208 results about "Bulk drug" patented technology

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 spectrum on-line detection, and discloses a raw material medicine purity on-line detection method based on spectrum data fusion, which comprises the following steps: arranging two spectrum probes of the same type on a pipeline at an interval; a time sequence self-adaptive calibration mechanism is constructed, cross-correlation peak value tracking is adopted in the mechanism when signals can be tracked, and instantaneous thermal pulses are actively applied for calibration when the signals cannot be tracked, so that accurate transit time is obtained; according to the method, through space-time difference self-calibration, dependence on multi-spectrometer hardware is eliminated, high suppression of physical noise is achieved by using a single type of spectrometer, the principle is clear, and the method is suitable for large-scale popularization and application. And through active thermal pulse calibration, the problem of cross-correlation failure under homogeneous fluid is solved.

The invention provides a UPLC-MS / MS (Ultra Performance Liquid Chromatography-Mass Spectrometry / Mass Spectrometry) detection method for N-nitroso landiolol in a landiolol hydrochloride bulk drug. The method comprises the step of carrying out qualitative detection or quantitative analysis on a potential nitrosamine impurity-N-nitroso landiolol in a landiolol hydrochloride bulk drug by adopting an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS), wherein the structural formula of the N-nitroso landiolol is shown as a formula I in the specification. The detection method disclosed by the invention is high in sensitivity, strong in specificity and good in repeatability, can be used for rapidly and effectively detecting N-nitroso landiolol in the landiolol hydrochloride bulk drug, and has important significance on quality control of the landiolol hydrochloride bulk drug. ; formula I.

The application discloses a preparation method of enciferstat bulk drug and belongs to the field of drug synthesis. 9,10-dimethoxy-2-(2,4,6-trimethylphenylimino)-3,4,6,7-tetrahydro-2H-pyrimido[6,1-a]isoquinolin-4-one (SM) is used as a raw material, and the raw material is reacted with cyclohexylamine under alkaline conditions, and the reaction is washed with water, dried, and concentrated to obtain an intermediate I; the intermediate I is reacted with urea under pressurized heating conditions to prepare an enciferstat drug molecule, the two-step yield is more than 67%, and the purity is more than 99%, the method has a simple operation process, the product is easy to purify, the yield is high, the product purity is high, and a new method for preparing enciferstat bulk drug is provided.

The invention relates to the technical field of drug analysis and detection, in particular to a method for detecting related substances in moxifloxacin hydrochloride bulk drugs. According to the detection method provided by the invention, the separation efficiency of the known impurity (impurity F) can be improved, and the separation degree between the main component and the adjacent impurity can reach 1.5 or above; in addition, a solvent formula is optimized, so that a test sample is more stable, and the detection method is more accurate; the detection accuracy is improved, and the recovery rate is controlled within the range of 93-102%.

The present application relates to the technical field of pharmaceutical chemistry, and particularly relates to a preparation method of fenofibrate and impurities thereof. The present application carries out Friedel-Crafts acylation reaction on 4-chlorobenzoyl chloride, anisole, Lewis acid and benzene solvent, then carries out demethylation reaction, and then separates and purifies to obtain compound II, impurity compound IV and impurity compound V; the compound II (or impurity compound IV), 2-bromoisobutyric acid isopropyl ester, an alkaline reagent and an alcohol solvent are mixed to carry out etherification reaction, and then separated and purified to obtain fenofibrate (or impurity compound VI). The preparation method provided by the present application has high yield and high purity of fenofibrate, can realize identification of impurities in the preparation process of fenofibrate, and provides a convenient condition for quality control of bulk drug. Moreover, the raw materials and solvents used are widely sourced, low in cost and small in danger, the preparation method is high in safety factor, simple in operation, and suitable for large-scale industrial production.

The invention belongs to the technical field of medicine synthesis, and discloses a preparation method of a sodium nitroprusside raw material medicine. According to the method, weak acid is adopted for catalysis, the effect of remarkably reducing generation of toxic substances such as cyanide and nitrogen dioxide is achieved by controlling the material dripping speed and the dripping pH, the reaction is mild, the technological operation is safe and controllable, and industrial production of the sodium nitroprusside raw material medicine is facilitated. According to the preparation method of some examples, silica gel filtration is used for post-treatment, the residual risk of impurities such as sodium ferricyanide, ferric ferrocyanide and ferric ferricyanide is reduced, and the purity of the raw material medicine is larger than or equal to 99.9% and is far superior to the requirements of pharmacopoeia of various countries.

