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475 results about "Bulk drug" patented technology

Definition of Bulk Drug Substance Bulk Drug Substance means any substance that is represented for use in a drug and that, when used in the manufacturing, processing, or packaging of a drug, becomes an active ingredient or a finished dosage form of the drug. The term does not include intermediates used in the synthesis of such substances.

Method for detecting impurities in moxifloxacin hydrochloride bulk drug

PendingCN119715896AComponent separationPhosphateUv detector
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.
Owner:NANJING CHIA TAI TIANQING PHARMA

Solid-phase synthesis method of semeglutide

The invention provides a solid-phase synthesis method of semeglutide, and belongs to the technical field of synthesis of medical intermediates, and the method specifically comprises the following steps: segmenting a semeglutide main chain into three shorter polypeptide fragments, namely a fragment 4, a fragment 5 and a fragment 2, which are 7-14 sites, 15-22 sites and 23-37 sites; and respectively synthesizing and then assembling fragments to obtain a target product. The method specifically comprises the following steps: a) synthesizing a 7-14 peptide fragment and a 15-22 peptide fragment, and assembling the 7-14 peptide fragment and the 15-22 peptide fragment into a 7-22 peptide fragment, namely a fragment 1; b) synthesizing a 23-37 peptide fragment, selectively removing a protecting group A11oc on Lys26, and connecting with a side chain to form a fragment 3; c) connecting the peptide fragment 7-22 with the peptide fragment 23-37, and removing a protecting group to obtain a crude product; and d) separating and purifying to obtain a finished product. According to the invention, the purpose of high-purity, high-yield and low-cost synthesis of the semeglutide bulk drug can be achieved.
Owner:SICHUAN OPEN MEDICINE CO LTD

Determination method of tandospirone and salt intermediate thereof

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.
Owner:SHENYANG HUATAI MEDICATION RES CO LTD

Method for detecting bacterial endotoxin in melphalan hydrochloride bulk drug

The invention relates to a method for detecting bacterial endotoxin in a melphalan hydrochloride bulk drug, and belongs to the technical field of drug analysis. The invention provides a test solution for detecting bacterial endotoxin in a melphalan hydrochloride raw material medicine, which comprises a test product melphalan hydrochloride raw material medicine, a 2-8 DEG C sulfobutyl beta-cyclodextrin sodium water solution and calcium and / or magnesium ions. The detection method disclosed by the invention is simple to operate, the sample can be dissolved in BET water without reanalysis, and the detection result is accurate; no organic solvent is used for preparing a test solution, so that the safety to operators is good, and bacterial endotoxin interference experiments prove that no interference effect exists; and the detection limit of the bacterial endotoxin in the melphalan hydrochloride bulk drug can reach 0.2 EU / mg.
Owner:SICHUAN HUIYU PHARMA

Raw material medicine freeze-drying plate layer structure

The bulk drug freeze-drying plate layer structure comprises a main body plate layer and a bent plate layer and further comprises a connecting block, the bent plate layer comprises a horizontal part and an inclined part which is connected with the horizontal part and is arranged obliquely upwards, an upper panel and a lower panel of the horizontal part are parallel, an upper panel and a lower panel of the inclined part are parallel, the length of the main body plate layer is a, the length of the horizontal part is b, a is larger than b, and a is larger than b. One side of the connecting block is welded with the main body plate layer, and the opposite other side is welded with the horizontal part. The processing method comprises the following steps: S1, respectively processing the main body plate layer and the bent plate layer; s2, welding the main body plate layer and the bent plate layer; s3, the welded main body plate layer and the bent plate layer are leveled, and then the horizontal part of the bent plate layer is leveled; s4, fourth sealing blocks on the edges of the bent plate layers are assembled and welded, leveling is conducted after welding is completed, and the fourth sealing blocks and the connecting blocks are oppositely arranged; and S5, the welded main body plate layer and the bent plate layer are leveled again, and then the horizontal part of the bent plate layer is leveled.
Owner:TRUKING TECH LTD

Analysis method of mutagenic impurities in small molecule fungal inositol acyltransferase 1 inhibitor bulk drug

