3859 results about "Acetonitriles" patented technology

The present invention relates to crystalline forms of salts of the KRas G12C inhibitor 2-[(2b)-4- [7-(8-chloro-1-naphthyl)-2-[[(25)-1-methylpyrrolidin-2-yl]methoxy]-6,8-dihydro-5H -pyrido [3,4- d]pyrimidin-4-yl]-1-(2-fluoroprop-2-enoyl)piperazin-2-yl]acetonitrile, pharmaceutical compositions comprising the crystalline forms, processes for preparing the crystalline forms and methods of use thereof.

The present invention discloses a method for detecting and applying C1-C2-alkyl-substituted phenol isomers, which relates to the technical field of environmental detection and includes: selecting a corresponding sample pretreatment process to prepare a test sample according to the petroleum content range in the sample; under a mobile phase of methanol-5.0-6.5 mmol / L ammonia water, using LC-MS to detect the test sample to obtain the concentration of the first component and the standardized concentrations of co-eluted 3,5-dimethylphenol and 2,6-dimethylphenol; under a mobile phase of acetonitrile-4.0-10.0 mmol / L ammonia water, using LC-MS to detect the test sample to obtain the concentration of 3,5-dimethylphenol, or the standardized concentrations of co-eluted 3,5-methylphenol and 3-ethylphenol, or the standardized concentrations of co-eluted 2,6-dimethylphenol and 2,4-dimethylphenol; under a mobile phase of methanol-5.0-6.5 mmol / L ammonia water or acetonitrile-4.0-10.0 mmol / L ammonia water, using LC-MS to separately detect the calibration samples of the co-eluted components, and calculate the conversion factor of the co-eluted components and the concentration of the other component. The present invention realizes the accurate quantification of phenol and 12 C1-C2-alkyl-substituted phenol isomers.

A construction method for and a use of rhizoma pinellinae praeparata decoction piece, standard decoction and formula granule characteristic spectra. The construction method comprises the following steps: dissolving a test sample by using a solvent, and extracting to obtain a solution to tested; and measuring said solution by using high-performance liquid chromatography (HPLC) to obtain rhizoma pinellinae praeparata decoction piece, standard decoction and formula granule characteristic spectra, wherein chromatographic conditions of the HPLC are as follows: the chromatographic column is a C18 column; and gradient elution is performed by using acetonitrile as mobile phase A and a 0.1% phosphoric acid aqueous solution as mobile phase B. HPLC is used, gradient elution is performed by using acetonitrile and a 0.1% phosphoric acid aqueous solution as mobile phases, and 4-hydroxybenzoic acid is used as a reference object, so that rhizoma pinellinae praeparata decoction piece, standard decoction and formula granule HPLC characteristic spectra are established; the method has good repeatability and precision, is stable and reliable, and can control the quality of rhizoma pinellinae praeparata decoction pieces, a standard decoction and formula granules.

The invention relates to the technical field of organic synthesis, and discloses a preparation method of bromo-pyrrole nitrile. The method comprises the following steps: (1) mixing p-chlorophenylglycine, acetonitrile, trifluoroacetic acid and a catalyst, then dropwise adding acyl chloride and carrying out acylation reaction, and after the reaction is completed, purging with an inert gas; (2) under the inert gas, mixing the mixture obtained in the step (1) with inorganic salt, then dropwise adding 2-chloroacrylonitrile, carrying out cyclization reaction, and separating a liquid phase from the obtained mixture; and (3) under the inert gas, mixing the liquid phase obtained in the step (2), hydrobromic acid and hydrogen peroxide, carrying out a bromination reaction, then extracting with acetonitrile to obtain an acetonitrile layer, then removing the acetonitrile, and then carrying out cooling crystallization to obtain the bromo-pyrrolenitrile. According to the technical scheme, the reaction yield is high, different solvents do not need to be frequently replaced, and the solvents can be recycled.

