355results about How to "High column efficiency" patented technology

The invention relates to a preparation method of covalent organic framework composite microspheres with core-shell structures. The method comprises the following steps: dissolving silicon dioxide microspheres, a first construction element and a second construction element in an organic solvent; and after adding a catalyst, rapidly synthesizing into the composite microspheres with core-shell structures at a certain temperature. In a preparation process, reaction conditions are gentle, the method is simple, and the yield is high; the prepared covalent organic framework composite microspheres have the advantages of good core-shell morphology, high specific surface area, ordered pore structures, good mechanical stability, thermal stability, chemical stability and the like, if the microspheres are used as a chromatographic stationary phase, the chromatographic mass transfer resistance can be reduced effectively, the theoretical plate height is improved, and finally, column efficiency and degree of separation are improved; and if the microspheres are used as solid-phase extracting filler, the enrichment effect can be improved remarkably. The covalent organic framework composite microspheres with core-shell structures have good application prospects in the aspect of separation and enrichment of small organic molecules.

This invention publishes a kind of gas phase chromatography method which can measure the air content and the specific gas in the insulating oil with just once sampling. This invention uses Ar as carrier gas. It also uses the packed column sample entrance. What is more, it has six-way value color-spectrum-switching column, heat transmission detector and the H-fire ionization detector. During the process, Ar is divided into 2 parts. One part will directly go out after it goes through the heat transmission detector's reference arm 6, while the other part will go by steps through the sample entrance 1, the first color spectrum column 2, the six-way value 4, the second color spectrum column or gas lock 3, the heat transmission detector 7, the Ni catalysis CH4 converter 8 with H2, and at last the H fire ionization detector 9 with the air. Then it will go out. During the only one sampling, the invention can meanwhile measure the air content and analyze the accident specific gas in the simple oil. To sum up, it operates easily, needs little work and can decrease the analysis error relatively. So it can do the work of analyzing the sample oil which has low degassing ratio well, as it can satisfactorily separate all the groups.

The invention relates to a method for producing crocin with higher than 95% purity from gardenia. The invention adopts a normal-temperature water-percolation extraction process, can effectively reduce the extraction of pectins, proteins and other impurities, and avoids difficulty in the subsequent separation and purification. Before extraction, seed crushing is avoided in the gardenia fruit pulverizing process, thereby reducing the extraction of oil. Water extract microfiltration can remove solid particles, pectins and other impurities in the water extract and filter out bacteria and other microbes, and the microfiltered water extract can be directly continuously adsorbed by a macroporous resin column. Fine macroporous resin is used instead of conventional large-particle-diameter macroporous resin for adsorption chromatography, normal pressure technology is upgraded to pressurization technology, and a continuous circulation chromatography method is used instead of the traditional linear chromatography method, thereby enhancing the column efficiency and chromatography efficiency; and in cooperation with the refinement of the C18 column, the pure crocin can be directly prepared. The whole technological process is simple, has the advantages of solvent saving, low cost, high efficiency and environmental protection, and is suitable for industrial production of the crocin product of which the purity is higher than 95%.

The invention relates to a preparation of cyclodextrin bonded stationary phase, in particular to a method which prepares bonding-typed cyclodextrin stationary phase by adopting click chemistry reaction; the preparation method comprises two steps: an azid group or alkyne group is led in the surface of silica gel by a silane coupling agent to prepare azide group silica gel derivatives or alkyne group silica gel derivatives; a 1, 3-ring addition reaction of the azid group and the alkyne group which is also the click chemistry is then carried out for 24-72 hours under the temperature of 20-80 DEG C; the cyclodextrin where the alkyne group or azid group is decorated is bonded onto the surface of the silica gel. The bonding reaction provided by the invention has high selectivity, can excellently keeps the structure of the cyclodextrin, and has simple preparation method and wide applicable range; the prepared cyclodextrin bonded stationary phase has high surface bonding quantity, which is suitable for being used for high-effect liquid phase chromatography separation material and is especially applicable for separating strong polar compounds under the mode of hydrophilic liquid phase chromatography.