The invention relates to the technical field of medicine analysis, in particular to a method for analyzing mutagenic impurities in a small molecule fungal inositol acyltransferase 1 inhibitor raw material medicine, the analysis method can be used for trace detection of potential mutagenic impurities I and II in the raw material medicine, the limit of quantitation concentration of the impurity I is not higher than 0.53 ng / ml, and the limit of quantitation concentration of the impurity II is not higher than 0.53 ng / ml. The detection limit concentration of the impurity I is not higher than 0.27 ng / ml; the quantitation limit concentration of the impurity II is not higher than 0.52 ng / ml, and the detection limit concentration of the impurity II is not higher than 0.26 ng / ml. The analysis method suitable for the mutagenic impurities in the small-molecule fungal inositol acyltransferase 1 inhibitor bulk drug is high in sensitivity and high in specificity, and the blank solvent does not interfere with detection of the impurities.
Owner:TIANJIN CHENXIN PHARM RES CO LTD +1

Analysis method for measuring content of dihydroergoline mesylate bulk drug

The invention relates to the technical field of drug analysis, and particularly discloses an analysis method for measuring the content of a dihydroergoline mesylate bulk drug, which comprises the following steps: step S1, adding the dihydroergoline mesylate bulk drug into anhydrous acetonitrile to obtain a stock solution to be measured, precisely measuring 1mL of the stock solution, adding a cosolvent, uniformly shaking, and fixing the volume to obtain a solution to be measured; s2, taking a dihydroergoline mesylate raw material medicine, adding the dihydroergoline mesylate raw material medicine into anhydrous acetonitrile to obtain a control stock solution, precisely measuring 1mL of the control stock solution, adding a cosolvent, uniformly shaking, and fixing the volume to obtain a control solution; s3, measuring the content of the dihydroergoline mesylate raw material medicine by using a high performance liquid chromatography; according to the present invention, the cosolvent contains the 1-butyl-3-methylimidazole tosilate, the mobile phase of the high performance liquid chromatography contains the elution reinforcing agent, and through the reasonable ratio of the components, the solubility of the dihydroergoline mesylate can be improved, and the accuracy of the high performance liquid chromatography analysis can be improved.
Owner:宝利化(南京)制药有限公司

Preparation method of fusidic acid cream

The invention provides a preparation method of fusidic acid emulsifiable paste, and relates to the field of pharmaceutical preparations, and the preparation method comprises the following steps: step 1, preparation of fusidic acid nanoparticles, step 2, preparation of an oil phase of the emulsifiable paste, step 3, preparation of a water phase of the emulsifiable paste, step 4, emulsification, and step 5, mixing. According to the fusidic acid nanoparticles, firstly, a composite carrier is prepared, then fusidic acid, PLGA, the composite carrier and absolute ethyl alcohol are mixed, a nanoparticle oil phase is obtained, then PVA, PVP, sodium dodecyl glucoside sulfonate and dipotassium ethylenediaminetetraacetate are mixed with deionized water, a nanoparticle water phase is obtained, and finally a nanoparticle suspension is obtained through mixing. The fusidic acid emulsifiable paste prepared by the method can effectively solve the problems that the traditional emulsifiable paste bulk drugs are easy to agglomerate, the drug molecule particle size is large and the like, and the transdermal absorption rate and bioavailability of fusidic acid are improved, so that the antibacterial effect is enhanced.
Owner:CHONGQING CONQUER PHARML

Smeglutide

The invention provides semeglutide, which is synthesized by adopting the following method, and the specific steps are as follows: 1) segmenting the main chain of semeglutide into three polypeptide fragments: 7-14 sites, 15-22 sites and 23-37 sites; (2) respectively preparing the 7-14-site fragments, the 15-22-site fragments and the 23-37-site fragments through solid-phase synthesis; 3) connecting the 7-14-site fragment with the 15-22-site fragment to form a 7-22-site fragment, and activating the C end of the fragment into active ester; (4) selectively removing an Alloc protecting group of Lys26 in the 23-37-site fragment, and then carrying out fatty acid modification to obtain a modified 23-37-site fragment; 5) in a liquid phase system, coupling the activated 7-22-site fragment and the modified 23-37-site fragment according to a molar ratio of 1: (0.6-1.4) to form a complete polypeptide chain; and 6) removing the protecting group and purifying to obtain a semaglutide finished product. The method provided by the invention can effectively realize high-purity, high-yield and low-cost synthesis of the semeglutide bulk drug.
Owner:SICHUAN OPEN MEDICINE CO LTD