The invention discloses a method for simultaneously detecting ergothioneine, ergosterol, ergosterol peroxide and lentinine in lentinus edodes, and belongs to the technical field of measurement of active ingredients of the lentinus edodes. The method comprises the following steps: detecting a shiitake mushroom extracting solution by adopting an ultra-high performance liquid chromatography-tandem mass spectrometry mode, wherein a chromatographic column is an HILIC or C18 chromatographic column; the mobile phase A and the mobile phase B are an aqueous solution containing formic acid and a methanol or acetonitrile solution containing formic acid respectively; the mass spectrum conditions comprise an electrospray ionization source; a positive ion multiple reaction monitoring mode; the ion spraying temperature is 315-325 DEG C; the temperature of the ion transmission tube is 320-330 DEG C; and the ion spraying voltage is 3500 V to 3700 V. The method has the characteristics of high sensitivity, high selectivity and high accuracy, and is suitable for quantitative detection of ergothioneine, lentinine, ergosterol peroxide and ergosterol compounds in shiitake mushrooms.

The invention provides a continuous purification method of crude acetonitrile, and belongs to the field of acetonitrile purification. The continuous purification method of the crude acetonitrile comprises the following steps: rectification light component removal, membrane separation impurity removal, adsorption impurity removal and rectification purification. According to the continuous purification method of the crude acetonitrile, continuous purification of the crude acetonitrile can be realized, and meanwhile, the problems that new impurities are introduced by side reactions, the rectification efficiency and the rectification stability are influenced by treated products and the device is influenced by over-high alkalinity of the treated secondary rectification liquid due to the fact that sodium hydroxide and formaldehyde are adopted to treat the rectification liquid are avoided; the acetonitrile product with the purity meeting the requirement is prepared by continuously purifying the crude acetonitrile.

The invention relates to a preparation method and application of a porous material for preparing methanol through carbon dioxide adsorption and conversion. When the material is prepared, firstly, 4, 4 '4' '-(1, 3, 5-triazine-2, 4, 6-trimethylene) triphenylamine and 1, 2-acenaphthequinone are treated in a mixed solvent containing dioxane / acetonitrile / 6M acetic acid, and AT-COF is obtained; further synthesizing by adopting an impregnation method to obtain IrRu-COF; and finally, uniformly mixing the active gamma-aluminum oxide and the IrRu-COF material to form a carrier dispersion liquid, and then carrying out PEI loading, vacuum impregnation, washing and drying to obtain the PEI functionalized gamma-Al2O3 / COF composite catalyst. The technical closed loop from low-concentration CO2 capture to solar driven conversion is realized, the process flow is simple, and the energy consumption is low.

The invention discloses a method for detecting ethylene oxide and acetonitrile in stationary source waste gas, which comprises the following steps: collecting the stationary source waste gas according to a waste gas sampling device, and researching the movement direction of the stationary source waste gas to obtain movement characteristics; carrying out ethylene oxide and acetonitrile detection on the stationary source waste gas by adopting a gas chromatographic method according to the motion characteristics to obtain first detection data; carrying out ethylene oxide detection on the stationary source waste gas by adopting an electrochemical analysis method, and carrying out acetonitrile detection by adopting a liquid chromatography to obtain second detection data; and performing data fusion on the first detection data and the second detection data to obtain a comprehensive quantity, and outputting the comprehensive quantity as a detection result. The method not only can improve the detection precision of the ethylene oxide and the acetonitrile in the stationary source waste gas, but also has better interpretability, and can be directly applied to a detection system of the ethylene oxide and the acetonitrile in the stationary source waste gas.

The invention relates to the technical field of drug analysis and detection, and provides a detection method of moxifloxacin hydrochloride related substances. The related substances of moxifloxacin hydrochloride are detected by adopting a high performance liquid chromatography method, and the detection conditions are as follows: octadecylsilane chemically bonded silica is taken as a filling agent of a chromatographic column; the wavelength of a UV detector is 296 nm; the column temperature is 35-45 DEG C; the flow velocity of the mobile phase is 1.6-1.8 ml / min; the sample injection volume is 10-50 [mu] l; the mobile phase A is phosphate buffer solution-acetonitrile-methanol; the mobile phase B is phosphate buffer solution-acetonitrile-methanol; the elution mode is gradient elution; the diluent is a mobile phase A; according to the method provided by the invention, effective separation between moxifloxacin hydrochloride and various impurities can be realized, the sensitivity is high, the accuracy is good, the reproducibility is relatively good, a good linear relation is shown in a certain range, and qualitative and quantitative determination can be carried out on various impurities in moxifloxacin hydrochloride bulk drugs.

