225 results about "Fluoroacetic acid" patented technology

The invention relates to the technical field of organic synthesis, and discloses a preparation method of bromo-pyrrole nitrile. The method comprises the following steps: (1) mixing p-chlorophenylglycine, acetonitrile, trifluoroacetic acid and a catalyst, then dropwise adding acyl chloride and carrying out acylation reaction, and after the reaction is completed, purging with an inert gas; (2) under the inert gas, mixing the mixture obtained in the step (1) with inorganic salt, then dropwise adding 2-chloroacrylonitrile, carrying out cyclization reaction, and separating a liquid phase from the obtained mixture; and (3) under the inert gas, mixing the liquid phase obtained in the step (2), hydrobromic acid and hydrogen peroxide, carrying out a bromination reaction, then extracting with acetonitrile to obtain an acetonitrile layer, then removing the acetonitrile, and then carrying out cooling crystallization to obtain the bromo-pyrrolenitrile. According to the technical scheme, the reaction yield is high, different solvents do not need to be frequently replaced, and the solvents can be recycled.

The invention is applied to the technical field of lithium ion batteries, and discloses a non-aqueous electrolyte for a lithium ion battery, which comprises the following substances in percentage by weight: 1-20% of electrolyte lithium salt, 70-90% of organic solvent and 0.1-10% of functional additive, the electrolyte lithium salt is composed of a lithium salt A and a lithium salt B, and the weight fraction of the lithium salt A is greater than that of the lithium salt B; the organic solvent is composed of a solvent C and a solvent D, the weight fraction of the solvent C is 3%-20%, and the weight fraction of the solvent D is 50%-88%. According to the non-aqueous electrolyte for the lithium ion battery, the lithium fluorosulfonyl difluoroacetate is adopted as the main lithium salt to prepare the non-aqueous electrolyte, so that the electrolyte has the advantages of high ionic conductivity, stability in air and good thermal stability, and the performance of the lithium battery is more excellent.

The invention discloses a method for analyzing oligosaccharide composition in American ginseng polysaccharide, and belongs to the technical field of pharmaceutical analytical chemistry, and the method comprises the following steps: 1) carrying out primary extraction on American ginseng through a methanol / methyl tert-butyl ether solution, and removing supernate to obtain American ginseng subjected to primary extraction; (2) adding pure water into the American ginseng subjected to primary extraction, extracting again, taking supernate, adding absolute ethyl alcohol into the supernate, standing, and centrifuging to obtain precipitate; 3) dissolving the precipitate with water, adding an n-butyl alcohol / chloroform solution, mixing and oscillating, and drying the aqueous solution to obtain crude polysaccharide; 4) adding water into the crude polysaccharide for redissolving, adding trifluoroacetic acid for reaction, and centrifugally concentrating to obtain oligosaccharide; and 5) dissolving the oligosaccharides in an acetonitrile aqueous solution, taking a sample to be detected, and detecting by using liquid chromatography-mass spectrometry to obtain the variety and proportion of the oligosaccharides in the sample to be detected. The problem that the structure of American ginseng polysaccharide is difficult to identify and analyze in the prior art is solved.

The invention relates to an electrolyte, the electrolyte comprises a lithium salt, an organic solvent and an additive, the additive comprises a pyridine trifluoroacetate compound, a chlorodifluoroacetate compound and LiNO3, the electrolyte provided by the invention can significantly reduce a Li < + > diffusion energy barrier and promote compact lithium deposition, and the lithium ion battery can be used as a lithium ion battery. According to the present invention, the pyridine trifluoroacetate, the chlorodifluoromethyl acetate and the LiNO3 in the electrolyte can form the uniform and compact CEI film on the surface of the positive electrode, such that the structure of the positive electrode active material is greatly protected, and the dissolution of the transition metal is inhibited so as to provide the excellent cycle performance of the lithium metal battery;

