3-methylimidazole phosphate ionic liquid, the pore-forming agent is one or more of methyl alcohol, methylbenzene, normal propyl alcohol, cyclohexanol, capryl alcohol, 1,4-butanediol and ethylene glycol, and the initiator is azodiisobutyronitrile. The iminazole type ionic liquid reversed phase electrochromatography organic monolithic column provided by the invention not only has typical reversed phase chromatographic performance, but also can provide ion exchange groups and generate higher electroosmotic flow, change polymerization quantity of ionic liquid and change the size of the electroosmotic flow. The stationary phase of the monolithic column can meet the requirement on rapid separation of polar compound, neutral compound and alkali compound.

The invention relates to a preparative electrochromatogram separation device, belonging to the field of process and separation technique of biological product. The device is a triple chamber rectangle electro chromatographic column, which comprises a gel chamber loaded with filler in the middle and electrode chambers at double- side, the gel chamber 8 being a hollow plexiglass body with symmetrical trenches at the double sides and the middle being rectangle; the trench being equipped with diaphragm 3 which can intercept the molecular of a molecular weight more than 1000 Dalton and can let conductive ion transit freely; two electrode chambers 9 which is equipped with inert platinum electrodes 5 being at double- outside of gel chamber; and the electrode chambers 9 and gel chamber 8 being loaded with acetate, phosphonate, hydrogen carbonate or trishydroxymethylaminomethane- hydrochloric acid solution. The device invented is characterized in that the separating power is strong, the handling capacity is large, the applicability extensive, and it has an extensive application prospect in separating and purifying the biomacromolecule such as protein and nucleic acid.

The invention discloses a preparation method and application of chiral bonded capillary electrochromatography open tubular column, which belongs to the technical field of the preparation of capillaryelectrochromatographic columns. By utilizing a special structure and molecular characteristics of beta-cyclodextrin, a derivative with an isocyanate group is designed and bonded with the inner wall ofan amination capillary tube, and a chiral capillary electrochromatogrpahy open tubular column which meets the electrochromatography separation requirement and is simple in method and good in reproducibility and stability is prepared. A stationary phase is firmly bonded onto the inner wall of the capillary tube by virtue of a chemical bond, and compared with the coated stationary phase, the mechanical strength and the stability are better.

The invention relates to a process of preparing chromatographic fixed phase using functional coupling agent by means of secondset reaction, which comprises three steps: (1) preparing gamma-amino propyl bonding silica gel prosoma; (2) adding excess chlorinated sulfoxide into emodic acid for ereaction under regurgitation condition for 2 hours, vacuum boiling left chlorinated sulfoxide and getting emodic acid chloride; (3) proceeding reaction under regurgitation and stirring condition with protective nitrogen for 10 hours with prosoma and emodic acid chloride, taking waterless toluene as disslovant and triethylamine as catalyst; extracting, washing, floating and fdrying solid and preparing emodic acid bonding silica gel fixed phase. The invention is chartacterized by simple process, low production cost, high concentration of bonded ligand on surface of said fixed phase, and hardness for bacteria growth because of antibiotic action of emodic acid. The emodic acid bonded silica gel fixed phase is suitable for high efficiency liquid chromatography, microcylinder liquid chromatography and electrochromatography analysis and separation. It can also suit to be used as relative enriched material.

The invention discloses an overall chiral stationary phase of silica gel capillary and a preparation method thereof. The preparation method is characterized by comprising the following steps: preparing a novel chiral group maleopimaric acid through reaction of natural chiral rosin and maleic anhydride, and synthesizing the novel chiral group maleopimaric acid onto a carrier through chemical bonds with propyl amine as a connecting unit of the novel chiral group and an overall column carrier of a silica gel-based capillary. The invention is applicable to the stationary phase of electrochromatography or liquid-phase chromatography of the capillary. Moreover, the invention has the advantages that: the cost of the prepared chiral stationary phase is low, the column efficiency is high, the scope of application is wide for various mobile phases, the manufacture is simple and rapid, and the commercial production can be realized.