The invention relates to a method for improving quality control of cefditoren pivoxil granules, which comprises the following steps: injecting a cefditoren pivoxil granule sample solution into a high performance liquid chromatograph for analysis so as to detect impurities in the cefditoren pivoxil granules, in the high performance liquid chromatography, a mixed solution of an ammonium formate solution, acetonitrile and methanol (43-47): (23-27): (23-27) is used as a mobile phase A, a mixed solution of an ammonium formate solution, acetonitrile and methanol (43-47): (53-57): (53-57) is used as a mobile phase B, gradient elution is adopted, and a cefditoren pivoxil particle sample solution is prepared by using the mobile phase A as a diluent. According to the method disclosed by the invention, the forward delay phenomenon of an open-loop impurity peak of the cefditoren pivoxil in the cefditoren pivoxil granules and the separation degree of an unknown impurity peak are improved, the reproducibility is good, and the accuracy is high, so that the quality control level of the cefditoren pivoxil granules is improved.

The invention discloses an acetonitrile hydrogenation catalyst and a preparation method and application thereof. The acetonitrile hydrogenation catalyst is a transition metal modified Pt supported catalyst. A transition metal precursor adopted in the transition metal improvement is an oxide containing transition metal elements; the transition metal element is selected from at least one of titanium, vanadium, manganese, iron, cobalt, nickel and copper; the acetonitrile hydrogenation catalyst also comprises a carrier; the carrier is selected from at least one of gamma-Al2O3, SiO2, an MOR molecular sieve and a ZSM-5 molecular sieve. The catalyst can effectively catalyze acetonitrile hydrogenation to prepare ethylamine under mild reaction conditions. The supported catalyst provided by the invention has excellent reaction performance such as high acetonitrile conversion rate in acetonitrile hydrogenation reaction, the reaction condition is mild, the operation is simple, and the catalyst is easy to prepare and can be recycled.

The invention belongs to the technical field of medicine detection, and particularly relates to a high-sensitivity liquid chromatography method for detecting mutagenic impurities in atomoxetine hydrochloride key starting material 3-chlorobenzene propanol, the method adopts an HPLC (High Performance Liquid Chromatography) analysis method, a chromatographic column adopts octadecylsilane chemically bonded silica as a filler, and the composition of a mobile phase A is a buffer solution; the mobile phase B is methanol or acetonitrile; carrying out gradient elution on the mobile phase; the flow velocity is 0.4 to 0.8 ml / min; the detection wavelength is 230 to 250 nm; by adopting an HPLC analysis method, the content of mutagenic impurities in the key starting material 3-chlorobenzene propanol of atomoxetine hydrochloride can be effectively separated and measured, and the method is high in sensitivity, strong in specificity and good in accuracy and repeatability, and has extremely important significance on quality control of the key starting material 3-chlorobenzene propanol of atomoxetine hydrochloride.

The invention provides a content detection method for a salvia miltiorrhiza medicinal material, a salvia miltiorrhiza clear paste and a musk heart-dredging dropping pill. According to the method, a high performance liquid chromatography method is adopted, octadecylsilane chemically bonded silica is used as a chromatographic column filler, acetonitrile is used as a mobile phase A, 0.02%-0.1% trifluoroacetic acid is used as a mobile phase B, gradient elution is carried out, and rosmarinic acid and salvianolic acid B in the salvia miltiorrhiza medicinal material are synchronously and quantitatively detected. And synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid and salvianolic acid B in the salvia miltiorrhiza clear paste, and synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid, salvianolic acid B, arenobufagin and bufalin in the musk Tongxin dropping pill. The method is used for monitoring the content of specific components, can also judge the transfer rate in the medicine production process, and facilitates traceability in the production link. In addition, the method is relatively low in equipment requirement and suitable for industrial popularization.