The invention provides a system and a process method for co-production of hexafluoropropylene oxide and trifluoroacetic acid, and relates to the technical field of fluorine chemical industry. The system comprises a raw material storage device, a liquid phase oxidation reaction device, a rectifying tower, a hydrofluoric acid absorption tank, a trifluoroacetic acid absorption tank, a process water tank, a hydrofluoric acid concentration detector and a trifluoroacetic acid concentration detector. According to the method, the hydrofluoric acid and the trifluoroacetic acid are co-produced while the hexafluoropropylene oxide is produced, so that complex production processes such as use of non-renewable resources, high raw material price, use of a catalyst for catalysis, addition of an auxiliary agent and the like in the traditional hydrofluoric acid and trifluoroacetic acid production process are avoided; the technology for continuously producing hydrofluoric acid and trifluoroacetic acid, which is simple and efficient in technological process, low in raw material price and free of catalyst catalysis, is developed, and the technology is relatively high in technicality, low in safety risk and suitable for industrial application.

The invention relates to the technical field of photo-thermal therapy, in particular to a monomolecular photo-thermal agent with high photo-thermal conversion efficiency and a preparation method and application of the monomolecular photo-thermal agent. The preparation method comprises the following steps: S1, synthesis of a compound X1: under the protection of argon, dissolving 2, 4-dimethyl pyrrole in dichloromethane, stirring in an ice bath, adding trifluoroacetic anhydride, heating to room temperature after stirring, extracting after quenching reaction, combining organic phases, drying, filtering, concentrating under reduced pressure and purifying by silica gel column chromatography to obtain the compound X1. The prepared monomolecular photothermal agent with the high photothermal conversion efficiency is high in water solubility, has the high photothermal conversion efficiency in an aqueous solution and is high in light stability, the immune escape phenomenon possibly caused by introduction of a high polymer material is avoided, and the technical problem that an existing photothermal agent is difficult to achieve the high photothermal conversion efficiency in the aqueous solution is solved.

The invention relates to the technical field of compound preparation, and particularly provides a preparation method of alkyl cyclophosphoric anhydride, which comprises the following step: reacting alkyl phosphoric acid with trifluoroacetic anhydride to generate alkyl cyclophosphoric anhydride. The preparation method provided by the embodiment of the invention has the advantages of simple operation, high reaction activity, low reaction temperature, short reaction time and easy raw material recovery, and is suitable for industrial production. Besides, the boiling point difference between the residual raw material trifluoroacetic anhydride and the by-product trifluoroacetic acid reaches 32 DEG C, the trifluoroacetic anhydride can be well separated through rectification, and the separated and recycled trifluoroacetic anhydride can be further used for reaction, so that the production cost is greatly reduced.

A method for producing an aromatic heterocycle-substituted difluoroacetic acid derivative having a partial structure represented by the formula (III), by reacting an N-oxido aromatic heterocyclic compound having a partial structure represented by the formula (I) with tetrafluoroethylene in the presence of a compound represented by the formula (II): R—YH, in a solvent selected from an aromatic hydrocarbon solvent, an ester solvent and an ether solvent:

The invention discloses an electrolyte suitable for high-rate charge-discharge and low-temperature circulation and a lithium metal battery, and belongs to the technical field of lithium batteries. The electrolyte comprises the lithium salt, the additive and the cosolvent mixture, the cosolvent mixture is composed of the methyl acetate, the methyl difluoroacetate and the fluoroethylene carbonate, and due to the synergistic effect of a mixed solvent system, the electrolyte can have high high voltage resistance and oxidation resistance; meanwhile, a low-impedance electrode electrolyte phase interfacial film rich in inorganic matter LiF can be formed, rapid desolvation of Li < + > is promoted, the rate capability and the low-temperature performance of the battery are further remarkably improved, and the battery can also normally work at the high rate of-30 DEG C and 2C. The preparation raw materials of the electrolyte are cheap and easy to obtain, the preparation process is simple and convenient, and a thought is provided for industrial production of the low-temperature electrolyte.

