234 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 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 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 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 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 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.

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 relates to a method for determining the content of nitrosamine impurities in a pramipexole dihydrochloride sustained-release tablet, which comprises the following steps: grinding the pramipexole dihydrochloride sustained-release tablet into fine powder as a sample to be detected, and extracting with a diluent to obtain a test solution; and carrying out liquid chromatography-mass spectrometry detection on the test solution, and calculating according to the detection result to obtain the content of the nitrosamine impurity N-nitroso-pramipexole in the pramipexole dihydrochloride sustained release tablet. According to the method, the nitrosamine impurity N-nitroso-pramipexole can be effectively extracted from the pramipexole dihydrochloride sustained release tablet, and the nitrosamine impurity is quantitatively detected by liquid chromatography-mass spectrometry, so that the problems that the nitrosamine impurity N-nitroso-pramipexole is low in content, difficult to detect and easy to interfere are successfully solved. The method is high in accuracy, precision and sensitivity and good in linearity, specificity and system adaptability.

Systems and methods are provided for non-invasive measurement of endogenous S-nitrosothiols and related measurements thereof. One or more sensors non-invasively measures a set of one or more biometric parameters within a region of interest of a subject to provide a time series of measurements for each of the set of biometric parameters. A medium stores machine-readable instructions that are executable by an associated processor to perform processing comprising receiving the time series of measurements of the biometric parameter, generating, using a predictive model, a value representing an endogenous S-nitrosothiol content of tissue within the region of interest from the time series of measurements of the biometric parameter, and providing, by a user interface, the value representing the endogenous S-nitrosothiol content of tissue within the region of interest to a user.

The invention relates to the technical field of flocking adhesives, in particular to a high-performance single-component flocking adhesive and a preparation method thereof.The high-performance single-component flocking adhesive is at least prepared from, by mass, 40-60% of blocked polyurethane, 5-15% of phenol novolac epoxy resin, 0-5% of aromatic nitroso compounds, 0-5% of imine compounds and the balance solvent, the closed polyurethane has an oxime carbamate structure, the weight-average molecular weight is 60000-90000, by optimizing a product formula system, the problems of poor wear resistance, poor solvent resistance and the like after an adhesive is coated are effectively solved, meanwhile, the operation is convenient and fast, the efficiency is high, the application scene and the application range of the adhesive are expanded, and the market demand is better met.

The invention discloses a method for removing trace or trace N-nitrosodimethylamine in water by using a self-assembled metal coordination polymer catalytic membrane. The self-assembled metal coordination polymer catalytic membrane material is added into a reaction flask of an N-nitrosodimethylamine solution subjected to nitrogen deoxidation treatment, the amount of loaded zero-valent iron is 25.7 mg / g to 171.4 mg / g, and the initial concentration of N-nitrosodimethylamine is 47.4 mu g / L to 196.5 mu g / L. The reaction bottle is sealed and then placed on a multi-point intelligent magnetic stirrer for magnetic stirring reaction, the rotating speed is 200 rpm, the temperature is 25 DEG C, the pH is 2.5-9.5, and stirring is conducted for 1.5 h. A carboxylated high-molecular polyacrylonitrile membrane is used as a base material, poly (diallyldimethylammonium chloride) polycation and polyacrylic acid polyanion electrolyte are assembled on the surface of the base membrane by adopting an electrostatic self-assembly technology, and the high-molecular self-assembled composite membrane with a large number of carboxyl groups is prepared. And preparing the self-assembled metal coordination polymer catalytic membrane through a metal-polycation electrolyte coordination technology and a classical liquid phase reduction method. The content of iron in the self-assembly metal coordination polymer catalytic membrane and the thickness of a surface functional layer are conveniently and effectively regulated and controlled by controlling the number of assembly layers, the concentration of iron ions in coordination reaction, the pH value of the solution and the like, high activity and stability are kept, and the method has the advantages of being simple in preparation process, low in cost, high in removal rate and the like.

This invention discloses a method for synthesizing 2,6-difluorophenyl-1-(4,5-dihydroisoxazole)-3-ethyl ketone. The method uses compound 1, acetylacetone, as the starting material. First, compound 2, 3-isonitroso-2,4-pentanedione, is prepared. Then, compound 2 undergoes oxidation to give a 1,3-dipolar compound, which undergoes a 1,3-dipolar cycloaddition reaction with an olefin to obtain 2,6-difluorophenyl-1-(4,5-dihydroisoxazole)-3-ethyl ketone. The process of this invention is simple, the raw materials are readily available, the yield is high, and it is environmentally friendly, making it very suitable for industrial production.

This invention belongs to the field of biomedical materials and nanotechnology, specifically relating to the synthesis and application of a multifunctional mesoporous nanomaterial. The inventors synthesized a core-shell structured mesoporous nanoparticle using mesoporous silica nanoparticles and dopamine via emulsion epitaxy. The core of the core-shell structured mesoporous nanoparticle is S-nitrosoglutathione supported on mesoporous silica, and the outer shell is pentafluorophenyl chlorophyll supported on mesoporous polydopamine, forming MSN / G@mPDA / F nanoparticles. These nanoparticles rapidly increase in temperature to 45°C under 808 nm laser irradiation. o At temperatures above a certain temperature, S-nitrosoglutathione decomposes to produce nitric oxide. Further irradiation at 750 nm generates a large amount of reactive oxygen species, killing bacteria. This combination of photothermal and photodynamic therapy effectively inhibits bacterial growth. Therefore, this method exhibits excellent antibacterial effects and can play a role in the future treatment of bacterial infections.