The invention discloses a preparation method for selectively oxidizing thioether into sulfoxide through photo-initiation, and belongs to the field of synthesis of medical compounds. The preparation method comprises the following steps that in the air atmosphere, a thioether compound is dissolved in an acetonitrile-water mixed solvent, inorganic metal salt catalysts such as ferric chloride and copper sulfate are added, the mixture reacts for 8-48 h at the temperature of 0-45 DEG C under illumination with the wavelength of 295-405 nm, selective oxidation is carried out, and the sulfoxide product is obtained, and the molar ratio of thioether to the catalysts is 5: 1. The method overcomes the problems of excessive oxidation risk, complicated operation, environmental pollution and the like caused by dependence of a noble metal catalyst and use of a strong oxidant in the existing thioether oxidation method, has the advantages of high catalytic efficiency, high yield and excellent selectivity, can greatly reduce the production cost, is suitable for later industrial synthesis and amplification, and has wide application prospects. The method has the advantages of no expensive metal catalyst or oxidant, simple preparation process, high efficiency, environmental protection, safety and cost saving.

The invention belongs to the field of high-molecular polymer equipment, and particularly relates to a polyacrylonitrile slurry demonomerisation device and a demonomerisation method. Comprising an acetonitrile separation unit, a transpiration PAN capture unit and a slurry discharge unit, the acetonitrile separation unit comprises a main body tank and multiple groups of first tower plates, the multiple groups of first tower plates are arranged in the main body tank in a staggered manner, and the main body tank is provided with a slurry inlet pipeline, a steam inlet pipeline, a vacuumizing pipeline and a temperature control jacket; through combined arrangement of the inclined baffle and the horizontal segmental plate with the exhaust holes, fluid area spreading of slurry is achieved, and meanwhile separation of residual AN monomers in the slurry is achieved through combination of reverse steam introduction and slurry fluid spreading. A plurality of groups of staggered tower plates with segment structures are arranged in the upper auxiliary tank and are matched with a water mist spraying device, so that a small amount of transpiration PAN in slurry is captured and dissolved, and the demonomerisation device can be conveniently disassembled, assembled and maintained.

The invention relates to a method for synthesizing 1, 2-allene ketone, and discloses a method for synthesizing 1, 2-allene ketone by taking eneyne, 1, 4-dihydropyridine and benzoyl fluoride as substrates, 2, 4, 5, 6-tetra (diphenylamino)-isophthalonitrile as a photocatalyst, 5, 6, 7, 8-tetrahydro-3-(2, 6-diisopropyl phenyl)-4H-cycloheptyl thiazole perchlorate as N-heterocyclic carbene, cesium carbonate as alkali and acetonitrile as a solvent through a one-pot method. And reacting at room temperature for 4 hours under visible light of 12W and 460nm LED blue light to obtain allene ketone. The reaction conditions are mild, and the method has good functional group tolerance.

The invention provides a construction method and application of a fingerprint spectrum of a dampness-removing stomach-poria cocos decoction, and belongs to the technical field of drug detection.The construction method comprises the steps that the dampness-removing stomach-poria cocos decoction is used for preparing a test solution, and then the fingerprint spectrum of the dampness-removing stomach-poria cocos decoction is obtained through high performance liquid chromatography detection with acetonitrile (A)-0.18-0.22 wt% formic acid aqueous solution as a mobile phase; a standard fingerprint spectrum is established by adopting a traditional Chinese medicine chromatographic fingerprint spectrum similarity evaluation system and is used for quality evaluation or control in the whole process of research / development / production / clinical application of the dampness-removing stomach-poria decoction. According to the construction method of the fingerprint spectrum of the dampness-eliminating stomach-poria cocos decoction, main medicinal material components in the dampness-eliminating stomach-poria cocos decoction can be detected only through high performance liquid chromatography, so that the quality condition of the dampness-eliminating stomach-poria cocos decoction can be reflected more comprehensively.

The invention provides a construction method and application of an angelica sinensis potion fingerprint spectrum, and belongs to the technical field of drug detection.The construction method includes the steps that firstly, an angelica sinensis potion is used for preparing a test solution, then 0.08-0.12 wt% phosphoric acid aqueous solution (A)-acetonitrile (B) serves as a mobile phase, and the angelica sinensis potion fingerprint spectrum is obtained through high performance liquid chromatography detection, a standard fingerprint spectrum is established and is used for quality evaluation or control in the whole process of research / development / production / clinical application of the angelica sinensis potion. According to the construction method of the fingerprint spectrum of the angelica sinensis potion, main medicinal material components in the angelica sinensis potion can be detected only through high performance liquid chromatography, so that the quality condition of the angelica sinensis potion is reflected more comprehensively.