The present invention relates to a method for separating biological macromolecular component by using two-dimensional or multidimensional capillary electrophoresis and its interface. The biological macromolecular component undergone the process of one-dimensional capillary electrophoresis separation can be passed through the interface and fed into two-dimensional capillary electrophoretic separation operation to implement two-dimensional capillary electrophoresis, the small molecular substance can be diffused and freely permeated through the hollow fibre in the interface and can obtain balance in it, and when the described biological macromolecular component is flowed through the interface, the buffer solution containing low molecular substance can be on-line added / removed into the hollowfibre in the interface.

The invention discloses polar liquid chromatogram filler comprising double amido bonds. The chemical structural formula of the filer is shown in the specification, in which R1 is C1-20 alkyl, R2 is C1-8 alkyl or phenyl, a is 0, 1, 2, and X is halogen, alkoxyl, acyloxyl or amido. The filler provided by the invention can form a hydrogen bond or an ion pair with residual silicon hydroxyl on a silica-gel substrate by means of a novel polar double amido bond functional group as a silica-gel surface bonded phase, so that the activity of silicon hydroxyl is better shielded and the influence of residual silicon hydroxyl is eliminated. Compared with conventional C18 chromatographic column, the novel chromatographic fixed phases have more excellent selectivity and separation degree, so that the filler is high in column efficiency and wide in application range.

A high-efficiency cone-shaped preparation column for liquid chromatography is composed of head body and tail of column with inside diameter of head inlet larger than inside diameter of tail outlet. Cone-shaped liquid flow guide channel, distribution disk and sieve plate constitute the liquid flow distributing system located on the head of the column. The distribution disk consists of multiple radial liquid flow channels concentric liquid collecting channel and liquid exuding holes. Inside diameter of the inlet is 2R=10mm-2000mm and inside diameter of the outlet is 2r=3mm-1800mm, the length ofthe column is L=5cm-100cm. Angle of cone is is in range of 1-20 degrees. Various chromatographic separation media can be filled into the cone. The ivnented cone-shaped preparation column can increasecolumn efficiency and specimen loading and its diluting effect of separated components is lower than that of cylindrical chromatographic column.

The invention discloses a method for establishing a lonicerae and forsythiae powder UPLC fingerprint spectrum.The method can quickly and accurately identify authenticity and merits of a product and has the advantages of simplicity, convenience, stability, high precision, good repeatability and the like.By means of the method, kinds and quantity of chemical components contained in lonicerae and forsythiae powder can be comprehensively reflected, global description and evaluation are conducted on the quality of the lonicerae and forsythiae powder, the quality and the medicine effects of the lonicerae and forsythiae powder are truly combined, which is conductive to illuminating the function mechanism of the lonicerae and forsythiae powder, and a basis is provided for technical promotion and deep development of the lonicerae and forsythiae powder.By means of the method, the number of the chemical components detected in the lonicerae and forsythiae powder fingerprint spectrum is relatively large, characteristic peak height proportions are moderate, a base line is stable, and the separation degree, peak shapes and column efficiency are good.

A method for synthesis of linking polysaccharide chiral stationary phase, includes the following steps: 1) in the reactor with organic solvent, polysaccharide and derivative solvent of polysaccharide react with including functional group which can react with polysaccharide hydrocarbon radical, then though centrifugal separation the solid substance is collected; 2) coat the prepared polysaccharide derivative containing trihydroxyme or on the surface of silica gel matrixof chromatogram filler, then they are mixed with toluene and pyridine in reactor , cooled after reaction, then use tetrahydrofuran and carbinol separately to wash the creature, which are dried in vacuum, acquiring the linking polysaccharide chiral stationary phase. Its advantages are: wide field of use, simple and rapid preparation.

The invention relates to a novel core-shell structure silica gel chromatographic packing material suitable for super rapid separation, preparation and application of the core-shell structure silica gel chromatographic packing material. A silica gel microsphere synthesized from the novel core-shell structure silica gel chromatographic packing material has a clear core-shell structure, a core is pore-free silica gels, and mesopores exist on a shell layer. The preparation method comprises the steps of 1. synthesizing pore-free silica gels with different particle sizes by adopting a program temperature control manner, wherein the pore-free silica gels are good in monodispersity and narrower in particle size distribution; 2. selecting multiple cationic surface active agents from an ammonia water solution and selecting organic amine or long-chain alkane as a reaming additive, preparing a mesopore shell layer the thickness of which can be adjusted on the pore-free silica gels, controlling the thickness to be within a range of 100-360nm; and 3. performing chambering optimization on the pore diameter of the mesopore shell layer, respectively adjusting the pore diameter to be 9nm, 15nm or more according to the requirement of separating samples, and finally, performing derivatization on the silica gel microsphere to prepare a chromatographic stationary phase. The novel core-shell structure silica gel chromatographic packing material is applied to rapid separation, with a column efficiency being above two hundred thousand, and polypeptide and integral protein samples can be rapidly and efficiently separated in a short time.