The invention relates to a lithium ion battery. In order to solve the problem that the performance of the battery is influenced by solvent decomposition and gas production due to the fact that active oxygen is released in the using process when a lithium supplementing agent is added, a solvent ethylene carbonate in an electrolyte is promoted to be subjected to a ring-opening reaction, and the lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte, the positive electrode comprises a positive electrode active material and a lithium supplement agent, the electrolyte comprises an organic solvent, a lithium salt and an additive, the organic solvent comprises fluoro carboxylic ester, fluoro ether and carbonic ester and does not contain ethylene carbonate, and the additive comprises trimethylsiloxyethyl isocyanate and / or 2-(1, 1-thiophane-3-dioxide)-2, 2-methyl difluoroacetate. Through the synergistic effect of the solvent system and the additive, the stability of the electrolyte in a battery containing a lithium supplement agent is improved, the wettability and low-temperature performance of the battery, especially a high-compaction battery, are improved, and meanwhile, the lithium ion battery has relatively good normal-temperature cycle performance and high-temperature performance.

The invention belongs to the technical field of chromatographic separation materials, and discloses a preparation method and application of a GM-8 nanosheet material. The preparation method of the material comprises the following steps: respectively dissolving Cu (NO3) 2.3 H2O and 1, 3, 6, 8-tetra (4-carboxybenzene) pyrene in an organic solvent, mixing, transferring into a reaction bottle, adding trifluoroacetic acid and pyridine, and uniformly mixing and stirring to obtain a reaction mixture; and heating the reaction mixture to react for 7-9 hours to obtain a blue precipitate, cooling the blue precipitate to room temperature, and washing and drying the blue precipitate to obtain the ultra-stable microporous GM-8 nanosheet material. The nanosheet GM-8 is used as a gas chromatography stationary phase, high-efficiency separation and trace detection of xylene isomers can be realized, and the chromatographic column still keeps excellent separation capacity after being stored in an environment with air humidity of 65-90% for 31 months. The capillary gas chromatographic column can realize high-efficiency separation of disubstituted benzene isomers such as xylene, the separation degree of m-xylene / p-xylene is up to 18.2, and a new solution is provided for high-efficiency separation of isomers with similar properties.

The invention belongs to the technical field of drug synthesis, and particularly discloses a preparation method of a low-single-impurity and high-purity olpinapone intermediate 05, which comprises the following steps: adding UHP into a dichloromethane solution of an intermediate 04 while cooling, and keeping stirring for 0.5-1 hour; adding trifluoroacetic anhydride at a controlled low temperature, returning the temperature after adding, and carrying out heat preservation and stirring reaction; after the reaction is finished, filtering, leaching a filter cake with dichloromethane, washing filtrate with water, adding a material subjected to vacuum concentration into methylbenzene, adding formic acid, heating and stirring, cooling after stirring, filtering, collecting a filter cake, and drying under reduced pressure to obtain the low-single-impurity and high-purity olpinapone intermediate 05.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a detection method of an evocamide enantiomer, which comprises the following steps: S1, preparing a test solution; s2, preparing a contrast solution; s3, preparing a system applicable solution; s4, carrying out a system applicability test; s5, testing a test sample and a contrast solution; a chromatographic column is a chiral chromatographic column taking a polysaccharide derivative or a cellulose derivative as a filler, and a mixed solution of n-hexane, isopropanol, trifluoroacetic acid and diethylamine is taken as a mobile phase to detect the Evocadum enantiomer. The method has the characteristics of simplicity in operation, high sensitivity and high accuracy, the chromatographic peaks are high in separation degree, do not interfere with one another, the peak shape is good, the result accuracy is guaranteed, the method can be used for detecting enantiomers in the Evocamide and the Evocamide preparation, the level of the enantiomers of the Evocamide is effectively controlled, and the medication safety is guaranteed.