Traditional Chinese medicine plaster bulk drug split charging device

The utility model relates to the technical field of traditional Chinese medicine plasters, in particular to a traditional Chinese medicine plaster bulk drug split charging device which comprises a material containing shell, a split charging shell is fixedly installed at the lower end of the material containing shell, a rotating disc is rotationally arranged in the split charging shell through a motor, and a material distributing groove is formed in the side face of the rotating disc. The at least two material distributing grooves are distributed in a circumferential array mode along the circumference of the rotating disc, a material guiding hole is formed in the upper end of the sub-packaging shell, a discharging hole is formed in the lower end of the sub-packaging shell, an adjusting mechanism is further fixedly installed in the rotating disc, a rotating shaft is rotationally installed in the material containing shell, a stirring rod is fixedly installed on one side of the rotating shaft, and the stirring rod is fixedly installed on the other side of the rotating shaft. The traditional Chinese medicine plaster raw material medicine split charging device can be used for uniformly and equivalently split charging and conveying medicine raw materials, and is worthy of popularization.
Owner:ANHUI JIUHETANG NAT PHARM CO LTD

Method for detecting residual solvent benzene in ziprasidone hydrochloride bulk drug

The invention relates to a method for detecting residual solvent benzene in a ziprasidone hydrochloride bulk drug. According to the detection method, dimethyl sulfoxide is used as a diluent, a 2.8 mol / L potassium hydroxide solution is used as a cosolvent, and a dimethyl sulfoxide solution of high-concentration ziprasidone hydrochloride can be completely dissolved under a high-temperature heating condition, so that the sensitivity of benzene meets the requirement; and detecting the benzene in the ziprasidone hydrochloride bulk drug by using a gas chromatograph (GC-FID headspace sampling) connected with a hydrogen flame ionization detector. The detection method can be used for quantitatively detecting benzene higher than 0.4 ppm in ziprasidone hydrochloride bulk drugs. The method is high in sensitivity and practicability, and the detection process is simple and rapid.
Owner:CHONGQING RUIEN PHARM CO LTD +1

Stable AST-3424 raw material medicine ethanol composition solution

< TableDetails number = '0001' > < Title / > < tbl: tgroup cool = '2' > < tbl: colspec cool = 'c001' cool = '46%' / > < tbl: colspec cool = 'c002' cool = '54%' / > < tbl: cool > < tbl: cool = '1' > impurity < / tbl: cool > < tbl: cool = '1' > HPLC percentage content < / tbl The mobile phase B is a 8mmol / L ammonium acetate solution, and the solvent is a mixed solvent of acetonitrile and water in a volume ratio of 95: 5; and carrying out gradient elution at a flow rate of 1.0 ml / min.
Owner:SHENZHEN ASCENTAWITS PHARM TECH CO LTD

Flavonoid compound-meglumine co-amorphous substance and preparation method thereof

The invention belongs to the technical field of medicines, and particularly relates to a flavonoid compound-meglumine co-amorphous substance and a preparation method thereof. The flavonoid compounds comprise baicalein, hesperetin, naringenin, kaempferol, quercetin, isoliquiritigenin and the like, and the co-amorphous substance consists of a single flavonoid compound and meglumine and is prepared by adopting a melting shock cooling method or a rotary evaporation method. The miscibility of the flavonoid compounds and the meglumine is screened through Hansen solubility. The crystal diffraction characteristics, thermodynamic properties and intermolecular interaction of the co-amorphous substance are measured through PXRD, DSC and FTIR, and it is shown that the six flavonoid compounds and meglumine successfully form a co-amorphous system. The solubility and the dissolution rate of the six flavonoid compound-meglumine co-amorphous substance are obviously superior to those of flavonoid bulk drugs, and the physical stability of the formed co-amorphous substance is obviously superior to that of a single amorphous drug, so that the co-amorphous substance shows good patent medicine performance.
Owner:CHANGZHOU UNIV

Inducer, reagent combination and application of inducer and reagent combination in preparation of anisodamine

PendingCN120240469ABiocidePlant growth regulatorsBiotechnologyL-Hyoscyamine
The invention relates to the technical field of biology, in particular to an inducer, a reagent combination and application of the inducer in preparation of anisodamine. The inducing agent comprises silver nitrate, acetylsalicylic acid and methyl jasmonate, the components of the inducing agent cooperate with one another, compatibility is high, synergistic interaction can be achieved, and the efficiency of the inducing agent for rapidly converting hyoscyamine into anisodamine is further improved. According to the invention, a suspension cell culture technology is adopted, and an optimized callus culture medium, a precursor substance hyoscyamine and an inducer are combined, so that compared with an initial material anisodamine tanguticum used by an existing anisodamine hydrobromide raw material medicine, the anisodamine hydrobromide raw material medicine has the advantages of short growth cycle, stable content and components, environmental protection and no damage to natural resources; the invention provides a new approach for obtaining a starting material for the production of an anisodamine hydrobromide bulk drug, and is suitable for popularization and application.
Owner:CHENGDU FIRST PHARMACEDTICAL CO LTD

