195results about How to "Accurate determination of content" patented technology

The invention provides a quality control method of a preparation of white paeony roots. The method comprises the following steps of: establishing a synchronous content measuring method of white paeony root herbs, white paeony root total glycosides and paeoniflorin and albiflorin in the white paeony root preparation by adopting the same liquid-phase chromatography condition; and accurately measuring the contents of the paeoniflorin and the albiflorin. The method is simple to preprocess a sample, keeps complete characteristic components and provides a stable sample solution and has higher accuracy, favorable reproduction and a certain specificity; characteristic peaks in the obtained fingerprint map have favorable separation effect, the fingerprint maps of the white paeony root herbs, the white paeony root total glycosides and the preparation have favorable relativity; the standard fingerprint map of the white paeony root herbs is established at a new angle by utilizing the relativity research of the fingerprint maps, can be used for identifying the qualities of the white paeony root herbs and improving the controllability of the production process of the white paeony root preparation and is favorable to ensuring the quality stability and the clinical curative effect of the white paeony root preparation.

The invention discloses a method for detecting free radical ration in coal tar. The method comprises the steps of removing moisture in the tar in a high speed centrifuging manner, and preserving a tar sample under low temperature or inert atmosphere; adopting a diamagnetism substance to deliquate DPPH(1,1-Diphenyl-2-picrylhydrazyl radical 2,2-Diphenyl-1-(2,4,6-trinitrophenyl) hydrazyl) to prepare a plurality of DPPH standard samples with different free radical concentrations, carrying out EPR (electron paramagnetic resonance) measurement, carrying out secondary integration on an EPR spectrogram, and recording the corresponding secondary integration area; establishing a standard curve according to the free radical contents of the DPPH standard sample with different free radical concentrations and the secondary integration area of the corresponding EPR spectrogram; and filling the tar sample into a pipe, measuring according to the same EPR measuring condition, carrying out secondary integration on the measured EPR spectrogram, and substituting the secondary integration area into the standard curve so as to obtain the free radical content N. The method provided by the invention can exactly measure free radical content in coal tar, meanwhile, the change of the content of the free radical in the coal tar along with the preservation condition is exactly measured, and the method for detecting ration is provided for the research of the free radical in the coal tar and is very simple and easy.

The invention relates to a dipping resin with the surface covered by an ionic liquid film containing extractant, and a fabrication method as well as application thereof. The ionic liquid containing the extractant is fixed in adsorption resin XAD-7; acid or alcohol or heat is not required to be added by using a direct dipping method, the stability of the ionic liquid is hardly affected, and the loading of ionic liquid matrix system in the material is large. Solid-liquid extraction is carried out by using the dipping resin, therefore, the contact area of ion liquid phase and water phase can be effectively increased, the mass transfer efficiency of the system can be improved, clamp strap loss of the ionic liquid can be reduced, and the phenomena of emulsion, phase splitting, etc. in the extraction process can be improved. In an extraction restriction complexation method, complexation agent is added in the water phase, and the extraction efficiency of the ionic liquid phase on the target metallic ions and selection among different metallic ions are improved by the difference of stability constants between the complexation agent and the metallic ions, thus effectively avoiding the phenomena of extraction efficiency reduction and ionic liquid decomposition in the separation process by adjusting the pH value. The two methods can be combined to be applied to imetallic ion separation with excellent separation effect.

The invention relates to a determining method of an atorvastatin calcium related substance. The method comprises the following steps of 1, preparing a test solution, i.e. taking a proper amount of atorvastatin calcium, adding a solvent to dissolve and quantitatively dilute the atorvastatin calcium until about 1mg of atorvastatin calcium is contained in 1ml of solution, and taking the solution as the test solution; 2, preparing a mixed reference substance solution, i.e. weighing a proper amount of reference substances of an impurity A, an impurity B, an impurity C, an impurity D and an impurity E, and a proper amount of reference substance of the atorvastatin calcium, adding the solvent to dissolve and quantitatively dilute the reference substances until about 3 micrograms of impurity A, 2 micrograms of impurity B, 2 micrograms of impurity C, 2 micrograms of impurity D, 2 micrograms of impurity E and 10 micrograms of atorvastatin calcium solution are contained in 1ml of solution, and taking the solution as the mixed reference substance solution; 3, performing HPLC (High Performance Liquid Chromatography) analysis, i.e. taking 20 microliters of test solution and 20 microliters of mixed reference substance soulution, respectively filling the test solution and the mixed reference substance into a liquid chromatograph, recording a chromatogram until a gradient elution program is finished, and according to the peak area of the chromatogram, calculating the content of each component.