The invention belongs to the field of preparation of medical intermediates, and particularly relates to a preparation method of an On-DNA sulfinic acid structure compound. The method for preparing the On-DNA sulfinic acid structure compound comprises a step of oxidizing On-DNA thiol (phenol) into the On-DNA sulfinic acid structure compound under alkaline and heating or illumination conditions, a solvent used in the reaction step is a mixed solution of water, dimethyl sulfoxide, N, N-dimethylformamide, acetonitrile, ethanol or tetrahydrofuran, the reaction temperature is not more than 80 DEG C, and the reaction time is not more than 2 hours. And the illumination wavelength ranges from 365 nanometers to 535 nanometers. The On-DNA sulfinic acid structure compound obtained in the invention can be directly used for constructing a structure compound with a sulfonyl group, the reaction condition is mild and convenient, a new method and a new idea are provided for construction of a DNA coding compound library, and the On-DNA sulfinic acid structure compound has a very good application prospect in lead drug development.

The invention discloses a flame-retardant polyoxyethylene composite solid electrolyte and a preparation process thereof, and relates to the technical field of solid electrolytes. Comprising the following steps: 1, mixing and stirring modified polyacrylonitrile, polyacrylonitrile and N, N-dimethylformamide, and putting the mixture into an electrostatic spinning machine to obtain a polyacrylonitrile fiber membrane; 2, mixing and stirring the modified beta-cyclodextrin, acetonitrile, polyoxyethylene, lithium perchlorate and succinonitrile to obtain a mixed solution; and 3, putting the polyacrylonitrile fiber membrane into a polytetrafluoroethylene mold, dropwise adding the mixed solution, and drying and demolding at 40 DEG C to obtain the composite solid electrolyte. The composite solid electrolyte has the beneficial effects that beta-cyclodextrin and polyacrylonitrile are modified, so that the compatibility of beta-cyclodextrin and polyacrylonitrile with a polymer matrix is improved, and the ionic conductivity and tensile strength of the composite solid electrolyte are improved. Meanwhile, the grafted spirocyclic phosphate group enables the overall flame retardance of the composite solid electrolyte to be improved to a certain extent.

The invention belongs to the field of detection and analysis, and relates to a method for separating and detecting enantiomers in (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride. According to the method, HPLC is adopted for separation and detection, a polysaccharide derivative chiral chromatographic column is selected as a chromatographic column, a mobile phase A is a weak base aqueous solution, and a mobile phase B is acetonitrile and / or methanol. The method is strong in specificity, high in separation degree, high in accuracy, stable, reliable and high in sensitivity, and a simple, accurate, rapid and reliable detection method is provided for control of impurities in a starting material of (S)-2-amino-3-[2-(tert-butoxy)-2-oxoacetamido] tert-butyl propionate hydrochloride.

The invention provides a triphenylamine derivative as well as a preparation method and application thereof in killing gram-positive bacteria. The preparation method comprises the following steps: firstly, synthesizing an intermediate molecule 4-di-p-methoxyanilino benzaldehyde (s); the s respectively reacts with 3-pyridylacetonitrile and 4-pyridylacetonitrile to generate intermediate molecules a and b; the intermediate molecules a and b respectively react with methyl iodide to generate triphenylamine derivatives 1 and 2, and the intermediate molecules a and b respectively react with 9-bromomethyl anthracene to generate triphenylamine derivatives 3 and 4. The prepared triphenylamine derivative has a donor-acceptor structure and is a D-pi-A structure, the modified triphenylamine is used as a donor, a carbon-carbon double bond is used as a covalent bridge, and cyano and N positive ions have electron withdrawing property. As all the components contain positive ions, the components can be anchored on a bacterial membrane to kill bacteria; and the compound has a short alkyl chain and can be combined with gram-positive bacteria, so that the bacteria are killed.