The invention discloses a preparation method of an alkali-resistant silica gel chromatographic column filling material. The preparation method provided by the invention comprises the following steps of preparing a silica gel matrix of which the surface has alkali resistance by a short-carbon chain silane coupling agent-based silica gel surface organic hybridization method, and carrying out stationary phase bonding. The preparation method is characterized in that a part of silanol groups on a totally porous spherical silica gel surface undergo bonding reactions in the presence of a short-carbon chain silane coupling agent so that the totally porous spherical silica gel surface is covered partly with short carbon chains, and thus organic hybridization of the totally porous spherical silica gel surface is realized and alkali-resistant silica gel having a thin and uniform organic covering layer is obtained; and through surface stationary phase bonding and last end-capping, the alkali-resistant silica gel chromatographic column filling material is obtained. The alkali-resistant silica gel chromatographic column filling material obtained by the preparation method has good alkali resistance, reduces a residual silanol effect, covers metal impurities on a silica gel surface, and has good application potentials.

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 discloses a method for purifying lysostaphin by antibody affinity chromatography, comprising the following steps of: (1) cleaning and eluting an antibody sample containing lysostaphin by passing the antibody sample through a chromatographic column which is filled with protein A resin and is balanced by buffer liquid A; collecting and drying by freezing eluting peak; (2) mixing the freeze-dried product with an affinity chromatography medium to form an immunized affinity chromatography medium; (3) making the lysostaphin sample pass through the chromatography column which is filled with immunoaffinity chromatography medium and is previously balanced with the buffer liquid A; then cleaning the sampled immunoaffinity chromatography column with the buffer liquid A; and eluting the lysostaphin from the chromatography column with a buffer liquid C; and collecting the eluting peak. The method has the advantages of rapid processing speed, high recycling rate and good repeatability, long column efficiency and basically invariable joint efficiency, along with a recycling rate of an active protein of between 85 and 95 percent, a specific activity of more than 1000 U / mg, a multiple of protein purification of more than between 3 and 5 times, and a purity of between 95 and 98 percent.

The invention discloses an extraction method of bovine tendon collagens. The method comprises the steps of pretreatment, extraction, precipitation, salting-out, purification, drying, and collagen preservation. The extraction method of bovine tendon collagens allows type I collagens to be separated and purified from yak tendons through using enzymatic hydrolysis and high performance liquid chromatography preparation, and has the advantages of high efficiency, high selectivity and easiness in amplification.

The invention discloses a method for separating camptothecin and 10-hydroxycamptothecin by the adoption of rosin-based macromolecules. According to the method, alpha-methacrylic acid (or methyl methacrylate) is used as a monomer, maleated rosin-[(2-acryloyloxy) ethyl] ester is used as a cross-linking agent, and an micro-suspension free radical polymerization method is adopted to prepare rosin-based macromolecule microspheres, wherein the microspheres are a spherical porous material, the article size distribution of the rosin-based macromolecule microspheres is 3-10 microns, the average pore size of the rosin-based macromolecule microspheres is 10-15 nm, the specific surface area of the rosin-based macromolecule microspheres is 90-120 m<2> / g, and the acid value of the rosin-based macromolecule microspheres is 50-150 mgKOH / g; wet column packing is conducted on the rosin-based macromolecule microspheres by the adoption of a column packing machine, so that a chromatographic column is prepared; HPLC separation is conducted on the camptothecin and the 10-hydroxycamptothecin, wherein the detecting wave length is 230-290 nm, the temperature is 30+ / -10 DEG C, the flow speed is 0.3-1.0 mL / min, and the separation degree of the camptothecin and the 10-hydroxycamptothecin is 1.80-2.15. By the adoption of the method for separating the camptothecin and the 10-hydroxycamptothecin by the adoption of the rosin-based macromolecules, a high separation degree of the camptothecin and the 10-hydroxycamptothecin is achieved, the selectivity is high, the method is high in sensitivity, easy to operate, rapid and efficient, and no secondary pollution to medicine, health care products and food is caused.