The invention discloses a method for detecting phosphate impurities, namely diethyl phosphoacetic acid and diethyl phosphate, in afatinib, and establishes a simple and sensitive ion chromatography detection method based on the hydrolysis property of a phosphate compound under an alkaline condition. Sodium hydroxide or potassium hydroxide solution-water is used as a mobile phase for isocratic or gradient elution, and a conductivity detector is used for detection. According to the present invention, the accurate quantification of the impurities in the afatinib is achieved, the detection speed is fast, the cost is low, the operation is simple, and the good specificity, the sensitivity, the precision and the accuracy are provided, such that the product quality of the afatinib maleate bulk drug synthesized by using the diethyl phosphoacetic acid as the starting material and the related preparation can be further ensured.

The utility model relates to the technical field of bulk drugs, in particular to a bulk drug centrifugal machine which comprises a centrifugal machine body, a buffer plate is arranged on the outer wall of the centrifugal machine body, a buffer assembly is arranged at the bottom of the centrifugal machine body, and a sealing mechanism is arranged in the centrifugal machine body. According to the centrifugal machine for the raw medicine, through the arrangement of the first fixing plate, the first sealing plate, the bolts, the limiting plate, the second sealing plate, a sealing ring and a second fixing plate, when the centrifugal machine conducts centrifugal treatment on the raw medicine, the internal structure of the centrifugal machine can be effectively protected, and the influence of vibration and impact force generated by high-speed rotation on equipment is reduced; by means of the structural design, the sealing mechanism can ensure that in the operation process of the centrifugal machine, raw material medicine in the centrifugal machine cannot leak, meanwhile, the interior of the centrifugal machine is protected against external pollution, and cleanliness and safety in the centrifugal process are guaranteed.

The invention provides a crystal form VI of an acrylamide compound, and the acrylamide compound is (S)-N-(5-((6-(2-(7, 7-dimethyl-1-oxo-1, 3, 4, 6, 7, 8-hexahydro-2H-cyclopentane [4, 5] pyrrolo [1, 2-a] pyrazine-2-yl)-3-(hydroxymethyl) pyridine-4-yl)-4-methyl-3-oxo-3, 3, 4-triazolo [1, 2-a] pyrazine-2-yl)-3-(hydroxymethyl) pyridine-4-yl)-4-methyl-3-oxo-3, 3, 4-triazolo [1, 2-a] pyrazine-2-yl)-3-(2, 3, 4-triazolo [1, 2-a] pyrazine-2-yl)-4- The crystal form VI is a 2-(2, 4-dihydropyrazine-2-yl) amino)-2-(2-methyl-4-(tetrahydro-2H-pyran-4-yl) piperazine-1-yl) 5phenyl) acrylamide compound, and an X-ray powder diffraction pattern of the crystal form VI comprises diffraction peaks with the following 2 theta angle values: 8-3 + / -0.2 degrees, 13.2 + / -0.2 degrees and 18.9 + / -0.2 degrees. The crystal form VI has the advantages of good stability and low hygroscopicity, and is suitable for industrial production of bulk drugs and development of preparation prescriptions.

The invention relates to the technical field of pharmaceutical analysis, in particular to a chromatographic method for determining optical isomers in a carbidopa raw material medicine and a preparation thereof by using an HPLC (High Performance Liquid Chromatography) method. The detection method is simple, convenient, rapid and accurate to operate, and specifically comprises the following steps: dissolving a proper amount of a sample with a solvent, diluting to a certain concentration, taking a certain volume of the sample, carrying out isocratic elution at a certain column temperature by adopting a high performance liquid chromatography, using a hand-type chromatographic column, a mobile phase A and a mobile phase B, and carrying out quantitative analysis by adopting a self-control method with correction factors. And calculating the isomer in the test solution. The method is good in specificity, solution stability, linearity, repeatability, intermediate precision and durability, and the detection result is accurate and reliable through verification.

The utility model relates to pantoprazole sodium bulk drug processing technical field discloses a kind of crushing devices for pantoprazole sodium bulk drug processing, including crushing box, the crushing box outer circle one side is connected with feed hopper and is fixedly connected to be penetrated, the crushing box outer circle top is fixedly connected with first motor, the first motor output end is connected with second rotating shaft and is fixedly connected to be penetrated, the second rotating shaft outer circle top is fixedly connected with two first scrapers, the first rotating shaft is rotatably connected with first rotating shaft in the top of the inner wall of two first scrapers and is penetrated, the first rotating shaft and second rotating shaft outer circle are fixedly connected with the uniformly distributed crushing knife of second rotating shaft, the second rotating shaft bottom end is fixedly connected with spiral blanking bar. In the utility model, first motor drives second rotating shaft and first scraper rotation, second rotating shaft and first rotating shaft drive crushing knife rotation, under the location of first gear, first rotating shaft and crushing knife autorotation, improve crushing effect.