Lcidipine film-controlled sustained-release pellet capsule and preparation method thereof

The invention discloses a lacidipine film-controlled sustained-release pellet capsule and a preparation method thereof, relates to the technical field of medicines, and aims to solve the problem of release reduction caused by film aging of a lacidipine film-controlled sustained-release pellet prepared by an aqueous dispersion coating. The preparation method comprises the following steps: respectively weighing a lacidipine bulk drug, a polymer carrier material and a plasticizer according to a prescription amount, grinding and uniformly mixing to prepare the lacidipine solid dispersion. A sustained-release coating film of the pellet capsule contains Eurdragit RL30D, a plasticizer triethyl citrate and an anti-sticking agent talcum powder, and a pellet core contains croscarmellose sodium and an excipient. According to the lacidipine solid dispersion solid preparation provided by the invention, lacidipine exists in the carrier material in a microcrystalline state, an amorphous state, a colloidal dispersion state or a molecular dispersion state, so that the lacidipine solid dispersion solid preparation has high dispersity, the dissolution speed of a medicine is accelerated, the absorption of the medicine can be promoted, and the bioavailability is improved.
Owner:HARBIN PHARMA GROUP TECH CENT

Preparation method of salt of 2, 4-disubstituted-5-fluoropyrimidine derivative

The invention belongs to the technical field of organic synthesis, and relates to a preparation method of a salt of a 2, 4-disubstituted-5-fluoropyrimidine derivative, which comprises the following steps: carrying out protecting group removal and salt forming reaction on a compound VI in a reaction solvent in the presence of hydrochloric acid to obtain a compound I; wherein the preparation method of the compound VI comprises the following steps: carrying out salt forming reaction on a compound V in a hydrochloric acid solution to prepare the compound VI; after the reaction is completed, post-treatment is carried out, and the post-treatment comprises the steps that an anti-solvent is added, and crystallization is carried out at a certain temperature. The invention provides the preparation method of the salt of the 2, 4-disubstituted-5-fluoropyrimidine derivative, which has the advantages of high yield, high purity, lower cost and simplicity and convenience in operation. By optimizing a plurality of preparation steps, the yield and purity of the target compound are improved, and the prepared finished product can meet the general standard requirements of bulk drugs.
Owner:CENT SOUTH UNIV

Methotrexate-cationic polypeptide conjugate as well as preparation method and application thereof

The invention discloses a methotrexate-cationic polypeptide conjugate as well as a preparation method and application thereof, and belongs to the technical field of medicinal chemistry. According to the conjugate, MTX and cationic polypeptide with the amino acid sequence shown as SEQ ID NO: 1 are connected through chemical bonding, the membrane binding characteristic of oligomeric lysine and the transmembrane capacity of TAT cell-penetrating peptide are creatively fused, and a polypeptide carrier system with efficient cell penetrating capacity is constructed; mTX obtains amphipathy and electropositivity through peptide fragment modification, stable nanoparticles can be spontaneously formed, and the problems of poor water solubility and instable acidity of raw material medicines are effectively improved; according to the conjugate, the accumulation efficiency of the medicine at a diseased region is remarkably improved by utilizing the targeting characteristic of the polypeptide carrier, the action time of the medicine is prolonged through a precise delivery mechanism, and meanwhile, the system toxicity is reduced. The preparation method adopts mild coupling reaction conditions, and the product is high in purity and excellent in stability; the compound is suitable for treating immune-mediated inflammatory diseases and specific malignant tumors, and provides an innovative solution thought for treating related diseases.
Owner:CHINA PHARM UNIV