The invention discloses a method for separating and assaying impurities in apremilast and preparations thereof through liquid chromatography. In the method, octadecylsilane chemically bonded silica is employed as a filler in a chromatography column; a buffer solution is employed as a mobile phase A; and a methanol-acetonitrile mixture solvent is employed as a mobile phase B, wherein a gradient elution method is employed in the mobile phases to assay the impurities in apremilast and the preparations thereof. The method can effectively separate and assay unknown impurities and known impurities from the apremilast. The method has strong specificity, is high in accuracy, is easy to use and can be used for effectively control the quality of the apremilast and preparations thereof.

The invention discloses an establishment method for a UPLC fingerprint spectrum of a gynecological reconstruction pill. According to the method, the authenticity and merits of the product can be quickly and accurately identified, and the advantages of being easy and convenient to use, stable, high in precision, good in reproducibility and the like are achieved; in addition, the variety and number of chemical components contained in the gynecological reconstruction pill can be comprehensively reflected, then the quality of the gynecological reconstruction pill is integrally described and evaluated, therefore, the quality and the medicine effect of the gynecological reconstruction pill can be truly combined together, illumination of the action mechanism is promoted, and a basis is provided for technology improvement and deep development of the gynecological reconstruction pill. Furthermore, the fingerprint spectrum, detected through the method, of the gynecological reconstruction pill contains relatively more chemical components and is moderate in height proportion of all characteristic peaks, stable in base line and good in separation degree, peak shape and column efficiency.

A method for splitting a Bepotastine Besilate optical isomer and quantitatively measuring R-isomer impurity is disclosed. According to the invention, high performance liquid chromatography is adopted. A mobile phase contains n-hexane and ethanol. The method is characterized in that normal-phase liquid chromatography is adopted; packing used in a chromatographic column is silica gel with its surface coated with amylase-tris-(3,5-xylyl carbamate); and the mobile phase also contains an alkaline additive. In comparison with the prior art, the method provided by the invention has advantages as follows: the mobile phase is simple to prepare, and resolutions of two isomers are both within 4.5-5.5. Especially, the chromatographic column of the method has good durability, and the chromatographic column still has high column efficiency after having been used for one year. Thus, analytic determination cost is greatly reduced.

The invention relates to a method for packing a separation column and a nozzle needle integrated capillary column and manufacturing a stopper, which comprises the following steps: preparing a chromatography packing into a homogenate with a certain concentration; reversely pressing the homogenate into the capillary column to pack by nitrogen under a certain pressure, wherein one end of the capillary column is a tapered taper; sintering the chromatography packing at the mouth of the taper to form the stopper; and during the process of sintering, using a stainless steel tube to control the lengthof the stopper and protect the chromatography packing at the back of the stopper. The method for packing the separation column and the nozzle needle integrated capillary column and manufacturing thestopper is simple and fast to operate without special equipment and high in success ratio. The capillary column packed according to the method has high separation efficiency and good separation reproducibility; and the stopper manufactured according to the invention has small volume, no sample adsorption and no post-column effect. The method for packing the separation column and the nozzle needleintegrated capillary column and manufacturing the stopper has very good application value in the fields of protein sciences, micro environments and biological sample analyses based on capillary liquidchromatography-electrospray ionization mass spectrometry technology.

The invention relates to a method for providing an aseptic chromatography column, said method comprising the steps of:pre-sterilize an empty chromatography column;pre-sterilize a chromatography medium;introducing the pre-sterilized chromatography medium into the pre-sterilized chromatography column using aseptic equipment, thereby providing an aseptic chromatography column comprising chromatography medium.

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.

The invention relates to the capillary electrophoresis method in stereo multiple dimensions and multiple modes as well as its special equipment. Switching voltage makes the mobile phase be switched between different flow paths. The sample components are separated into at least two capillary columns by using different separation modes of the capillary electrophoresis through flow paths in forms of series connection, parallel connection or their combination. The special equipment is mainly composed of at least two caillary columns, at least one connecting piece and high voltage source. The connecting piece transports the samples between columns. The container containing flow path is installed on the capillary columns or the free end of the vacant capillary.