The invention discloses a stationary phase of HILLIC (hydrophilic interaction chromatography) and a preparation method of the stationary phase. The stationary phase of the HILLIC refers to a monolithic silica column with polyvinyl pyrrolidone bonded on the surface of porous silica gel or a monolithic capillary column with polyvinyl pyrrolidone directly bonded on the inner wall of a capillary; the monolithic capillary column comprises a capillary liquid chromatography monolithic column and a monolithic electrochromatography monolithic column. Experiments prove that the stationary phase of the HILLIC has a typical retention mechanism of hydrophilic interaction chromatography, effective separation of a series of polar compounds can be realized, efficient separation of the polar compounds can be realized without a buffer salt mobile phase, reproducibility is good, and electrochromatography column efficiency can be up to 200000 plates / m. Besides, preparation conditions of the stationary phase of the HILLIC are easy to control, raw materials are cheap and available, a preparation process is simple, and industrialization is easy to realize.

The invention discloses an MBA bridged cyclodextrin functionalized chiral monolithic column and preparation and application thereof, and belongs to the field of analytical chemistry. According to theMBA bridged cyclodextrin functionalized chiral monolithic column, a cyclodextrin SH-beta-CD and a ligand derivatizing agent MBA are first dissolved in deionized water, a bridged cyclodextrin is formedby a reaction under the condition of AIBA as an initiator, then a nucleophilic reagent urea and a protonation reagent formaldehyde solution are added, and the MBA bridged cyclodextrin functionalizedchiral monolithic column is prepared by one-step polymerization under the action of the catalyst urea. A method for preparing the MBA bridged cyclodextrin functionalized chiral monolithic column is simple, the reaction is fast, a cyclodextrin bimolecular bridged structure constructed through a functional bridge can fully exert the synergistic effect between every two molecules and a bridge chain,the chiral recognition ability of a stationary phase is significantly enhanced, the MBA bridged cyclodextrin functionalized chiral monolithic column is enabled to show excellent resolution ability todifferent types of chiral drugs such as amino acid and metoprolol tartrate in electrochromatography, and thus the MBA bridged cyclodextrin functionalized chiral monolithic column can be used in the field of chiral resolution of the drugs.

The invention relates to the field of preparation of liquid chromatography capillary monolithic columns, in particular to a novel bifunctional group mixed mode organic polymer monolithic column and apreparation method and application thereof, wherein the polymer monolithic column is formed by copolymerization of a bifunctional group monomer and an inner wall vinylation modified capillary tube ina capillary tube; one functional group monomer is N,N,N-trimethylvinylbenzenemethylammonium chloride with extremely strong hydrophilicity and pi-pi interaction, while the other functional group monomer is 4-vinylbiphenyl with excellent reverse chromatography retention performance; the vinylation modified solution is a solution taking methacryloyloxypropyltriethoxysilane as a solute and methanol asa solvent. The organic polymer electrochromatography monolithic column has the advantages of rich porous structure, good permeability, reverse phase and hydrophilic chromatographic separation performances, and realization of the separation of a plurality of substances in different chromatographic modes, high application values. The invention provides a new idea for the development of the novel mixed mode organic polymer electrochromatography monolithic column.

The invention discloses an electrical isolation device. The electrical isolation device comprises a support, a solution cavity filled with buffer solution and a capillary tube, wherein a capillary tube slot is formed in the support, the solution cavity is formed in the support, one end of the solution cavity is open, the other end of the solution cavity is closed, an electrode is arranged at the opening, a through hole is also formed in the closed end, one end of the capillary tube is inserted into the capillary tube and passes through from the solution cavity by virtue of the through hole, and the through hole is sealed by arranging a sealing ring. The invention also discloses a manufacturing method of the electrical isolation device. The electrical isolation device and the manufacturing method thereof can be successfully applied to electric separation instruments such as capillary electrophoresis and electrochromatography and have a special power up use; by adopting a rusting method, a porous structure can be formed on the surface of the capillary tube, electricity can be conveniently introduced into a capillary tube separation channel, the defects of tedious process, short life and the like of the traditional manufacturing method are avoided, the manufacturing method disclosed by the invention is simple and stable, and life is long; and the electrical isolation device has the potential to be applied to analysis separation of a more complex sample.