The application discloses indazole nitrogen oxide and a synthesis method and anticancer activity application thereof, and belongs to the technical field of organic synthesis and drug discovery. N-nitrosoaniline compound 1, diazindione compound 2, a catalyst, an additive and hexafluoroisopropanol are mixed, and the mixture is reacted by temperature rising to obtain indazole nitrogen oxide. The chemical structure of the indazole nitrogen oxide is as follows: researches show that the indazole nitrogen oxide has the activity of inhibiting the proliferation of Hela, A549 and HCT-116 cancer cells, and has potential medicinal value. Meanwhile, the synthesis method provided by the application is completed by one-pot multi-step tandem reaction, and the process is simple and efficient. The synthesis method has the following remarkable characteristics: raw materials are cheap and easy to obtain, the product is valuable, the steps are economical and atomic economy is high.

In an embodiment, there is provided a varenicline formulation consisting essentially of about 0.85% varenicline tartrate and greater than 1.75% to about 3.0% propyl gallate, wherein the formulation maintains a level of N-nitrosovarenicline (NNV) impurity over the shelf-life of the formulation of not more than 18.5 ppm (37 ng / day) of acceptable daily intake (ADI). In another embodiment, there is provided a varenicline formulation comprising a tablet core comprising about 0.85% varenicline tartrate, about 60.50% microcrystalline cellulose, about 33.33% dibasic calcium phosphate anhydrous, about 2.00% croscarmellose sodium, about 2.57% propyl gallate, and about 0.75% magnesium stearate; and a film coating.

A method includes mixing a liquid carrier and a powder formulation including an S-nitrosothiol (RSNO) powder to form a nitric oxide generating solution; and within a predetermined time of mixing, introducing the nitric oxide generating solution into an inflatable and nitric oxide permeable balloon of a urinary catheter that is inserted in a patient.

The application provides application and synthesis of a water-based polyurethane composition in an environmentally-friendly product capable of long-term air tightness. The composition is used in products that need long-term inflation pressure maintaining and are environmentally-friendly and non-toxic; the long-term inflation pressure maintaining air tightness of the product is that, after being sealed, the product is filled with helium to the size of a mold in a constant temperature and humidity environment (25 DEG C, 50% humidity), the size is maintained for more than 90% of time for greater than or equal to 7*24h; the N-nitroso content in the product is 0-0.5mg / kg. The synthesis method is as follows: a low-boiling-point organic solvent is added to an isocyanate-terminated prepolymer, a dibasic amine chain extender is added, a neutralizing agent is added after chain extension, water dispersion is added under high-speed shearing, the water-based polyurethane coarse emulsion is obtained after the end, and the low-boiling-point organic solvent is removed. The product has excellent long-term air tightness, is environmentally-friendly and non-toxic, and can meet the application requirements in high-performance products with excellent long-term air tightness, environmental friendliness and non-toxicity.

This invention relates to a new process for preparing N-(3-(6-Amino-5-(2-(N- methylacrylamido)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2- fluorobenzamide (LOU064) drug substance substantially free of nitrosamine impurities as well as new crystalline forms of salt and solvate of LOU064 used in the process. 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 discloses a method for detecting the impurity content of ticagrelor, the impurity is N-nitrosoticagrelor, and the detection method comprises the following steps: diluting an initial sample, and preparing to obtain a detection sample; a detection sample enters a mobile phase through a sample injector, a chromatographic column with phenyl-hexyl bonded silica gel particles as a filler is adopted to carry out gradient elution treatment on the detection sample to obtain an eluted sample, the mobile phase comprises an organic phase and a water phase, and the gradient elution conditions comprise that in the first stage, the ratio of the organic phase to the water phase is in direct proportion to the duration; in the second stage, the ratio of the organic phase to the water phase is the ratio at the end of the first stage; in the third stage, in the mobile phase, the ratio of the organic phase to the water phase is inversely proportional to the duration; a fourth stage, in the mobile phase, the ratio of the organic phase to the water phase is the ratio at the end of the third stage, and the ratio of the organic phase to the water phase in the fourth stage is smaller than the ratio of the organic phase to the water phase in the second stage; and performing mass spectrometry analysis on the eluted sample to determine the components of the eluted sample.

The application belongs to the technical field of fluorescent probe, and particularly relates to a non-oxygen-dependent multi-mode selenium rhodamine-based photodynamic photosensitizer as well as preparation and application. In order to develop a non-oxygen-dependent and efficient photosensitizer, based on the selenium rhodamine spiro ring 'on-off' mechanism, a N-nitroso functionalized selenium rhodamine photosensitizer SeR-NO is developed, which exists in the form of lactone with closed ring in PBS, has very small cell dark toxicity and excellent cell permeability; under light, the photosensitizer can not only produce a large amount of ROS through type I and type II mechanism, but also can catalyze NADPH oxidation and Cyt c reduction in an oxygen-independent manner, therefore, SeR-NO has large phototoxicity, and can induce cell death through ferroptosis in normoxia (21% O2) and hypoxia (2% O2).