The present invention provides a bisamide-containing novel liquid chromatographic media and method of synthesizing the same. A novel polar bisamide functional group, which can form hydrogen bonds or ion pairs with residual silanols on the surface of silica gel, is used as the bonded phase on the surface of silica gel to better shield the activity of silanols and to eliminate the influence of residual silanol groups. Compared with conventional C18 columns, these novel bonded phases have different selectivity; they can work not only in 0 to 100% water but also in 0 to 100% organic mobile phase. In particular, they exhibit good peak shapes and resolutions for polar and basic compounds and have good stability within a very wide pH range. These properties make the new stationary phases a useful complement to conventional C18 columns for a variety of HPLC applications.

The invention belongs to the field of chiral fixed phases and relates to a chiral chromatographic column fixed phase in which an amino acid derivative is taken as a matrix of a chiral selective agent and the amino acid derivative is modified onto the surface of a carrier with a chemical bonding method. The chiral fixed phase consists of a chiral monomer and a carrier, wherein the general structure of the chiral monomer is shown in the specifications, wherein m is any integer from 1 to 17; n is any integer from 1 to 10; R is an amino acid side chain group; and the carrier is silica gel. The chiral selective agent is modified on the surface of the carrier by taking amino acid as the matrix with a bonding method, so that the bonding force between the chiral selective agent and the carrier isgood, and the obtained chiral chromatographic column fixed phase has stable chemical property, a good separation effect and high column efficiency, is convenient to use, and is prevented from tailing.

The invention relates to a novel preparation method of a monolithic column stationary phase having gradient distribution, comprising the following steps: 1, pretreating a chromatographic column, 2, carrying out a preparation method of the monolithic column stationary phase having gradient distribution; and 3, preparing the monolithic column stationary phase having gradient distribution by using aspecial magnetic nano material. In the step 3, according to the preparation method disclosed in the step 2, magnetic nanoparticle-doped matrix of the monolithic column is rushed into a pretreated stainless steel tube or capillary tube, a coil or permanent strong magnetism is used to control the magnetic field intensity axially, heating reaction is carried out to solidify the matrix of the monolithic column to allow the magnetic nanoparticles to be distributed gradedly in the monolithic skeleton, so that the monolithic column stationary phase having gradient distribution is obtained. Accordingto the invention, the adjustment of the mobile phase is realized, and the stationary phase is used for gradient separation, so that the invention is suitable for separation of a complex sample; and the system has high column efficiency, high selectivity, and good repeatability of separation, and the preparation is easy to operate.

The invention provides a method for detecting 7 classes of 59 forbidden drugs in goat milk and goat milk products. The method comprises the following steps: (1) sample pretreatment: extracting a to-be-detected sample with an acid organic solvent, carrying out purification by virtue of an SPE column, dissolving a purified liquid by virtue of a primary flow phase, and carrying out UPLC-MS / MS detection; and (2) detection of 59 to-be-detected forbidden drugs: detecting the pretreated sample by virtue of an ultra-high performance liquid chromatography-mass spectrometry under specified instrument conditions of the method. The method has the advantages that many drugs can be detected, the type of the drugs is rich, the detection time is short, the sensitivity is high, and a result is accurate andstable; and meanwhile, the detection blank that multiple types and quantity of drugs in the goat milk and the goat milk products can be simultaneously detected is filled up, and the method has important significances to the guarantee of the body health of consumers and the increase of export trade competitiveness of the goat milk and the goat milk products.

The invention discloses a method for extracting gold from alkaline cyanide solution. Porous graphitized carbon black and surfactant acetone solution with the concentration of 10 percent are evaporated in a water bath by stirring, thereby obtaining a graphitized carbon black packing with the attached surfactant. The packing is arranged in a solid-phase extraction column for compaction and washed by dilute sodium hydroxide with pH of 9.4-13 for standby. Gold-containing material liquid passes through the extraction column at the flow rate of 10-100mL / min for extraction and enrichment, then eluate is further used for reverse elution, and the gold in the eluate is finally recovered by the electric deposition method. The method has small environmental pollution, the operable pH range is very wide, the one-time extraction rate of the gold exceeds 96.5 percent, the enrichment times are more than 250 times, and the extraction capacity of the material to the gold is greater than 29mg / g, thereby having a good industrial application prospect.