The invention relates to a compound as well as a preparation method and application thereof. The preparation method comprises the following steps: taking a compound 1 as an initial raw material, and sequentially carrying out condensation with thiourea, alkaline hydrolysis and oxidative coupling with pentafluoropentanethiol to obtain the compound 1, the raw materials are easy to obtain, the reaction conditions are mild, the post-treatment process is effectively simplified through an optimized pulping purification technology, the purity of the final product is up to 98.5% or above, and the method is suitable for industrial production. And a key material basis is provided for quality research of fulvestrant bulk drugs.

The invention discloses a raw material medicine, a medicine composition and a preparation method and application thereof, and belongs to the technical field of medicine preparations, the molecular formula of the raw material medicine is C24H32ClNO6, and the raw material medicine has the following characteristics that D50 is 20-75 microns, and the particle size distribution span is 1 < = (D90-D10) / D50 < = 2.5. The raw materials provided by the invention have good process stability, dissolution stability and chemical stability. The pharmaceutical composition and the pharmaceutical preparation adopting the raw material medicines have better process stability, dissolution stability and chemical stability.

The invention discloses a novel molecular chaperone-mediated autophagy (CMA) activating agent, relates to the technical field of biological cells, and is characterized in that the novel molecular chaperone-mediated autophagy activating agent is a novel anti-tumor drug chidamide, and the novel molecular chaperone-mediated autophagy activating agent is a novel anti-tumor drug chidamide. The chidamide can obviously up-regulate the mRNA and protein level of the key protein LAMP2A in the CMA process. According to the present invention, by constructing a human THP1-LAMP2luciferase reporter gene system, the compound capable of activating the LAMP2 promoter is screened from the bulk drug; through cell level primary screening, secondary screening and animal level verification, an effective CMA activator chidamide is finally determined. A good tool is provided for basic research of CMA, and novel drugs are further researched and developed by taking CMA as a target spot.

The utility model provides an energy-saving reaction kettle for producing chemical bulk drugs, which relates to the technical field of chemical bulk drug production and comprises a shell, a top cover arranged at the top of the shell, a motor fixedly mounted at the top of the top cover, an output end of the motor penetrating through the top cover and fixedly provided with a rotating shaft, and two groups of connecting pipes symmetrically mounted on the outer wall of the rotating shaft. Scraping plates are arranged on the back-to-back sides of the two sets of connecting pipes, and first springs are fixedly installed on the inner walls of the rotating shafts. When the scraper is replaced, a worker pulls a pull plate, the pull plate drives a moving rod to move, a first spring is compressed, the moving rod drives a pressing plate to move, and a clamping block leaves a connecting groove, at the moment, the worker can take out a connecting block, replace the scraper, insert a connecting block of a new scraper into a connecting pipe and loosen the pull plate, and then the scraper is replaced. And the clamping block enters the connecting groove under the elastic action of the second spring to fix the connecting block, so that replacement can be completed, and the replacement efficiency is improved.

The invention provides a method, a primer and a probe for qualitatively / quantitatively detecting an astragalus component in a Chinese patent medicine. The method for qualitatively or quantitatively detecting the astragalus membranaceus component in the Chinese patent medicine is constructed on the basis of the specific primer pair, the probe and ddPCR. The quantitative detection method comprises the following steps: extracting DNA (Deoxyribose Nucleic Acid) of a Chinese patent medicine which has a known feed ratio and contains astragalus membranaceus components in different proportions, and carrying out ddPCR amplification reaction based on a specific primer pair and a probe to determine copy number ranges corresponding to the astragalus membranaceus components in different proportions; dNA of the Chinese patent medicine to be detected is extracted, ddPCR amplification reaction is carried out based on the specific primer pair and the probe, and the target DNA copy number of astragalus membranaceus is calculated; and determining the content of the astragalus component in the Chinese patent medicine to be detected through comparison. The method provided by the invention can qualitatively and quantitatively detect the astragalus membranaceus component in the Chinese patent medicine in a high-specificity and high-sensitivity manner, and a new technical means is provided for quality control of Chinese patent medicine bulk drugs.