The invention discloses a separation method of salidroside impurities which includes the steps of first separation with silica gel column chromatography, elution with chloroform-ethanol gradients, collection by four sections and the separation and purification with semi-preparative high-performance liquid chromatography; wherein, the semi-preparative high-performance liquid chromatography is provided with the conditions as follows: a chromatographic column: ODS C18, 5mum and 250 * 10.0mm (I. D.); volume ratios of components of mobile phases: methanol to water equals to 11 to 89; flow rate: 3.0 mL/min; column temperature: 25 DEG C; detection wavelength: UV275nm; sample size: 50 muL; effluent liquid collection by section. The high-performance liquid chromatography of the salidroside and impurities thereof adopt the reversed-phase high-performance liquid chromatography with the following chromatographic conditions: a chromatographic column: ODS C18, 5mum and 150 * 4.6mm (I. D.); mobile phases: methanol to water equals to 15 to 85; flow rate: 1.0 mL/min; column temperature: 25 DEG C; detection wavelength: UV275nm; sample size: 20 muL. The contents of the salidroside and the impurities HEPG, HPAG and PAPG of the salidroside samples can be determined accurately and simultaneously by adopting the high performance liquid chromatography of the salidroside and impurities thereof, which provides a simple and reliable method for the quality control analysis in the production process.

The invention relates to a measuring method of solid-solution boron content in steel, and belongs to the technical field of analytical chemistry. The method comprises the steps of: using a constant current electrolysis method to extract solid-solution boron at low temperature; transferring electrolyte with a certain volume, and diluting the electrolyte to be in a ruled volume; using an inductively coupled plasma source mass spectrometer to measure the solid-solution boron; and using a matching method to eliminate the influence of the components of the electrolyte on the measurement of the inductively coupled plasma source mass spectrometer. The measuring method has the advantage that the solid-solution boron content in the steel can be accurately measured.

The invention belongs to the field of natural medicine chemistry and quality control, and relates to a method for measuring the weight-average molecular weight and the content of soluble salt of mannuronic acid substances. Weight-average molecular weight and content results of acid sugar measured by an SEC-MALS (size exclusion chromatography with multi-angle laser scattering detector) are corrected by the aid of the metal ion content of soluble salt samples of the mannuronic acid substances. The weight-average molecular weight and the content of the soluble salt w of the mannuronic acid substances can be rapidly and accurately measured by the method.

The invention discloses a high-performance liquid chromatographic analysis method of 2-methoxymethyl-4-aminophenol and impurities thereof. The method comprises the following steps of: selecting reverse high-performance liquid chromatography; setting chromatographic conditions, wherein the chromatographic column is C18, 5 mum, 150*4.6 mm (I.D.), the mobile phase includes acetonitrile: phosphoric acid -phosphate buffer solution (pH 7.0) at a volume ratio of 45:55 with a flow rate of 0.8 ml/min, the column temperature is 30 DEG C, the detection wavelength is 232 nm, the injection dose is 5 to 10 mul, and (NH4)2HPO4 20 mmol/l is added into the mobile phase; adding phosphoric acid to adjust pH to 7.0; diluting the concentration of the injection sample to 1/50; and determining the contents of 2-methoxymethyl-4-aminophenol and the impurities thereof. The invention provides a simple and reliable method for quality control and analysis of 2-methoxymethyl-4-aminophenol.

