330 results about "Nitroso" patented technology

The present invention provides a pharmaceutical composition, the composition comprises a therapeutically effective amount of bumetanib, one or more specific antioxidants and other necessary one or more pharmaceutically acceptable pharmaceutic adjuvants, and the specific antioxidants are selected from one or more of fat-soluble vitamin C derivatives or phenolic antioxidants. In addition, the invention also discloses a method for improving the stability of the bumetanib pharmaceutical composition. According to the technical scheme, the problems of generation and growth of N-nitroso bumetanib and other related substances in the production and storage process of the bumetanib solid preparation are effectively solved, and the drug stability and the medication safety are remarkably improved.

The present invention relates to: a temperature-sensitive hydrogel for cancer treatment; a photothermal composition comprising the hydrogel as an active ingredient; and a preparation method for the temperature-sensitive hydrogel for cancer treatment. The temperature-sensitive hydrogel of the present invention includes gold nanostars as active ingredients, and thus can generate heat by light irradiation, thereby exhibiting a photothermal therapy effect. In addition, the hydrogel temperature increases so that the release of nitric oxide (NO) from S-nitrosocysteine can be induced. In addition, the temperature-sensitive hydrogel of the present invention includes S-nitrosocysteine as an active ingredient so that, upon a temperature rise due to a photothermal reaction, the penetration of drugs into a tumor site can be improved by the release of NO, and at the same time, apoptosis of cancer cells can be directly caused; and includes an immunotherapy agent as an active ingredient so that tumor size can be effectively suppressed even with the passage of time. Therefore, as a material that enables complex treatment combined with photothermal therapy and immunotherapy, the temperature-sensitive hydrogel of the present invention having the aforementioned effect can be usefully utilized in the field of medicine for cancer treatment.

The disclosure relates to a method of producing a multi-metal catalyst film and of producing a reactor system for catalytic removal of a wide variety of contaminants (for example, nitrate, nitrite, perchlorate, chlorate, chromate, selenate, chlorophenols, 2,4-D, dicamba, atrazine, trichloroacetic acid, bromochloroiodomethane, NDMA, TCE, TCA, chloroform, freons, RDX, HMX, TNT, PFOA, and PFOS) from water and wastewater. The disclosure also relates to a method of using the multi-metal catalyst for the removal of such contaminants and a system comprising the multi-metal catalyst film for removing such contaminants.

The invention provides a betahistine hydrochloride pharmaceutical preparation and a preparation method thereof. The betahistine hydrochloride pharmaceutical preparation comprises conjugated linoleic acid, betahistine hydrochloride and auxiliary materials. Conjugated linoleic acid and betahistine hydrochloride are combined together for the first time, and conjugated double bonds of conjugated linoleic acid can be specifically combined with nitrite to block the generation of nitrosamine, so that the content of N-nitrosobetahistine can be remarkably reduced. Based on the chemical characteristics of conjugated linoleic acid, conjugated linoleic acid is used as a functional additive, targeted removal of nitrosamine impurities is achieved, and meanwhile the situation that exogenous toxic substances are introduced to affect the drug effect of betahistine hydrochloride is avoided. In the experiment process, it is also accidentally found that after the conjugated linoleic acid is added, the positive effect on cerebrovascular diseases is also achieved.

This invention relates to N-(3-(6-Amino-5-(2-(N-methylacrylamido)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide drug substance substantially free of a nitrosamine impurity, e.g. the nitrosamine impurity N-(3-(6-amino-5-(2(methyl)(nitroso)amino)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide and novel processes of preparation thereof. The invention further relates to pharmaceutical composition comprising N-(3-(6-Amino-5-(2-(N- methylacrylamido)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide, wherein the composition is substantially free of a nitrosamine impurity, e.g. the nitrosamine impurity N-(3-(6-amino-5-(2(methyl)(nitroso)amino)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide. Pharmaceutical products containing said drug substance and compositions are also disclosed, as well as methods for preparing said drug substance, pharmaceutical compositions and products.

The invention relates to the technical field of medicines, relates to a preparation method and application of a genotoxic impurity standard substance in acarbose, and in particular relates to a preparation method and application of a genotoxic impurity N-nitrosyl acarbose in an acarbose tablet. According to the method, the nitrosamine new structure compound NNA is prepared for the first time, the genotoxic impurity NNA with high purity can be effectively prepared through the method, the blank of an impurity preparation method at present is filled, the preparation process is simple, and a large number of high-purity NAA impurity standard substances can be prepared. The invention provides a UHPLC-Orbitrap-HRMS (Ultra High Performance Liquid Chromatography-Orbitrap-High Resolution Mass Spectrometry) combined technology, so that the quality control of the NNA in the acarbose tablet is effectively realized, the side reaction of medication is reduced, and the medication safety is ensured to a certain extent. Meanwhile, reference is provided for quality evaluation of other starting materials or intermediates capable of generating NNA.