Preparation method of edaravone dextroborneol injection

The invention provides a preparation method of an edaravone and dextroborneol injection, the injection comprises edaravone, dextroborneol, propylene glycol and sodium pyrosulfite, in the preparation process, the propylene glycol accounting for 60%-85% of the prescription dosage and water accounting for 5%-25% of the prescription dosage are injected into a liquid preparation tank according to the volume ratio, the mixture is heated to 50-60 DEG C, edaravone is added and stirred to be dissolved, and the edaravone and dextroborneol injection is prepared. The preparation method comprises the following steps: dissolving propylene glycol in the remaining prescription dosage, adding dextroborneol which is dissolved by propylene glycol in the remaining prescription dosage in advance, uniformly stirring, adding water which is close to a constant volume, cooling to 25 DEG C or below, adding sodium pyrosulfite, adjusting the pH value to 4.0-5.0, and fixing the volume to a full volume. According to the preparation method of the edaravone dextroborneol injection, auxiliary materials in a specific proportion are matched with the preparation steps, the problem that raw material medicines are extremely easy to separate out in the preparation process is solved, the requirement of the preparation process for an industrial liquid preparation tank is low, industrial operation is convenient, and the preparation cost is low.
Owner:GUANGDONG YUEHEZE PHARM RES CO LTD

Method for determining content of various residual solvents in clozapine bulk drug by capillary gas chromatography

The invention discloses a method for determining the content of various residual solvents in a clozapine bulk drug by using capillary gas chromatography, and belongs to the technical field of drug analysis. According to the method, a gas chromatographic method is adopted, a capillary chromatographic column with 6% of cyanopropyl phenyl-94% of dimethyl polysiloxane as a stationary liquid is adopted, an FID detector is adopted for detection, and the content of the residual solvent is calculated by peak area according to an external standard method; wherein the multiple residual solvents are methanol, ethanol, isopropanol, n-amyl alcohol, n-butyl alcohol and toluene. The method disclosed by the invention is good in specificity, good in linearity, reliable in accuracy and high in sensitivity; the gas chromatographic method can be used for rapidly, effectively, accurately and reliably separating and detecting the content of various residual solvents in the clozapine raw material medicine, the product quality of the clozapine raw material medicine is improved, and the medication safety of a patient is improved.
Owner:JIANGSU CIXING PHARM CO LTD

On-line detection method for purity of bulk drug based on spectral data fusion

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.
Owner:HE BEI SHENG ZHONG YI YUAN (FIRST AFFILIATED HOSPITAL OF HEBEI UNIVERSITY OF TRADITIONAL CHINESE MEDICINE HEBEI CENTER FOR PREVENTION & CONTROL OF SCOLIOSIS IN CHILDREN & ADOLESCENTS)

Method for determining nitrosamine impurity N-nitrosobumetanib in bumetanib

The invention discloses a method for determining nitrosamine impurity N-nitrosobumetanib in bumetanib, which comprises the following steps: using a high performance liquid chromatograph and an ultraviolet detector, using octadecyl silane bonded silica gel as a chromatographic column filler, using formic acid solution as a mobile phase A, using methanol as a mobile phase B, the content of the nitrosamine impurity N-nitrosobumetanib in the bumetanib is determined through gradient elution. The novel high performance liquid chromatography is designed, the content of the nitrosamine impurity N-nitrosobumetanib in the bumetanib can be accurately measured, the blank that a method for measuring the N-nitrosobumetanib in the bumetanib bulk drug does not exist at present is filled, and the analysis method is verified; the method for determining the nitrosamine impurity N-nitrosobumetanib in the bumetanib, provided by the invention, is good in repeatability, high in selectivity, good in accuracy and high in precision and sensitivity; according to the invention, the quality control of the medicine can be effectively enhanced.
Owner:NINGBO DAHONGYING PHARM CO LTD

Preparation method of Alasset bulk drug

The invention relates to a preparation method of an ilastrant bulk drug, which comprises the following steps: taking a compound 1 as an initial raw material, carrying out Suzuki-Miyaura coupling reaction on the compound 1 and a compound a, and carrying out palladium-carbon reduction to obtain a key intermediate 6, so that the synthesis steps of the intermediate 6 can be shortened; subsequently, the intermediate 6 is subjected to chiral resolution and then is converted into an intermediate c through a Sandmeyer reaction, and a final product can be synthesized through a Buchwald-Harwig coupling reaction and a protection group removal. According to the invention, the reaction route is shortened, the cost is reduced, the reaction yield is improved, and the industrial production of the process is easier to realize.
Owner:LANZHOU KEJU BIOCHEMICAL CO LTD

UPLC-MS / MS (Ultra Performance Liquid Chromatography-Mass Spectrometry / Mass Spectrometry) detection method for N-nitroso landiolol in landiolol hydrochloride bulk drug

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.
Owner:BEIJING MEDISAN TECH +1

Detection method and application of related substances in sinomenine hydrochloride bulk drug