The invention discloses a method for detecting 3-amino-2-azepanone through a high performance liquid chromatography. According to the method, the following chromatographic conditions are adopted: a chromatographic column is an ODS column; a mobile phase A is a 0.01-0.09 mol/L monopotassium phosphate solution; a mobile phase B is a mixed water solution of methanol and acetonitrile in which the volume ratio of methanol, acetonitrile and water is (1-5):(1-5):1; the flow velocity is 0.4-1.2 ml/min; the detection wavelength is 100-300 nm; the column temperature is 20-60 DEG C; the sample size is 5-20 [mu]l. Through adoption of the method, the content of the impurity of 3-amino-2-azepanone degraded by lysine can be accurately measured, and the specificity is good; the quantification limit repeatability is good, the recovery rate is high, and a solution is high in stability; when the column temperature, the detection wavelength and the flow velocity change slightly, the difference between a detected recovery rate of 3-amino-2-azepanone and a result detected at a basic condition is very small, so that the durability of the method is high.

The present invention provides a correction method for determination of trace element in a sample by isotope dilution mass spectrometry, and belongs to the field of isotope dilution mass spectrometry determination. During value determination of the trace element in a to-be-tested sample by isotope dilution mass spectrometry, when isotopic abundance ratios of a to-be-tested element in a standard material solution and a to-be-tested sample solution are not equal due to matrix interference, the isotopic abundance ratio of the to-be-tested element in the standard material solution and the isotopic abundance ratio of the to-be-tested element in the to-be-tested sample solution are respectively measured, and then according to the correction method, correction coefficient K is calculated; and measurement value associated with the to-be-tested sample can be calibrated by use of the K value for finally realizing the accurate determination of the content of the trace element in the to-be-tested sample by isotope dilution mass spectrometry. The method solves the to-be-tested sample matrix interference effect on the value determination accuracy during determination of the content of the trace element in the to-be-tested sample by isotope dilution mass spectrometry.

The invention discloses a method for measuring the content of amino acid in a black-bone chicken milk increasing preparation. The method comprises the following steps: subjecting a black-bone chicken milk increasing preparation to a protein hydrolysis treatment; and then using an amino acid analyzer to analyze the hydrolysate so as to measure the amino acid content. In the conventional standards, the protein content can be only represented by total nitrogen content, the provided method can overcome the shortage, moreover, the method can precisely measure contents of 17 amino acids in the preparation, has the advantages of simple pretreatment, strong specificity, good repeatability, and high precision, can well control the quality of the black-bone chicken milk increasing preparation, and improves the safety and effectiveness of the preparation.

The invention provides a method for measuring the content of luteolin in lamiophlomis rotata by liquid chromatography. The method comprises the following steps that the octadecylsilane chemically bonded silica is taken as a filling agent and the acetonitrile-tetrahydrofuran-0.5 percent of phosphoric acid is taken as the mobile phase; under the chromatographic conditions that the detected wavelength is 350 plus or minus 2 nm, the column temperature is 25 DEG C to 50 DEG C, the flow velocity is 0.5 ml/min to 1.5ml/min and the sample size is 5 mul to 20 mul, the liquid chromatography analysis is carried out on the prepared test solution, the chromatographic peak area of the corresponding position of the reference solution is measured, and the corresponding content is calculated according to the standard curve. The measuring method has the advantages of high precision, good reproducibility, high recovery ratio and accurate measuring result, improves the quality standard of the pharmaceutical preparation containing the lamiophlomis rotata herb, facilitates the quality stability and the quality control of the industrial production and ensures the security and the validity on medication use by people.

The invention belongs to the technical field of a chemical detection method and particularly relates to a specific method for determining the content of zirconium in a uranium-zirconium alloy by adopting an EDTA (Ethylene Diamine Tetraacetic Acid) titration method. The invention establishes a detection method of the content of the zirconium in the uranium-zirconium alloy by adopting the EDTA titration method. By carrying out experiments including selection of a sample dissolving temperature, an adding amount of hydrofluoric acid, an interference experiment of uranium, titration acidity, a titration temperature and the like and taking 0.2g of a uranium-zirconium alloy sample as the standard, the precision density of the method is better than 1%; and the method is accurate and reliable, and index requirements of a project analysis technology are met.

A method for discriminating the active component of Chinese elder flower particle and measuring its content features that the HPLC/MS method is used to discriminating the polypeptide as its active component and the efficient liquid-phase chromatography is used to measure the content of polypeptide.