The invention relates to the technical field of hydrogel materials, in particular to NO controlled release polyvinyl alcohol / sodium alginate hydrogel and a preparation method thereof. The preparation method comprises the following steps: mixing and stirring a polyvinyl alcohol solution and a sodium alginate solution to obtain a mixed solution; s-nitroso-N-acetyl-penicillamine and graphene oxide are added into the mixed solution, the obtained solution is poured into a mold, hydrogel is obtained after freezing, the hydrogel is taken out of the mold and unfrozen at the room temperature, freezing and thawing cycles are repeated, and the polyvinyl alcohol / sodium alginate hydrogel capable of controllably releasing NO is obtained. According to the NO controlled release polyvinyl alcohol / sodium alginate hydrogel and the preparation method thereof, the prepared NO controlled release polyvinyl alcohol / sodium alginate hydrogel has excellent antibacterial property, conductivity, slow release property, mechanical property and biocompatibility, and the technical problems that existing hydrogel is insufficient in mechanical property and poor in antibacterial property are solved.

The invention belongs to the technical field of medicine detection, and particularly relates to a method for detecting a nitroso compound in a raw material medicine in a riptacaine emulsifiable paste, which comprises the following steps: preparing a test sample: taking the riptacaine emulsifiable paste, adding a 5mol / L sodium hydroxide solution, uniformly mixing, then adding a 5mol / L hydrochloric acid solution, and uniformly mixing; diluting with a solvent with the pH value of 7.20 + / -0.02, and then centrifugally filtering to obtain a test sample; wherein the solvent is a mixed solvent composed of monopotassium phosphate and acetonitrile; liquid chromatography separation: the tested sample is separated by liquid chromatography, and a mobile phase A is a 0.2% formic acid solution; the mobile phase B is methanol; the chromatographic column is SB-C18, 2.1 * 100 mm, 1.7 [mu] m; and mass spectrum detection: detecting the substance separated by the liquid chromatography by using a mass spectrometer to obtain the content of the nitroso compound. The detection method is efficient, sensitive and excellent in reproducibility.

The invention discloses a fermentation process for shortening a fermentation period and efficiently synthesizing Ectoine. The fermentation process comprises the following steps: screening and activating high-yield strains, preparing a fermentation culture medium, performing fermentation culture, performing sectional dissolved oxygen regulation and control, performing double-stage pH dynamic regulation and control, performing carbon-nitrogen ratio dynamic regulation based on metabolic flow analysis, performing osmotic pressure gradient induction in the later stage of fermentation, and extracting and purifying a product. According to the fermentation process for shortening the fermentation period and efficiently synthesizing the Ectoin, the expression quantity of key enzymes for synthesizing the Ectoin is increased by 80% or above compared with that of an original strain through the Halomonassp.ECT-09 strain bred through ultraviolet-nitrosoguanidine compound mutation, the basic yield reaches 35 g / L, a foundation is laid for high yield, and the method is suitable for industrial production. A glucose-trehalose mixed carbon source and a yeast extract-ammonium nitrate mixed nitrogen source are adopted, and an L-aspartic acid-L-asparagine mixed precursor is added, so that the metabolic pathway is shortened, and the loss of an intermediate product is reduced.

Disclosed is a process for the synthesis of mono- and bis-nitrosylated propanediols, as well as compositions and pharmaceutical formulations that includes the compounds. The process proceeds by reacting a corresponding propanediol that is not nitrosylated with a source of nitrite, optionally in the presence of a suitable acid. When the source of nitrite is an organic nitrite, reacting step is performed in a suitable organic solvent, and when the source of nitrite is an inorganic nitrite, the reacting step is performed in a bi-phasic solvent mixture comprising an aqueous phase and a non-aqueous phase. Also disclosed are methods of treating a condition wherein administration of nitric oxide (NO) has a beneficial effect by administering said compounds, compositions or formulations.

The invention belongs to the technical field of medicines, and particularly relates to bletilla striata polysaccharide hydrogel as well as a preparation method and application thereof. The BSP-MA / HA-NB hydrogel is prepared by screening the variety, dosage and preparation process of each component in the hydrogel, and the hydrogel is prepared from the following raw materials: methacrylated bletilla striata polysaccharide, o-nitrobenzaldehyde modified hyaluronic acid and the like. The adhesive property and the mechanical property of the hydrogel are obviously improved; the long-acting slow-release effect of the medicine components is achieved, the proliferation activity and migration ability of the bone marrow mesenchymal stem cells are promoted, and the bone marrow mesenchymal stem cells have good application prospects in the aspect of bone defect repair treatment.