The invention belongs to the technical field of chemical analysis, and particularly relates to a method for separating and determining a rucotinib mesylate intermediate Z1 and related impurities thereof. The impurities comprise any one or more of an impurity SM2a, an impurity SM1d, an impurity Z1c, an impurity Z1b, an impurity Z1a, triphenylphosphine oxide, an impurity SM2, an impurity SM1 and an impurity Z1d. Octadecylsilane chemically bonded silica is adopted as a chromatographic column filling agent; a monopotassium phosphate buffer solution is used as a mobile phase A, a mixed solution of methanol and acetonitrile is used as a mobile phase B, and main components are separated from impurities through gradient elution; and detecting in a detector to obtain a chromatogram. The method is high in specificity, short in separation time, high in sensitivity and good in durability, and has important significance on quality control of rukotinib mesylate bulk drugs and preparation products.

Heterocyclic compound drugs with a nitrogen atom as a heterocyclic atom may be used as a kinase inhibitor. The preparation of a free base crystal form of the compound is also provided. The compound used as a kinase inhibitor is a compound as shown in formula I, or a deuterated compound thereof, or a pharmaceutically acceptable salt, solvate or prodrug. Biological activity experiments prove that the compound has a good inhibitory activity on exon 20 insertion mutations in EGFR and HER2, exon 19 deletion in EGFR and exon 21 point mutation in EGFR, and can be used as the bulk drug in relevant drugs.

The application discloses a preparation method of an amido pyrazole compound and a method for preparing sildenafil by using the same. The amido pyrazole compound is shown as formula I. The compound of formula I is prepared by using 2-pentanone as an industrial chemical, and can be used for synthesizing sildenafil which is a selective inhibitor of type 5 phosphodiesterase (PDE5). The method has the advantages of easy availability of raw materials, simple operation, avoidance of nitration reaction, avoidance of safety hidden dangers caused by the nitration reaction from a technical source, and avoidance of environmental protection pressure caused by a large amount of nitration waste liquid, and is suitable for development into a green and sustainable production process of sildenafil bulk drug.

The invention discloses a method for detecting nitrite in a metronidazole bulk drug. According to the method, an ultraviolet spectrophotometric method is adopted, diazotization with sulfanilamide is carried out, then color development with N-(1-naphthyl) ethylenediamine hydrochloride is carried out, and the content of nitrite is detected at the wavelength of 530-534 nm. According to the detection method, the content of nitrite in the metronidazole bulk drug can be rapidly and accurately detected, and the method is high in recovery rate and sensitivity and good in precision, repeatability and linearity.

The utility model discloses a raw material medicine fine separation and purification device which comprises a base, the upper surface of the base is rotationally connected with a rotating table, a first motor is installed in the rotating table, the output end of the first motor is fixedly connected with a first gear, the outer surface of the first gear is connected with a second gear in a meshed mode, and the upper surface of the second gear is fixedly connected with a stirring rod. A purification device main body is fixedly connected to the upper surface of the rotating table, a split pipe is fixedly connected to the upper surface of the purification device main body, and a gear I is rotated through a motor I, so that a meshed gear II rotates in a stirring rod in the purification device main body; a motor II rotates a gear III, so that a meshed gear ring and a rotating table on the inner wall of the gear ring rotate, the rotating table rotates to enable the purification device main body to do circular motion, and meanwhile, the rotating directions of a stirring rod and the rotating table are opposite, so that the liquid medicine stirring effect is further improved, the liquid is more fully mixed, and the phenomena of chromatography and non-uniform mixing can be effectively reduced.

The application discloses a raw material medicine trace heavy metal ion detection method and system based on a micro-fluidic chip, relates to the technical field of micro-fluidic detection and electrochemical analysis, and comprises the following steps: weighing, constant volume, clarification of the raw material medicine sample, solidifying target ions, standard calibration and peak interval / scanning parameters into a detection parameter table; according to the detection parameter table, the flow and valve control are controlled to complete liquid preparation, muSPE enrichment, washing, elution and constant volume loading on the chip; blank, no standard addition, one-time standard addition and numbered archiving are sequentially measured; baseline is made according to the solidified parameters, integration and blank deduction are carried out, the solution concentration is calculated combined with standard addition measurement, and the content is output. The method disclosed by the application can constrain micro-fluidic liquid preparation, enrichment, elution and constant volume loading, so that blank, no standard addition and standard addition three rounds are measured under the same source condition; the curve and standard addition measurement are numbered and archived, integral, blank deduction and concentration are solved simultaneously, and the quantitative consistency, traceability and calculation reliability are improved.