The invention belongs to the technical field of traditional Chinese medicine detection, and discloses a detection method for a characteristic spectrum of Uighur medicine Kspecific heat extracting tablets and application of the detection method. The detection method provided by the invention comprises the following steps: preparing a test sample solution by taking a 75% methanol solution as a solvent, and determining the test sample solutions prepared from different batches of test samples by adopting ultra-high performance liquid chromatography to obtain a characteristic spectrum; the chromatographic conditions of the ultra-high performance liquid chromatography are as follows: a chromatographic column is a C18 chromatographic column, a mobile phase A is acetonitrile, a mobile phase B is a 0.1 vol% phosphoric acid solution, and the flow velocity is 0.25-0.35 mL / min; the detection wavelength is 0 to 18 minutes, and the wavelength is 327 nm; the time is 18 to 28.5 min, and the wavelength is 254 nm; when the time is 28.5 to 37.6 minutes, the wavelength is 242 nm; after 37.6 to 70 minutes, the wavelength is 210 nm; the sample size is 1 microliter, the column temperature is 20-40 DEG C, and gradient elution is carried out. The invention provides a more scientific identification and quality control method for the Kespecific heat tablets.

The invention belongs to the technical field of lignin depolymerization, and particularly relates to a selective fracture method of micromolecular mercaptan mediated lignin beta-O-4 connection. In an H-type electrolytic tank, an anode electrolytic tank takes a buffer solution as an electrolyte, a cathode electrolytic tank takes a lignin beta-O-4 model compound as a reaction substrate, and an acetonitrile / buffer solution mixed solution of small molecular mercaptan is taken as an electrolyte for electrochemical cracking reaction. Wherein a micromolecular mercaptan medium is used as a single electron transfer medium, and can efficiently and selectively break key C beta-O bonds in a lignin beta-O-4 model compound at normal temperature and normal pressure under the catalytic action of current to obtain corresponding phenol and ketone monomers, so that the problems that high temperature, high pressure and expensive catalysts are usually needed in depolymerization in a lignin reduction way are solved.

The invention belongs to the technical field of liquid chromatography-mass spectrometry detection pretreatment, and particularly relates to a pretreatment method for liquid chromatography-tandem mass spectrometry analysis of pesticide and veterinary drug residues in serum, which comprises the following steps: (S1) carrying out heating reaction on Sc (III) salt, Cu (II) salt and 1H-pyrazole-4-formic acid (H2PyC) in a polar aprotic solvent, and cooling to obtain a green crystal, namely MOF-919; the chemical formula of the MOF-919 is [Sc < 3 > (mu3-O) (OH) < 3 >] [Cu3 (mu3-O) (mu-PyC) < 3 > (H2O) < 6 >] < 2 >; (S2) mixing the serum sample with an acetonitrile solution containing formic acid, carrying out ultrasonic treatment, vortex oscillation and centrifugation, taking supernate, and diluting the supernate with an aqueous solution containing formic acid to obtain a to-be-purified solution; and (S3) adding MOF-919 into the to-be-purified liquid, mixing, performing ultrasonic treatment, performing vortex oscillation, centrifuging, and taking supernate, thereby completing the pretreatment of the to-be-purified liquid. According to the method, the MOF-919 is used for adsorbing chemical pollutant residues in serum, especially phospholipids, so that the purpose of removing the chemical pollutant residues in blood is achieved. The method is simple and convenient to operate, small in organic solvent consumption and good in purification effect, and can be widely applied to residue analysis of chemical pollutants in serum.

The invention discloses a method for purifying acetonitrile, and belongs to the technical field of organic solvent purification. The acetonitrile purification method comprises the following steps: dehydrating an acetonitrile solution through a membrane dehydration device, enabling the dehydrated acetonitrile to pass through an adsorption column filled with a magnetic iron oxide / graphene composite adsorbent, and collecting effluent; and carrying out normal pressure rectification on the effluent, controlling the reflux ratio to be 10: 1-8, the heating temperature of the rectification kettle to be 110-150 DEG C, the temperature of the acetonitrile liquid in the kettle to be 80-90 DEG C and the temperature of the distilled liquid to be 75-85 DEG C, and collecting to obtain purified acetonitrile. The method effectively solves the problems that a traditional potassium permanganate oxidant is adopted for purification at present, impurities generated by reaction are insoluble in water and difficult to remove, the environment is polluted to a certain extent, the impurities need to be filtered and removed, the operation is tedious and the like, is green and safe, and does not generate waste residues; and the final acetonitrile yield is greater than 90%, and the purity reaches 99.99%.

