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1461 results about "Column temperature" patented technology

Water base dispersion of fluorinated polymer and process for producing the same

The object of the present invention is a fluoropolymer aqueous dispersion showing only a moderate viscosity increase upon temperature rise and having a low fluorine-containing anionic surfactant concentration as well as a method of producing such fluoropolymer aqueous dispersion. The present invention provides a fluoropolymer aqueous dispersion comprising a particle comprising a fluoropolymer dispersed in an aqueous medium in the presence of a nonionic surfactant, wherein a supernatant for assaying as obtained by subjecting the fluoropolymer aqueous dispersion to 30 minutes of centrifugation at 25° C. and at a gravitational acceleration of 1677 G, when subjected to high-performance liquid chromatography [HPLC] under the conditions of a flow rate of 1.0 ml/minute and a column temperature of 40° C. using an acetonitrile/0.05 M aqueous solution of phosphoric acid (60/40% by volume) mixture as a developing solution, followed by detection at an absorption wavelength at which the nonionic surfactant can be identified, shows a ratio (A1/A0), which is the ratio between the total area (A0) under the detected line and the area (A1) under the detected line over a retention time period shorter than 16 minutes, of not lower than 0.4 and the supernatant for assaying has a fluorine-containing anionic surfactant content of not higher than 100 ppm.
Owner:DAIKIN IND LTD

Method for rapidly, accurately and repeatedly determining foot-and-mouth disease vaccine antigen 146S

The invention discloses a method for rapidly, accurately and repeatedly determining foot-and-mouth disease vaccine antigen 146S. A size exclusion high-efficiency liquid-phase chromatographic column in a molecular weight separation range of 2*10<4> to 1*10<7>Da is adopted to carry out the chromatographic separation on a detected sample on a high-efficiency liquid-phase chromatography. The operation pressure of the chromatography is 1.0MPa to 2.5MPa, the flow rate in the chromatographic column is 0.5 to 1.0 ml/min, a flow phase is phosphate buffer (pH 7.0 to 7.5) containing 0.1M sodium sulfate, and the column temperature is 15 to 25 DEG C. An ultraviolet and laser detector is used for detecting an optical signal of effluent at an outlet of the size exclusion high-efficiency liquid-phase chromatographic column, and a peak area of a sample can be analyzed by virtue of a computer software system of the high-efficiency liquid-phase chromatography. A standard curve of the absorption peak area and 146S concentration is established by virtue of a relation between the ultraviolet absorption peak and the concentration of different 146S standard products of different concentrations. Chromatograph is carried out on the detected sample through the size exclusion high-efficiency liquid-phase chromatographic column. The ultraviolet absorption peak area is measured, and the concentration of 146S in the detected sample can be acquired according to the standard curve.
Owner:INST OF PROCESS ENG CHINESE ACAD OF SCI

Method for establishing fingerprint spectrum of liver-enhancing medicine

The invention provides a method for establishing a fingerprint spectrum of a liver-enhancing medicine. The liver-enhancing medicine is composed of oriental wormwood, isatis root, angelica, white paeony root, red-rooted salvia root, Radix curcumae, Astragalus mongholicus, Codonopsis pilosula, rhizoma alismatis, sealwort, rehmannia, yam, hawthorn, large-leaved gentian, liquorice and medicated leaven. The establishing method comprises the step of detecting paeoniflorin in the liver-enhancing medicine by using a high efficiency liquid chromatography method, wherein conditions are as follows: a chromatographic column takes octadecylsilane chemically bonded silica as a filling material; mobile phases comprise a mobile phase A which is acetonitrile and a mobile phase B which is an acidic water solution, and the mobile phases are subjected to gradient elution; the flow velocity is 1.0mL/min; the column temperature is 30 DEG C; the detection wavelength is 210nm to 400nm; and the number of theoretical plates is calculated according to the paeoniflorin peak and should not be less than 6000. The obtained fingerprint spectrum is a chromatographic peak which mainly takes active ingredients of the large-leaved gentian, the white paeony root, the liquorice, the red-rooted salvia root, the oriental wormwood and the astragalus mongholicus in raw materials of the liver-enhancing medicine as main parts. According to the establishing method provided by the invention, the fingerprint spectrum capable of comprehensively representing the active ingredients of the liver-enhancing medicine can be effectively obtained and has the characteristics of high precision, stability and repeatability. The obtained fingerprint spectrum can be used for guaranteeing the stability and consistency of the product quality, so that the safety and effectiveness of a product are guaranteed.
Owner:SHIJIAZHUANG DONGFANG PHARMA