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 invention discloses a method for detecting an N-nitroso compound in vortioxetine hydrobromide, and the N-nitroso compound is 2, 2 '-(nitroso amino) bis-acetonitrile. According to the method, a high performance liquid chromatography is adopted, an octadecyl silane bonded silica gel filler chromatographic column and an ultraviolet detector are adopted, a mobile phase A is 0.05% phosphoric acid aqueous solution, a mobile phase B is methanol, and gradient elution is adopted. The method has good specificity and sensitivity.

The invention discloses a method for determining nitrosamine impurity N-nitrosociprofloxacin in ciprofloxacin lactate, and relates to the field of substance detection methods, the method adopts a liquid chromatography-mass spectrometry technology, and the liquid chromatography condition comprises that a mobile phase is a mixture of a formic acid solution with the concentration of 0.08%-0.12% and acetonitrile, and the volume ratio of the formic acid solution to the acetonitrile is (45-55): (45-55). According to the present invention, the liquid chromatography (LC) technology and the mass spectrometry (MS) technology are combined, such that the efficient separation ability of the liquid chromatography and the high sensitivity detection ability of the mass spectrometry are combined, the detection sensitivity and the detection accuracy are significantly improved, and the strict requirements of drug quality control and safety are met.

This application relates to a rifapentine-containing pharmaceutical composition and its preparation method. The rifapentine-containing granules are prepared by dry granulation, which reduces the content of impurities present in existing pharmaceutical compositions, especially the content of the genotoxic impurity 1-cyclopentan-4-nitrosopiperazine, thereby improving the safety and efficacy of the drug.

The invention provides a sterile, injectable pharmaceutical composition which includes a therapeutically effective amount of ketamine or a pharmaceutically acceptable salt thereof, a nitrite scavenger, a tonicity agent, and water, wherein the composition contains less than about 300 ppb of an N-nitrosoketamine impurity. The invention also provides a pharmaceutical product which includes a container and the composition of the invention aseptically sealed therein. The invention further provides a process for preparing the composition and product of the invention.

The present invention relates to a method for preparing nitrosamine impurities in vonoprazan fumarate, belonging to the technical field of chemical synthesis. By mixing vonoprazan with an organic solvent and reacting the mixture with a nitrosating agent at room temperature, the nitrosamine impurities prepared by this method have a purity exceeding 85%. This method solves the problem of preparing nitrosamine impurities and also provides a reference substance for the study of impurities in vonoprazan fumarate.

The invention discloses a detection method of vitamin K1, and belongs to the technical field of biological detection. The problems that a vitamin K1 detection method is tedious in operation, prone to being influenced by a matrix, low in sensitivity and the like are solved. The detection method comprises the following steps: (1) preparing a standard substance intermediate working solution, an isotope internal standard substance solution and a standard curve working solution of the vitamin K1; (2) treating a serum sample and a standard curve working solution: adding a 2-nitroso pyridine solution to carry out derivatization reaction; and (3) detecting the vitamin K1 by using a high performance liquid chromatography-tandem mass spectrometry method. According to the method, the 2-nitroso pyridine is used as a derivatization reagent, the vitamin K1 and the 2-nitroso pyridine are subjected to a Diels-Alder reaction to generate a new six-membered heterocycle containing N and O, the 2-nitroso pyridine can efficiently and completely react with the vitamin K1 in only 10 minutes at room temperature, the detection steps are simplified, the sample pretreatment time is shortened, and the detection efficiency is improved.

The invention provides a method for continuously and efficiently synthesizing 2, 6-diamino piperazine-1-oxide, which comprises the following steps: S1, preparing an N-nitroso iminodiacetonitrile solution at room temperature, and stirring and dissolving for 5 minutes; s2, sequentially adding hydroxylamine salt and alkali into a solvent, stirring at room temperature for 10-15 minutes for pre-dissolving, adding a proper amount of metal salt catalyst into the obtained solution, and continuously stirring for 5-10 minutes; s3, exhausting the continuous tubular reactor by using a hydroxylamine solution until the continuous tubular reactor is full of the solution; s4, feeding the N-nitrosoiminodiacetonitrile solution and the hydroxylamine solution into a continuous tubular reactor through a mixer according to a certain proportion by adopting a delivery pump, and optimizing the flow velocity and temperature of the reaction solution and the pressure in the continuous tubular reactor; and S5, enabling the reaction liquid to flow out from an outlet of the continuous tubular reactor, performing suction filtration, washing a filter cake with an alcoholic solution, and drying. The method can obviously improve the reaction rate, reduce the generation of impurities and improve the production efficiency.