The invention provides a construction method of fingerprint spectrums of katsumadai medicinal material, standard decoction and formula granules thereof, which comprises the following steps: preparing a mixed reference solution from alpinetin, pinocembrin, cardamonin and alnudinone; preparing a test solution from the alpinia katsumadai medicinal material, the standard decoction or the formula granules; respectively detecting the reference solution and the test solution by adopting a high performance liquid chromatography, and constructing fingerprints of the alpinia katsumadai medicinal material, the standard decoction and the formula granules of the alpinia katsumadai medicinal material; wherein the conditions of the high performance liquid chromatography are as follows: a mixed solution of acetonitrile and methanol is taken as a mobile phase A, a phosphoric acid aqueous solution with the volume concentration of 0.08%-0.12% is taken as a mobile phase B, and a gradient elution procedure is adopted. The method has the advantages of being simple, stable and high in specificity, and a comprehensive, effective and rapid evaluation method is provided for quality control of alpinia katsumadai medicinal materials, standard decoction and formula granules of the alpinia katsumadai medicinal materials.

The invention discloses a construction method and an identification method of characteristic chromatograms of a senecio scandens medicinal material as well as decoction pieces, standard decoction and formula granules thereof, and relates to the technical field of traditional Chinese medicine identification. The construction method of the specific chromatogram comprises the following steps: extracting a to-be-detected sample with methanol to obtain a test solution; the method comprises the following steps: dissolving 5-caffeoylquinic acid, chlorogenic acid, caffeic acid, 4-caffeoylquinic acid, rutin, hyperoside, isoquercitrin and 4, 5-dicaffeoylquinic acid with methanol to obtain a reference solution; and a liquid chromatograph is adopted for determination. A chromatographic column of the liquid chromatograph takes phenyl-methyl polysiloxane as a stationary phase, acetonitrile as a mobile phase A and 0.05 vol%-0.3 vol% formic acid aqueous solution as a mobile phase B for gradient elution. The information of the characteristic chromatogram constructed by the method is rich, and the quality of the senecio scandens medicinal material, decoction pieces, standard decoction and formula granules can be quickly and comprehensively reflected.

The invention relates to the field of pharmaceutical analytical chemistry, in particular to a method for determining tandospirone and salt intermediates thereof, high performance liquid chromatography is adopted, and chromatographic conditions include that a chromatographic column with octadecylsilane chemically bonded silica as a filler is adopted, and gradient elution is performed by a mobile phase A and a mobile phase B; wherein the mobile phase A consists of a first water phase and acetonitrile; the mobile phase B is composed of a second water phase and acetonitrile; the first water phase is a water solution containing monopotassium phosphate and sodium hexanesulfonate, and the pH value of the first water phase is 3.0-3.8; the second water phase is an aqueous solution containing monopotassium phosphate and sodium hexanesulfonate, and the pH value of the second water phase is 1.8-2.6. The testing method disclosed by the invention has good specificity, accuracy and repeatability, and can be used for monitoring the quality of the tandospirone raw material medicine.

The invention relates to the technical field of medicine production and detection, and particularly discloses a method for determining the content of paeoniflorin in radix astragali and cassia twig Wuwei decoction granules, which comprises the following steps: analyzing paeoniflorin by high performance liquid chromatography, and sequentially performing sample pretreatment, chromatographic analysis and content determination. An HP-20 resin column is adopted for pretreatment, ethanol with different concentrations is used for elution in sequence, and 50% and 70% ethanol eluents are collected and concentrated; a C18 chromatographic column is selected, an acetonitrile-0. 1% phosphoric acid aqueous solution is used as a mobile phase, a diode array detector is used for detection at the wavelength of 230 nm, and a multi-wavelength deconvolution algorithm is used for quantitative analysis. The determination method disclosed by the invention is high in specificity, stability, repeatability, intermediate precision, accuracy and the like all accord with regulations, and the durability of chromatographic conditions is relatively good.