The invention relates to a novel chemical detection method, and more specifically relates to a method used for measuring the content of 15 rare earth elements in thorium dioxide powder and blocks via inductively coupled plasma-atomic emission spectrometry. The method comprises following steps: sample dissolving, wherein a 0.2-0.5% hydrofluoric acid solution is added in dissolving of thorium dioxide, and adding amount is controlled to be 0.1ml or less; separation of thorium and the rear earth elements, wherein 3mol/L nitric acid is taken as a medium, an extraction agent composed of carbon tetrachloride and tributyl phosphate at 1:1 is used for three times of extraction so as to separate thorium and the rear earth elements; and sample measuring. According to the method, analytical line of the measured elements, sample substrate concentration, sample dissolving method, thorium and the rear earth elements separation method and conditions, and instrument parameters are determined, and inter element measuring interference test is carried out at the same time; an inductive coupling plasma emission spectrometer is used for simultaneous determination of the contents of the elements; method precision is high than 10%; and average recovery rate ranges from 91 to 110%. Operation of the method is simple; and the method is accurate and reliable.

The invention discloses a determination method of content of fulvic acid in fermentation liquor. The method comprises the following steps of 1) determining sugar in the fermentation liquor; and 2) determining the total fulvic acid in the fermentation liquor; 3) calculating the content of pure fulvic acid in the fermentation liquor: a, calculating the content of glucose equivalent to fulvic acid according to the linear relationship that glucose is corresponding to fulvic acid; and b, mapping by taking the glucose mass as an x-coordinate and the corresponding fulvic acid mass as a y-coordinate, thereby obtaining a working curve and an equation of linear regression as Y=aX+b, wherein a refers to slope, and b refers to intercept, converting the content of sugar in a sample into the content of fulvic acid, and then subtracting the content of sugar which is converted into fulvic acid by the content of the total fulvic acid, and then dividing the total amount of the fermentation liquor sample, thereby obtaining the percentage composition of pure fulvic acid in the fermentation liquor. The method provided by the invention can accurately determine the content of fulvic acid in the fermentation liquor.

The invention provides a kurarinone freeze-dry powder preparation and a preparation method thereof. The preparation method comprises the following steps: filtering the solution of three components - kurarinone, mannitol, disodium edetate or calcio-sodium edetate in an appropriate proportion, freezing and drying, and then obtaining the freeze-dry powder preparation. Compared with the prior product, the preparation has the advantages that the stability is obviously improved, the expiry date can be as long as 24 months, and the characters of the product are not changed obviously; compared with the prior art, the preparation method is more simplified, and the production cost is saved. The invention also provides a method for detecting the content of oxymatrine in the product of kurarinone freeze-dry powder preparation. By optimizing the mobile phase and the detection condition, a highly-effective liquid-phase chromatographic detection method with better differentiation and stronger specificity is established.

The invention discloses a pepper numb-taste component content detection based on a method of quantitative analysis of multi-components by a single marker. The pepper numb-taste component content detection based on the method of quantitative analysis of multi-components by the single marker comprises the steps: (1) establishing a hydroxy-beta-sanshol standard curve; (2) detecting the content of hydroxy-beta-sanshol in a sample to be detected; and (3) using a relative correction factor to calculate the contents of hydroxy-alpha-sanshol and hydroxy-gamma-sanshol in the sample to be detected. According to the pepper numb-taste component content detection based on the method of quantitative analysis of multi-components by the single marker, the method of quantitative analysis of multi-components by the single marker and an external standard method are mutually confirmed and have no obvious difference; and the results of the method of quantitative analysis of multi-components by the single marker and the external standard method are both reliable. The pepper numb-taste component content detection based on the method of quantitative analysis of multi-components by the single marker, disclosed by the invention, has the advantages that the contents of the hydroxy-alpha-sanshol and the hydroxy-gamma-sanshol are calculated by using the relative correction factor and determination of chromatographic peak in case of lacking comparison products of the hydroxy-alpha-sanshol and the hydroxy-gamma-sanshol, the quality controls of main numb-taste components of the hydroxy-alpha-sanshol and the hydroxy-gamma-sanshol in pepper are realized, and a new method is provided for pepper quality control.