The invention relates to a preparation method for a grapheme open-tube electric chromatographic column, and relates to the preparation method for a novel capillary electric chromatographic column. In the method, a conductive polymer polyaniline assisted polydopamine bonded graphite oxide is used as a fixed phase. The conductive polymer polyaniline is bonded to the inner wall of a capillary to serve as an underlying material, so that the specific surface area of the capillary is increased, the modification time and the modification frequency of dopamine are remarkably reduced, and the modification degree of the polydopamine is improved; and therefore, the reaction of the graphite oxide is facilitated. The preparation method is easy to operate and low in cost; the overall preparation process is performed in aqueous solution, and an organic solvent or a toxic reagent is not used; the environment is not polluted; each prepared coating has the high stability; the service life of the capillary column is long; according to the grapheme open-tube electric chromatographic column prepared by using the preparation method, the chromatographic performance of the grapheme open-tube column is remarkably improved, and the effect on separating the homologs of benzene is better compared with that of a polydopamine bonded graphite oxide open-tube.

The invention discloses a method for continuously separating synthetic pigments in multiple modes with pCEC (pressurized capillary electrochromatography). According to the method, a multi-mode capillary separating column is adopted, and a high-voltage electric field and liquid-phase high voltage are applied to the separating column simultaneously, so that the synthetic pigments are firstly subjected to first-dimension pressurized capillary electrophoresis separation in a hollow capillary area with the inner surface exposed and are continuously transferred to a capillary chromatographic column area filled with chromatography filler for second-dimension pCEC separation, and electrophoresis-electrochromatography multimode continuous separation of multiple components on the same separation column is realized; the multimode capillary separation column is seamlessly and continuously constituted by a section of quartz capillary with the inner wall exposed and a section of capillary chromatographic column. Multiple functions of multimode continuous chromatography, pressurized electrophoresis, pCEC separation and the like are comprehensively applied, the procedure is continuous, and the separation efficiency is high.

The invention discloses an integrated sol-gel matrix capillary column and a preparation method thereof. The preparation method comprises the steps: filling 10cm polymerized solution into alkenylation capillary, and then microwave-polymerizing for 14.5min at 80 DEG C and 700W. According to the invention, the integrated sol-gel matrix capillary column is in-situ prepared in the capillary through a temperature-controlling microwave synthesizer. The prepared integrated column is subjected to chromatography performance evaluation under a pressurizing electrochromatography (P-CEC) separating mode; the four matters of thiourea, naphthalene, methylbenzene and biphenyl are subjected to baseline separation; the lowest theoretical plate height of naphthalene can reach 1.83 mu m; compared with an experimental result of a common microwave method, the result is that the theoretical plate quantity of naphthalene is increased to 54749 / m from 10000 / m and the separation column effect of the compound is greatly increased. A scanning electron microscope result shows that the integrated materials in the tube of the integrated sol-gel matrix capillary column prepared through the temperature-controlling microwave method are uniformly distributed and are tightly combined with the inner wall of the capillary.

The invention discloses an efficient microflow electrochromatography separation method of a plant growth regulator containing carboxyl. Based on an inverse-phase capillary column, a compound containing a nucleophilic group is used as moving phase electrolyte to dynamically modify a reversed-phase column filler so as to form a nucleophilic base separation column; a high-voltage electric field and a micro-flow liquid phase analysis mode are applied to the columns to efficiently separate the plant growth regulator containing carboxyl. The method is characterized in that comprehensive functions of electro-osmotic flow, electrophoresis and polar chromatography are easy to achieve, and capillary electrophoresis separation of the polar carboxyl plant growth regulator and absorption chromatography separation of the nucleophilic group are realized.

The present invention provides an acrylate polymer capillary electrochromatography column decorated by macrocyclic polyamine and its preparing method, the column of acrylate polymer organic polymer decorated by macrocyclic polyamine is prepared by free radical polymerization and method of column back decoration, the whole surface of the acrylate polymer in the electrochromatography column is linked with a macrocyclic polyamine, the macrocyclic polyamine is 1, 4, 10, 13, 16-quinquevalent nitrogen trinuclear heneicosane-9, 17-diketone. The preparing method of acrylate polymer capillary electrochromatography column decorated by macrocyclic polyamine is simple, having better reproduction quality, the capillary electrochromatography column has a better separating effect to inorganic anions, benzenediol isomer, benzoic acid derivatives and ribonucleotide, having better application in the separating aspect for complicated component material.

