14 results about "Nitrosamine compound" patented technology

Provided are compositions comprising certain miglustat-related nitrosamine compounds, such as pharmaceutical compositions comprising miglustat and such miglustat-related nitrosamine compounds. Also provided are pharmaceutical compositions comprising miglustat and less than certain levels of such miglustat-related nitrosamine compounds. Also provided are methods of analyzing such miglustat-related nitrosamine compounds.

The application belongs to the technical field of substance analysis and detection, and provides an extraction method and a detection method for N-nitrosamine compounds in aquatic products. The N-nitrosamine compounds in the aquatic products to be measured are extracted by steam distillation, and the extraction rate of the N-nitrosamine compounds is high. The obtained distillate is purified and enriched by using an acid-modified coconut shell activated carbon column, the acid-modified coconut shell activated carbon column can effectively adsorb N-dimethyl-nitrosamine and N-diethyl-nitrosamine in the distillate, the acid-modified coconut shell activated carbon column is first eluted with n-hexane to remove part of the fat-soluble impurities, then N-dimethyl-nitrosamine and N-diethyl-nitrosamine are eluted with dichloromethane, due to the strong adsorption of the acid-modified coconut shell activated carbon column to the impurities, the impurities are not easily eluted by dichloromethane, so that the impurities, N-dimethyl-nitrosamine and N-diethyl-nitrosamine are effectively separated, and the purpose of purification is achieved.

Provided are compositions comprising certain miglustat-related nitrosamine compounds, such as pharmaceutical compositions comprising miglustat and such miglustat-related nitrosamine compounds. Also provided are pharmaceutical compositions comprising miglustat and less than certain levels of such miglustat-related nitrosamine compounds. Also provided are methods of analyzing such miglustat-related nitrosamine compounds.

The invention provides a method for detecting the genetic toxicity of nitrosamine compounds, and belongs to the technical field of biological detection. According to the method, key conditions of a detection system are systematically optimized, so that the detection sensitivity and the result reliability of the genotoxicity of the nitrosamine compounds are remarkably improved, and the mutagenicity which is difficult to detect under conventional conditions can be stably and clearly identified; the establishment of the method provides powerful technical support for early screening and safety risk assessment of nitrosamine impurities in drugs and chemicals, and has important practical application value for guaranteeing medication safety and product quality.

The invention belongs to the technical field of environment detection and analysis, and particularly relates to a method for detecting trace N-nitrosamine compounds in water. According to the method, a headspace solid-phase microextraction device with a dehydration and heat insulation device is used for extraction, the dehydration and heat insulation device is installed between a to-be-detected sample container and an extraction handle, the dehydration and heat insulation device comprises a double-layer quartz tube, degreasing cotton and a dehydrating agent, and the degreasing cotton with the dehydrating agent is placed at the top end of a ventilation connecting pipe of the dehydration and heat insulation device; and the bottom end of the ventilation connecting pipe is arranged above the to-be-tested sample. After the dehydration and heat insulation device is additionally arranged, the extraction temperature and the stirring speed can be increased, the extraction time is saved, and the problems of damage to an extraction head and a gas chromatographic column and desorption caused by water vapor adsorption possibly caused by too high temperature are solved; and the gas space above the liquid level is reduced by using the dehydration and heat insulation device, the adsorption of an object to be detected in a gas environment is promoted, the detection limit reaches 0.05-0.1 ng / L, and the recovery rate is 90-103.2%.

The invention discloses a method for determining N-nitrosamine compounds in animal-derived food, and belongs to the field of food detection. The method comprises the following steps: freezing and grinding animal-derived food, mixing the animal-derived food with an internal standard solution, deionized water and acetonitrile, and freezing and preserving to obtain a pretreated sample; the method comprises the following steps: treating a pretreated sample through a QuEChERS salt bag, centrifuging, carrying out nitrogen blowing concentration, and mixing with deionized water to prepare an enriched solution; purifying the enriched solution by adopting a purification bag or specific functional resin, and centrifugally filtering to obtain a sample solution; and calculating the content of the target compound through a peak area ratio by using a liquid chromatograph-high resolution mass spectrometer provided with an APCI source and taking N-nitrosodimethylamine-D6 as an internal standard. The functional resin is formed by cross-linking specific functional monomers and is large in specific surface area and high in adsorption selectivity; the method has strong anti-interference capability, and can efficiently detect the N-nitrosamine compounds in dried aquatic products and other animal-derived foods.

The invention relates to the technical field of medicine preparation, in particular to a synthesis method of dalbavancin demethylated B2 nitrosamine. The synthesis method comprises the following steps: S1, taking a dalbavancin precursor A-40926-B0 as a raw material, and carrying out methylation reaction to obtain an intermediate I; s2, performing esterification protection on the intermediate I to obtain an intermediate II; s3, carrying out condensation reaction on the intermediate II and 3-methylaminopropylamine to obtain an intermediate III, and carrying out alkaline hydrolysis to obtain an intermediate IV; s4, carrying out nitrosation on the intermediate IV through a nitrosation reagent to obtain dalbavancin demethylated B2 nitrosamine; the synthesis method is high in reaction yield, the purity of the demethylated B2 nitrosamine compound of the dalbavancin can be as high as that of the dalbavancin, and a reference substance is provided for quality control of the dalbavancin.