The invention relates to a method for reducing harmful components in cigarette smoke by using food-grade cyclodextrin metal organic framework materials, which is characterized in that two food-grade cyclodextrin metal organic framework materials CD-MOFs are added into cigarette filters for reducing the harmful components in the cigarette smoke. The unique pore structure and rich hydroxyl functional sites of the gamma-cyclodextrin-KOH and the beta-cyclodextrin-KOH are utilized to efficiently adsorb various harmful components in the mainstream smoke of the cigarette. Compared with a control group without any adsorbent and a control group with only activated carbon as the adsorbent, the CD-MOFs has efficient capturing capability on harmful gases such as carbon monoxide, nitrosonicotine, ammonia gas, benzo [a] pyrene and phenol in the cigarette smoke, and can obviously reduce the cigarette hazard index. The two materials are simple in preparation process, high in cost benefit and good in chemical stability, are food-grade porous materials and have incomparable practical application potential compared with traditional non-food-grade porous materials, and an effective solution is provided for developing novel low-harm cigarette products.

The invention provides a preparation method of high-purity nicotine. The content of nitroso substances in an obtained nicotine finished product is lower than the PPB level, and the content of single heavy metals such as lead, cadmium, mercury and hexavalent chromium is also lower than the PPB level. The low-content nitroso substance concentration and heavy metal concentration can effectively reduce the harm of the synthesized nicotine to the human body, and the method provided by the invention can realize continuous industrial production of nicotine, and fills the blank of the demand of the market for high-purity L-nicotine.

The invention provides an aqueous zinc ion battery electrolyte and an aqueous zinc ion battery, the aqueous zinc ion battery electrolyte comprises pure water, soluble zinc ion salt and an additive, and the additive is 1-nitroso-2-naphthol-6-sodium sulfonate ferric salt. The 1-nitroso-2-naphthol-6-sulfonic acid group generated by ionization in the electrolyte can be directionally adsorbed on the surface of a zinc negative electrode, so that dendritic crystal growth and hydrogen evolution reaction on the surface of the negative electrode are inhibited; fe < 3 + > ions generated by ionization can be embedded into the positive electrode material in the battery circulation process, and the capacity of the battery is improved, so that the problem of capacity fading in the battery circulation process is solved, and the circulation stability of the battery is improved.

The invention discloses a method for detecting nitro10-nitrosofolinic acid in calcium folinate injection by liquid chromatography. According to the method, a phenyl column is used as a chromatographic column, a 0.1% formic acid aqueous solution is used as a mobile phase A, methanol is used as a mobile phase B, a gradient elution mode is adopted, and an ion source is ESI (+). The method has the advantages of good specificity and stable separation effect, is suitable for determining nitrogen-10-nitrosofolinate in the calcium folinate injection, and has the sensitivity of 0.09 ppm.

The application discloses an electrolytic synthesis method of a pyrazolone compound intermediate, and the method uses a nitroso acid ester compound as raw material to obtain an electrolyte containing a hydrazine compound through electrochemical reduction; the electrolyte containing the hydrazine compound is subjected to a cyclization reaction to obtain a pyrazolone compound; the application uses a mild and efficient electrochemical reduction mode to replace a high-risk diazotization reaction to synthesize the pyrazolone compound; the electrolyte can be recycled for multiple times, and a large amount of sulfite, acid and other reagents needed in the synthesis process are avoided, and a large amount of 'three wastes' is reduced. The method has better product purity (> 95%) and yield (> 80%), the method is more green and environmental protection, no three wastes are generated, and is suitable for industrial production.

This invention relates to the field of organic synthesis technology, specifically to a method for preparing aryltriazene; comprising the following steps: (1) preparing an aromatic nitroso compound Ar 1 NO is dissolved in the first solvent in the first ratio to obtain solution A; (2) unsymmetrical disubstituted hydrazine R 1 R 2 NNH2 is dissolved in the second solvent in the second ratio to obtain solution B; (3) under stirring, solution A and solution B are mixed and subjected to dehydration condensation reaction for 1-4 hours, and the reaction temperature of dehydration condensation is 10-40℃; after the reaction is completed, aromatic triazine is obtained by separation and purification; the first solvent and the second solvent are aprotic solvents; Ar 1 It is any of the substituted or unsubstituted phenyl, heterocyclic aryl, and fused-ring aryl groups, and the substituents on the ring do not react with hydrazine; R 1 R 2 It is at least one of alkyl and aryl groups. This preparation method is simple to synthesize, produces no unstable diazonium salt intermediates, has mild reaction conditions, and a relatively fast reaction rate.