The invention discloses an electrochromatography device, which comprises an infusion system, a shunting system, a quantitative sampling system, a current circuit system, a chromatographic separation system, a temperature control system, a detector, a data processing system and a liquid waste pool, wherein the infusion system is introduced on the basis of reserving the advantages of a traditional separate analysis device and the work which cannot be done by a traditional electrophoresis instrument can be done; the quantitative sampling system is introduced and the problems of cross contamination, poor quantitative reproducibility and the like of a traditional electrophoresis apparatus are solved; the current circuit system is introduced and the multi-mode separate mode can be achieved by only one set of device; a novel chromatographic separation system (open tube-type chromatographic column) is introduced, the whole device has the selectivity of a high-performance liquid chromatographic instrument and is a potential separate analysis device while the problems that a traditional packed column is difficult to prepare, easy to block, short in service life and high in cost are solved; and the electrochromatography device is stable, reliable and simple in operation, and is expected to be popularized and applied to multiple frontier domains of biological medicines, environment analysis, bioscience and the like.

The microflow pump is composed of liquid phase pump in high pressure and cascaded columns with thin internal diameter (less than 2 mm) with pad being filled for providing sheath flow liquid for capillary electrophoresis / electrochromatography and mass spectrum combination instrument. The invention lowers cost of electrophoresis / electrochromatography and mass spectrum combination instrument, increases adaptability of experimentation as well as possessing wider suitable range and it is apt to expand the application.

The invention discloses a preparation method and application of a polar bridging cyclodextrin chiral monolithic column, and belongs to the field of analytical chemistry. The monolithic column is prepared by the following steps: dissolving cyclodextrin with N, N-(1, 2-dihydroxyethylene) diacrylamide DAA in deionized water, reacting under the condition of an initiator AIBA to generate polar bridgingcyclodextrin, adding urea and formaldehyde, and quickly preparing the polar bridging cyclodextrin chiral monolithic column within 30 minutes by virtue of a one-pot thermal polycondensation method. The preparation method is simple and rapid in reaction, a cyclodextrin bimolecular bridging structure is constructed by adopting a bridging agent with high polarity; the additional hydrophilic interaction can be provided, the chiral recognition ability of the stationary phase can be significantly enhanced, the excellent resolution ability on a variety of amino acids, RS-(+)-(4-methoxybenzene) ethylamine and other different types of drugs can be displayed in the electrochromatography, and the method can be used as the chromatographic chiral fixation so as to be correspondingly used in the field of drug chiral resolution.

The invention discloses an electrochromatography device, which comprises an infusion system, a shunting system, a quantitative sampling system, a current circuit system, a chromatographic separation system, a temperature control system, a detector, a data processing system and a liquid waste pool, wherein the infusion system is introduced on the basis of reserving the advantages of a traditional separate analysis device and the work which cannot be done by a traditional electrophoresis instrument can be done; the quantitative sampling system is introduced and the problems of cross contamination, poor quantitative reproducibility and the like of a traditional electrophoresis apparatus are solved; the current circuit system is introduced and the multi-mode separate mode can be achieved by only one set of device; a novel chromatographic separation system (open tube-type chromatographic column) is introduced, the whole device has the selectivity of a high-performance liquid chromatographic instrument and is a potential separate analysis device while the problems that a traditional packed column is difficult to prepare, easy to block, short in service life and high in cost are solved; and the electrochromatography device is stable, reliable and simple in operation, and is expected to be popularized and applied to multiple frontier domains of biological medicines, environment analysis, bioscience and the like.

The invention relates to a high-efficiency microflow electrochromatography similarity analysis method and an influence degree calculating method. The method comprises the following steps: aligning peaks on different atlas by an aligning step, and calculating the peaks by a similarity equation to obtain a similarity value of each detection substance in relative chromatogram, according to the value, determining that whether a substance to-be-detected and a standard sample belong the same substance or not. And finally, calculating influence degree of peaks in similarity calculation by using an influence degree equation. According to the method, whether the substance to-be-detected and the standard sample belong the same substance or not can be effectively compared, and the influence degree of peaks the same substance to be detected in similarity calculation can be obtained, so that high-efficiency microflow electrochromatography analysis and sample identification capability can be increased.

The disclosed electrokinetic current full analysis system comprises: an electro osmosis pump injection unit, an enrichment function unit, a micro-column separation detecting unit, a fiber spectrograph, a dc high-voltage stabilized power, and a microcomputer; both electro osmosis pump and electrokinetic for transport and separation; solenoid switch valve to control current direction ; both quartz tube electrophoresis and electrochromatography column filled with fine sand as heat-conducting medium to reduce current channel section.This invention has field micro-column electrophoresis / chromatogram / electrochromatography function with high sensitivity and simple structure.