The invention belongs to the technical field of medicine detection, and particularly discloses a method for detecting related substances in sinomenine hydrochloride raw material medicine and application, and the method comprises the following steps: preparing a test solution; preparing a contrast solution; preparing a mixed impurity reference substance solution; according to the determination method, the five known impurities in the sinomenine hydrochloride raw material can be accurately and quantitatively analyzed, the impurity content of the sinomenine hydrochloride raw material can be more accurately and comprehensively reflected, and the quality of sinomenine hydrochloride can be better controlled.
Owner:HUNAN ZHENGQING PHARM GRP CO LTD +2

Method for high-yield preparation of icodextrin bulk drug by single enzyme system

The invention relates to a method for high-yield preparation of an icodextrin bulk drug by a single enzyme system, which comprises the following steps: gelatinizing starch at high temperature, adding alpha-thermoamylase for hydrolysis, carrying out ultrafiltration separation on primary enzymatic hydrolysate to obtain high-molecular-weight dextrin and alpha-thermoamylase, returning the high-molecular-weight dextrin and the alpha-thermoamylase to a gelatinization tank for secondary enzymolysis, and combining ultrafiltration permeates of the secondary enzymatic hydrolysate and the primary enzymatic hydrolysate, and performing molecular weight screening by ultrafiltration to obtain icodextrin of which the weight-average molecular weight and the number-average molecular weight simultaneously meet the requirements of alpha-1, 6 glucosidic bonds. On the basis of a traditional icodextrin manufacturing process, the working procedures of recovering macromolecular dextrin and performing secondary enzymolysis are added, and the yield can reach 85-91%. Particularly, new amylase does not need to be additionally added in the secondary enzymolysis, the original amylase is continuously used, new equipment is not added, the production cost increase is small, and the preparation efficiency is high.
Owner:QINGDAO UNIV OF SCI & TECH

A preparation method of enasidenib bulk drug

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.
Owner:UNIV OF JINAN

Method for detecting related substances of moxifloxacin hydrochloride bulk drug

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%.
Owner:TIANJIN CHASE SUN PHARM CO LTD

Process for the preparation of fenofibrate and its impurities

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.
Owner:ZHEJIANG SANMEN HYGECON PHARMA CO LTD

Icaritin carbamate prodrug, and preparation method therefor and use thereof

Provided are a preparation method for and the use of an icaritin carbamate prodrug and a salt thereof, which belong to the pharmaceutical field. In particular, provided are an icaritin carbamate prodrug represented by formula 3-N or 7-N and a pharmaceutically acceptable salt thereof, and a preparation method therefor and the use thereof. Specifically, the icaritin carbamate prodrug is formed by subjecting a main metabolic site (3-site or 7-site hydroxyl) of a natural flavonoid compound icaritin to structural modification by means of a chemical synthesis method, and introducing a suitable group at the position. Amines used in such carbamates are aliphatic amines. The presence of the carbamate structure reduces the phase II metabolism of icaritin in SD rats. Compared with an icaritin bulk drug, the 3-N-01 prodrug has a significantly improved oral bioavailability, making same the optimal prodrug. In clinical medication, the prodrug is expected to be able to reduce the administration dosage and improve patient compliance, and is expected to offer an effective strategy for improving the oral bioavailability of phenolic drugs.
Owner:SHENYANG PHARMA UNIV

Continuous preparation method of platinum bulk drugs

The invention discloses a continuous preparation method of a platinum bulk drug, which comprises the following steps: by taking chloroplatinite as a starting material, in a reaction environment of taking water as a solvent, replacing the starting material with iodized salt to obtain iodoplatinite, and then adding an amine ligand to quickly react to generate an intermediate-cis-diiodo-platinum-amine complex; introducing the solid-liquid mixed system containing the intermediate into a filtering and washing device, filtering and washing, directly discharging the solid into a reaction kettle, adding silver salt and water, reacting completely, and filtering; and concentrating the filtrate to obtain a crude product of the target product, and recrystallizing the crude product to obtain the platinum bulk drug. Or reacting the filtrate with a leaving group (or a salt formed by the leaving group) of the target compound, concentrating, filtering and washing to obtain a crude product of the target product, and recrystallizing the crude product to obtain the platinum bulk drug. The production efficiency and quality consistency of the product can be improved, the process amplification flow is simplified, the production cost and material consumption are reduced, green manufacturing is realized, and the method is an optimal choice for industrial production of platinum bulk drugs.
Owner:YUNNAN HENGXIN PHARM CO LTD