The application discloses an organic boron reagent alpha-boryl oxime compound and a preparation method and application thereof, and belongs to the technical field of organic synthesis. N The alpha-boryl oxime compound is prepared by reacting a heterocyclic carbene borane adduct and a nitroso compound in an organic solvent. N The alpha-boryl oxime compound is prepared by simultaneously introducing an oxime group and a boron group functional group into both ends of the olefin with high selectivity through the boro-oximation reaction of the heterocyclic carbene borane, the nitrosamine compound and the olefin. The reaction avoids the use of a photosensitizer and a transition metal, has very good functional group tolerance and substrate universality, and also has good chemical selectivity, regioselectivity and stereoselectivity; the product alpha-boryl oxime compound can be efficiently used to synthesize various useful compounds through simple conversion, the types of the organic boron reagent are expanded, and the application prospect is good.

The invention relates to the technical field of medicine preparation, in particular to a method for preparing a nitrosamine compound. The method comprises the following steps: S1, carrying out esterification protection by taking a dalbavancin precursor A-40926-B0 as a raw material to obtain an intermediate I; s2, carrying out condensation reaction on the intermediate I and 3-methylaminopropylamine to obtain an intermediate II, and carrying out alkaline hydrolysis to obtain an intermediate III; s3, protecting secondary amine on a parent nucleus of the intermediate III through a protective reagent to obtain an intermediate IV; s4, carrying out nitrosation on the intermediate IV through a nitrosation reagent to obtain an intermediate V; s5, after the intermediate V is subjected to deprotection, dalbavancin demethylated B0 nitrosamine is obtained; the product prepared by the method is high in purity, a reference substance can be provided for quality control of dalbavancin, and important guiding significance is provided for safe medication.

The invention discloses a biomass-based fluorescent material as well as a preparation method and application thereof. The biomass-based fluorescent material comprises a matrix material and AIE fluorescent molecules bonded on the matrix material. According to the method, the fluorescence quenching effect of the tobacco-specific nitrosamine compound on the water-soluble cellulose derivative is utilized, the tobacco-specific nitrosamine compound with extremely low content in a normal tobacco product cannot be identified, and a counterfeit product generates macroscopic fluorescence change due to overhigh concentration; therefore, the authenticity of the tobacco material can be quickly and visually identified. Through the enrichment effect of the fluorescent cellulose microspheres and the electrostatic interaction between the fluorescent cellulose microspheres and to-be-detected molecules, a portable detection system capable of rapidly, sensitively and repeatedly identifying the authenticity of the tobacco is provided on the basis of the specific quenching of the nitrosamine compound specific to the tobacco on the fluorescence of the cellulose microspheres.

This invention discloses nitrosamine compounds, their preparation methods, their application in the detection of varenicline tartrate raw materials or preparations, and detection methods. Specifically, this invention discloses providing the compound shown in formula P08, its preparation method, detection method, and its application in the preparation of bactericidal drugs, as an insecticide, and further, its application as a standard, reference standard, or detection item in the impurity study, quality control, or detection methods of varenicline tartrate raw materials or preparations.

The invention provides a detection and analysis method of an N-nitrosamine compound, and N-nitrosamines with different structures can be measured through chemical derivatization reaction. In the embodiment of the application, a sample derivatization method is studied, and optimal reaction conditions for the N-nitrosamine compound are provided. The invention establishes a liquid chromatography-triple quadrupole mass spectrometry technology, and successfully establishes a derivatization analysis method for N-nitrosamine compounds with different structures. The method has high selectivity, sensitivity and accuracy, and meets the requirements of trace detection of complex samples and nitrosamine compounds with complex structures.

Disclosed is a method for removal of contaminating nitrosamine compounds from pharmaceutical ingredients. More specifically, this method may be used to remove both small-molecular weight nitrosamines and nitrosamine drug substance-related impurities (NDSRIs) from pharmaceutical ingredients. In an embodiment, the contaminated pharmaceutical ingredient is suspended or dispersed into an appropriate solvent and treated with a defined wavelength and intensity of light for a period of time, followed by recovery of the pharmaceutical ingredient by solvent exchange precipitation, or other method. The method is efficient and cost-effective and applicable to the entire drug synthesis process, from raw ingredients to final active pharmaceutical ingredient, or excipients used in drug product formulations. It provides a standardized approach for combatting the risk of carcinogenic nitrosamine contaminant drugs. In another embodiment a process is disclosed that provides for a streamlined method to tune the reaction conditions of the method to minimize or eliminate any degradation of the pharmaceutical product during nitrosamine removal.

This invention discloses a metal-organic coordination gel-protected whole-cell biosensor for monitoring nitrosamine compounds in the digestive tract. It utilizes Fe... 3+ Using a metal-organic coordination gel (MOC) formed through coordination with 2,2'-thiodiacetic acid as a carrier, a coordination gel biosensor formed from *Saccharomyces cerevisiae* bacteria expressing GFP in response to nitrosamines is encapsulated within the MOC. When nitrosamines cause DNA damage, the DNA damage repair pathway in the yeast is activated, leading to enhanced expression of the GFP reporter gene. The intensity of the fluorescence signal reflects the genotoxicity of nitrosamines. This invention also discloses the application of a whole-cell biosensor protected by an MOC for monitoring nitrosamines in the digestive tract. The coordination gel biosensor of this invention can be used for the detection of nitrosamines, exhibiting high specificity and ease of operation.