The application discloses a hydroxylamine hydrochloride detection method in azithromycin dry suspension, and relates to the trace detection field. The method uses isoamyl aldehyde as a derivatizing agent, generates isoamyl aldoxime by performing derivatization treatment on a sample to be measured, and then uses N-nitrosodiisopropylamine as an internal standard substance to quantitatively determine the isoamyl aldoxime by using liquid chromatography-tandem mass spectrometry. The detection method adopts an isoamyl aldehyde derivatizing agent-N-nitrosodiisopropylamine internal standard substance system, can correct detection errors caused by factors such as matrix effect, pretreatment loss and derivatization efficiency fluctuation, and improves the accuracy and sensitivity of the trace hydroxylamine hydrochloride detection result, thereby guaranteeing the safety of the medicine.

The present invention discloses the application of bio-gelatin modified with o-nitroso benzaldehyde group in the preparation of drugs for preventing or treating inflammatory bowel disease; the bio-gelatin modified with o-nitroso benzaldehyde group is prepared by the following method: S1. Add 4-(4-hydroxymethyl-3-nitro-2-methoxyphenoxy) butyric acid into the aqueous gelatin solution, and react the carboxyl group in 4-(4-hydroxymethyl-3-nitro-2-methoxyphenoxy) butyric acid with the amino group in gelatin to obtain bio-gelatin modified with o-nitrobenzyl alcohol group; S2. After irradiating the bio-gelatin modified with o-nitrobenzyl alcohol group with a near-ultraviolet light source, it is converted into bio-gelatin modified with o-nitroso benzaldehyde group. The present invention uses bio-gelatin modified with o-nitroso benzaldehyde group for preventing or treating inflammatory bowel disease, which can form a uniform, dense and stable coating on the intestinal surface and has good preventive and therapeutic effects on inflammatory diseases.

This invention provides a nitric oxide generating device and a method for manufacturing the same. [Solution] In an exemplary method, a solution is introduced into the lumen of a nitric oxide permeable polymer object. The solution contains a solvent and S-nitroso-1-adamantanethol dissolved in the solvent. The solution is immersed in the lumen of the nitric oxide permeable polymer object for a maximum of 12 hours. The solution is then removed from the lumen of the nitric oxide permeable polymer object.

The invention discloses a method for preparing p-trifluoromethoxyphenol by adopting a micro-channel reactor, and belongs to the field of fine chemical engineering. 4-trifluoromethoxyaniline and dilute sulphuric acid are pumped into the first micro-channel reactor for a reaction; then introducing inert gas, pumping the nitroso sulfuric acid solution, and carrying out diazotization reaction to obtain a diazonium salt solution; pumping the diazonium salt solution into a second micro-channel reactor, carrying out hydrolysis reaction, adding dichloroethane extract liquor into a rectifying tower after the reaction is ended, and rectifying to obtain p-trifluoromethoxyphenol; porous baffles which are inclined downwards are arranged on the inner wall of the rectifying tower in a crossed manner; a heat-conducting filler layer of 50-100 nm is arranged on the porous baffle plate; the heat-conducting filler layer is a three-dimensional net-shaped material layer which is formed by boron nitride nanosheets / titanium oxide nanorods and has a porous structure. The method is simple in process route, convenient to operate, high in controllability, high in safety, high in reaction efficiency, high in product yield, capable of effectively reducing the solid waste amount in production, energy-saving, environment-friendly and suitable for industrial production.

The invention provides a cleaning and preserving fluid for fetal brain tissues and a preserving method thereof, and belongs to the technical field of tissue preservation. The cleaning and preserving fluid comprises trehalose, nerve growth factors, a GlutaMAX supplement, Y27632, S-nitrosoglutathione, tert-butylhydroquinone, a Versene solution and polyvinylpyrrolidone, compared with a traditional tissue preserving fluid, the cleaning and preserving fluid not only can improve the purity of neural stem cells, but also can maintain the activity and the yield of the neural stem cells in fetal brain tissue, and the cleaning and preserving fluid has the advantages that the cleaning and preserving fluid is simple in structure and convenient to use. The structural integrity of the cells is guaranteed, a high-quality sample is provided for subsequent research on proliferation, differentiation and the like of the neural stem cells, and the method has a wide application prospect.