The utility model is applicable to the technical field of production of chemical pharmacy, and provides a chemical synthetic bulk drug impurity removal device which comprises a bottom plate, a stirring tank is fixedly arranged at the upper end of the bottom plate, a supporting frame is fixedly connected to the bottom plate, and a motor is fixedly arranged at the upper end of a top plate of the supporting frame. A second rotating shaft is fixedly connected to the driving end of the motor, a bearing plate is fixedly connected to the lower end of the second rotating shaft, a cleaning assembly is arranged on the bearing plate in a matched mode, a third rotating shaft is rotatably connected to the bearing plate, and a plurality of evenly-distributed stirring rods are fixedly connected to the third rotating shaft; a supporting ring is fixedly connected to the bottom end of a top plate of the supporting frame, a bearing ring is fixedly connected to the lower end of the supporting ring, and a thrust assembly is arranged between the bearing ring and the third rotating shaft in a matched mode. The stirring tank has the advantages that raw materials adhered to the inner wall of the stirring tank can be cleaned, impurities on the filter screen on the clamping plate can be cleaned, the filter screen is effectively prevented from being blocked, and the impurity removal effect is improved.

The invention discloses an analysis method for determining halogenated alkane impurities in tigliptin hydrobromide, and relates to the technical field of quality analysis. In order to solve the problem of detection of halogenated alkane impurities in tigliptin hydrobromide, the invention provides a convenient, efficient and accurate detection method. The method comprises the following steps: preparing a test solution and an impurity reference solution, and detecting by adopting a gas chromatographic method; the method can be used for accurately determining the content of halogenated alkane in tigliptin hydrobromide, plays a guiding role in development of a synthesis process, and contributes to establishment of quality standards of tigliptin hydrobromide bulk drugs.

The invention relates to a synthetic method of didrogesterone. According to the method, progesterone is subjected to ketalation, halogenation, elimination, illumination isomerization, deprotection and final isomerization, and the didrogesterone is obtained. The method has the advantages of high yield, cheap and easily available raw materials, green and safe whole process route, high bulk drug quality and purity of 99.8% or more, and is suitable for industrial production.

A method for preparing pyrotinib, which belongs to the technical field of chemical synthesis of medicines. The method comprises the following steps: 1. preparing R,E-N-(-2-hydroxy-4-nitrophenyl)-3-(-1-methylpyrrolidin-2-yl)acrylamide; 2. preparing (R,E)-N-(2-ethoxy-4-nitrophenyl)-3-(1-methylpyrrolidin-2-yl)acrylamide; 3. preparing (R,E)-N-(4-amino-2-ethoxyphenyl)-3-(1-methylpyrrolidin-2-yl)acrylamide; 4. preparing (2E)-N-(4-amino-3-cyano-7-ethoxyquinolin-6-yl)-3-[(2R)-1-methylpyrrolidin-2-yl]acrylamide; and 5. preparing pyrotinib. The method has the advantages of the raw materials being readily available and the process being simple, economical and environmentally friendly. The method is beneficial for improving and controlling the quality of a final product bulk drug.

The application belongs to the technical field of medicine production, and provides a preparation method of pramipexole hydrochloride related substance BI-II 786BS, which takes commercial reagent (S)-2, 6-diamino-4, 5, 6, 7-tetrahydrobenzothiazole as raw material, has simple preparation process, is easy to realize, has good reproducibility, is suitable for batch production of BI-II 786BS, and has high purity of pramipexole hydrochloride related substance prepared by the method, and can be used as a control (standard) for quality control of pramipexole hydrochloride bulk drug or preparation.

The invention relates to the technical field of drug detection, and discloses a method for detecting beta-lactam compound residues in a terbinafine hydrochloride bulk drug, which effectively corrects the matrix effect of terbinafine hydrochloride on a target object by adopting a matrix target method. According to the present invention, with the combination of the optimized pretreatment steps (the ratio of the diluent to the phosphate buffer), the chromatographic conditions and the mass spectrum parameters, the simultaneous quantitative detection of the eight beta-lactam compounds (cefoxitin sodium TBXD, cefotaxime sodium TBSW, cefminox sodium TBMN, cefmetazole acid TBMZ, meropenem MEP, imipenem IMP, ertapenem sodium ERP and biapenem BIP) is achieved, the quantification limit is as low as 0.008 ppm, and the detection sensitivity is high; the detection sensitivity and accuracy are remarkably improved, and the technical problem that the trace beta-lactam cross contamination in the terbinafine hydrochloride raw material medicine cannot be reliably monitored in the prior art is solved.