Quick qualitative and quantitative method for oligosaccharide in breast milk

The invention discloses a quick qualitative and quantitative method for oligosaccharide in breast milk. The quick qualitative and quantitative method mainly includes steps of 1, pretreating samples, to be more specific, removing fat and proteins from 150-250 micro-l of breast milk to obtain ultimate supernatant, adding ultra-pure water into the supernatant and diluting the supernatant to obtain the loaded samples; 2, establishing standard curves for standard substances by the aid of ultrahigh-performance liquid chromatography and mass spectrometry; 3, separating different components of the oligosaccharide in the breast milk in the loaded samples by the aid of ultrahigh-performance liquid mass spectrometry and carrying out quantitative analysis by the aid of mass spectrometry combined with the standard curves so as to obtain the content of the oligosaccharide in the breast milk. The ultrahigh-performance liquid chromatography is implemented by the aid of amino chromatographic columns with the sizes of 2.1*100 mm and 1.7 micrometers, 8-10 mmol/L of ammonium formate solution (A) and acetonitrile (B), and the ammonium formate solution (A) and the acetonitrile (B) are used as mobile phases; gradient elution programs are carried out by the aid of 95%-75% of B for 0-10 min or are carried out by the aid of 75% of B for 10-15 min or are carried out by the aid of 75%-65% of B for 15-20 min or are carried out by the aid of 65%-10% of B for 20-21 min or are carried out by the aid of 10% of B for 21-24 min or are carried out by the aid of 10%-95% of B for 24-25 min or are carried out by the aid of 95% of B for 25-35 min; the flow rates are 0.3 mL/min, and the column temperatures are 40-60 DEG C. The quick qualitative and quantitative method has the advantage that 12 types of oligosaccharide in the breast milk can be quickly detected by the aid of the quick qualitative and quantitative method and can be quantified by the aid of the quick qualitative and quantitative method.
Owner:INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI

A kind of olanzapine related substance and its preparation method and high performance liquid chromatography analysis method

The invention discloses an olanzapine related substance and a preparation method as well as a high-efficiency liquid-phase chromatographic analysis method thereof. The olanzapine related substance has a structural formula shown in the specification. The preparation method of the olanzapine related substance comprises the following steps of: concentrating olanzapine ethanol recrystallization mother liquor; and separating through silica gel column chromatography to prepare the olanzapine related substance. In addition, the invention provides the high-efficiency liquid-phase chromatographic analysis method of the olanzapine related substance. In the high-efficiency liquid-phase chromatographic analysis method, a reversed phase C18 chromatographic column is selected and used, the detection wavelength is 220-280nm, the flow velocity is 0.8-1.0ml/minute, the column temperature is 25-30 DEG C, acetonitrile and a 0.1-0.4-percent buffer solution of glacial acetic acid and triethylamine in equal proportion are used as a mobile phase to perform gradient elution; the olanzapine related substance and other eight related substances can be simultaneously detected; and thus, quality control of olanzapine and olanzapine-containing medicaments can be completely, scientifically, effectively and quickly realized.
Owner:DALIAN UNIV OF TECH

Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography

The invention discloses a method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography and belongs to the field of analytic chemistry. The method includes the followings steps of preparing and analyzing Cl- and SO42- mixed standard solution and obtaining a linear equation of concentration and peak area, pretreating the loprazolam samples, feeding the treated loprazolam samples to an ion chromatography by a disposable needle type filter, utilizing 3.6mmol/L sodium carbonate as leacheate and analyzing and measuring the content of the chlorodion and the sulfate radical according to the obtained linear equation, wherein a chromatographic column adopted in the ion chromatography is a high-capacity chromatographic column, the inner diameter of filler of the chromatographic column is 5 micrometers, the temperature of a column temperature box is set to be 45 DEG C, sampling input quantity is 100 microliters, applied curb current is 40mA, and flow velocity is 0.8ml/min. The method is quick and simple, high in accuracy, convenient and easy to operate and applicable to quality control in the process of production of loprazolam, the integral analyzing process can be completed within 25min, and the detection requirements of the fine chemical industry are met.
Owner:ANHUI WAYEE SCI & TECH CO LTD

Milk and milk product tetracycline antibiotic residual quantity checking method

The invention relates to a method for detecting the residue amount of terracycline antibiotics in milk and dairy products. The method utilizes an ultra performance liquid chromatography - electrospray tandem triple quadrupole mass spectrometer to determine the residue amount of the terracycline antibiotics. The method is as follows: a sample is extracted from Na2EDTA-McIlvaine buffer solution (pH4.0); proteins are removed by trichloroacetic acids; a columella is extracted through an HLB solid phase and then purified and enriched; the sample is separated by a chromatographic column, with the column temperature of 30 DEG C; gradient elution is performed by utilization of water solution (v/v) which contains 0.1 percent of methanoic acids and acetonitrile as a moving phase; and quantitative detection is performed by adoption of the multi-reaction monitoring means. The detection limit of instruments is between 1.0 and 2.0 mu g/kg; a related coefficient r reaches over 0.999 within the linear range of between 1 and 100 mu g/kg; and the recovery rate is between 81.7 and 100.7 percent (the addition levels are 10 mu g/kg, 50 mu g/kg and 100 mu g/kg). The method has the advantages of quickness, accuracy, high sensitivity and wide application scope.
Owner:INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD

Method for fast and high-efficient determination of phenolic acids in grape wine

The invention relates to a method for fast and high-efficient determination of 13 phenolic acids in grape wine, belonging to the technical field of analysis of flavor substances in the grape wine. According to the method disclosed by the invention, ultra-performance liquid chromatography is utilized for performing qualitative and quantitative analysis on phenolic acid substances in the grape wine, and the method specifically comprises the following steps: selecting a BEHC18 chromatographic column, taking 2% acetic acid water and methanol as a mobile phase, setting the flow rate at 0.3mL/min, performing ultraviolet detection on wavelength to get the result that the wavelength of gentisic acid is 320nm and the wavelength of the remainder is 280nm, setting the column temperature at 50 DEG C, setting the sample injection quantity at 1 mu L, and quantifying by a peak area external reference method; and by adopting the method, the detection and the analysis can be simultaneously performed on the 13 phenolic acids in the grape wine within 10min. According to the method disclosed by the invention, any sample pretreatment is not required, and the loss caused by the pretreatment can be avoided; and compared with traditional HPLC (high-performance liquid chromatography), by adopting the method disclosed by the invention, more phenolic acid type compounds can be simultaneously detected, the separation effect is good, the analysis process is greatly shortened, convenient and easy to operate, the detection efficiency is greatly improved and the cost of the mobile phase is saved. The method disclosed by the invention has important significance for further system research of the flavor substances in the grape wine and improvement of the quality of the grape wine.
Owner:JIANGNAN UNIV

Preparation purification method of germanium tetrachloride for optical fiber

InactiveCN103183375AMeet the requirements of germanium tetrachlorideSuitable for mass production applicationsGermanium halidesPurification methodsDistillation
The invention provides a preparation purification method of germanium tetrachloride for optical fibers, which adopts germanium concentrate as a raw material; hydrochloric acid, sulfuric acid, and ferric trichloride are added into a chlorination reaction vessel according to a certain proportion for reaction to prepare crude germanium tetrachloride; the crude germanium tetrachloride is fully mixed with hydrochloric acid and manganese dioxide according to a certain proportion in a repeated distillation reaction vessel for distillation and purification to obtain preliminarily purified germanium tetrachloride; the germanium tetrachloride after repeated distillation purification is processed in a quartz rectifying tower in inert atmosphere by controlling a tower bottom temperature to be 75-95 DEG C, a tower column temperature to be 30-95 DEG C, and a reflux ratio of 4:1-14:1, so as to obtain high-purity germanium tetrachloride. The high-purity germanium tetrachloride prepared through three procedures of chlorination distillation, repeated distillation, and rectification purification, has a content of transition metal impurities of less than 3 ppb, a content of hydrogen-containing impurities of less than 1 ppm, and meets the requirements for perform rod germanium tetrachloride for optical fibers.
Owner:GRINM ELECTRO OPTIC MATERIALS

HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata

The invention relates to an HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata. The method comprises the following steps: (1) preparing a sample solution; (2) preparing a comparison product solution; (3) determining by a high performance liquid chromatography: taking the comparison product solution and the sample solution and carrying out determination analysis under following chromatographic conditions: a chromatographic column is GL InterSustain-C18 (4.6mm*250mm, 5 microns), and a mobile phase is a phosphoric acid adjusted 0.03mol/L (NH4)H2PO4 buffering solution with the pH value of 2.0 and methanol; and the volume ratio is 97 to 3, the flow speed is 0.8mL/min, the column temperature is 30 DEG C and the detection wavelength is 210nm. Under the conditions of the method, oxalic acid, formic acid, malic acid, acetic acid, citric acid and succinic acid in pinellia ternata are effectively separated, and methodological results meet the analysis determination requirements. Compared with the traditional potentiometric titration method, the measurement for content of total organic acids is clear and objective by virtue of the HPLC method disclosed by the invention, and the content of the six organic acids in pinellia ternata can be effectively and rapidly determined and the quality of pinellia ternata can be comprehensively and accurately controlled.
Owner:CHONGQING MEDICAL UNIVERSITY

Method for detecting related substances of ibuprofen and its sodium salt and preparation

The invention provides a method for detecting related substances of ibuprofen or its sodium salt and preparation. The related substances comprise impurities A, B, C, D, E and F. The method comprises (1) preparation of a test sample solution: taking an appropriate amount of ibuprofen or ibuprofen sodium raw materials, putting the materials into a certain volume of a container, dissolving the materials, diluting the solution until a desired volume marked by a scale, shaking the solution, and filtering the solution to obtain a certain concentration of the test sample solution, and (2) sample detection: pouring the test sample solution into a chromatographic instrument, and acquiring a chromatogram map of the related substances separated effectively under chromatographic conditions of use of a chromatographic column containing octadecyl silane chemically bonded silica as a filler having size of 250*4.6mm and pore sizes of 5 micrometers and having a column temperature of 20 to 40 DEG C, use of a mobile phase having a volume ratio of organic phase acetonitrile to a water phase phosphoric acid aqueous solution of 32% to 48% and phosphoric acid content of 0.01 to 0.1% in the phosphoric acid aqueous solution, a flowing rate of 1.0 to 2.3 ml/min, and a detection wavelength of 205 to 225nm. The method can realize effective separation of a variety of impurities.
Owner:CHINA PHARM UNIV
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