The invention discloses an LC-MS (liquid chromatography-mass spectrometry) detection method for N, N-diethyl-N ', N'-dimethylethylenediamine in chlorpheniramine maleate, and belongs to the technical field of analytical chemistry. The method comprises the following steps: firstly, preparing a test solution and a reference solution for later use; then setting liquid chromatography-mass spectrometry detection conditions, and detecting N, N-diethyl-N ', N'-dimethylethylenediamine in chlorpheniramine maleate by adopting a Shim-pack Scept Diol-HILIC-120 chromatographic column, taking a 0.1% difluoroacetic acid aqueous solution-acetonitrile mixed solution as a mobile phase and taking a 1% diethylamine acetonitrile solution as a solvent. According to the method, a liquid chromatography-mass spectrometry technology is adopted, the problem that N, N-diethyl-N ', N'-dimethyl ethylenediamine has no ultraviolet absorption can be effectively solved, and meanwhile, the method is high in specificity, high in sensitivity and high in efficiency.

The application relates to the technical field of metal organic thin layer material preparation, in particular to a kilogram-level preparation method of metal organic thin layer material. The preparation method comprises the following steps: S1, adding zirconium tetrachloride and H2BPYDC into a polytetrafluoroethylene reaction kettle, dissolving the zirconium tetrachloride and the H2BPYDC, and then adding a composite; S2, sequentially adding a DMF solution of palladium fluoroacetate, a catalyst and concentrated hydrochloric acid into the reaction kettle; S3, transferring the reaction kettle into an oven, centrifuging to obtain a cyan suspension after 18-20 hours, dispersing the cyan suspension in a DMF solution in batches at 60 DEG C, placing for 5-6 hours, removing unreacted substrates, and obtaining a solid; S4, cleaning the solid obtained in S3 by using DMF and tetrahydrofuran respectively, and vacuum drying for 12 hours to obtain the metal organic thin layer material. The kilogram-level preparation method of metal organic thin layer material is provided, so as to solve the problems of low preparation yield, slow rate and difficulty in kilogram-level preparation of metal organic thin layer material in the related art.

The invention discloses a preparation method and application of a silicon-based functionalized fluorenyl polysubstituted acetylene copolymer and a gas separation membrane thereof. Belongs to the technical field of polymer material and gas separation. The invention provides a new thought for preparation of a high-permeability gas separation membrane material. The preparation method comprises the following steps: carrying out copolymerization on 1-phenyl-2-(7-trimethylsilyl-9, 9-bis (trimethylsilyl-fluorene-2-yl) acetylene and 1-phenyl-2-(7-trimethylsilyl-9, 9-dimethyl-fluorene-2-yl) acetylene under the catalysis of TaCl5-n-Bu4Sn, so as to prepare a copolymer with high molecular weight; the preparation method comprises the following steps of: carrying out film casting on a solution of the nano-silver oxide, and then carrying out desiliconization treatment by using normal hexane / trifluoroacetic acid to obtain a gas separation membrane with the thickness of 100-220 microns, the specific surface area of 298-492 m / g and the total pore volume of 0.134-0.299 cm / g. The prepared separation membrane has the advantages that the COpermeability is up to 36,900 Barrer, the Opermeability is 19,800 Barrer, the thermal decomposition temperature exceeds 420 DEG C, the separation membrane can be used for separating gases such as COO, ON and the like, the preparation process is simple and convenient, and the industrial potential is realized.

FIELD: pharmacology.SUBSTANCE invention can be used to determine the concentration of an anti-tuberculosis drug in blood serum. The method for determining the concentration of bedaquiline in the blood serum in patients with tuberculosis or mycobacteriosis is that whole blood samples are centrifuged at 3000 rpm for 20 minutes, then the blood plasma is collected in sterile 1.5 mL Eppendorf tubes, then 900 mcL of acetonitrile are added to 300 mcL of plasma and centrifuged at 13500g for 15 minutes, then 1 mL of the supernatant is transferred to a chromatographic vial and make the assay by UHPLC MS / MS using an Athena UHPLC C18, 1.8 mcM, 120A, 2.1×100 mm chromatography column, when using an aqueous solution containing 5 g / L of ammonium acetate, 25 ml / L of concentrated acetic acid, 2 ml / L trifluoroacetic acid as mobile phase A and 100% acetonitrile as mobile phase B, the concentration of bedaquiline is determined using a pre-plotted calibration curve.EFFECT: determination of bedaquiline in human blood plasma in a time not exceeding 6 minutes.1 cl, 9 dwg, 6 tbl

The invention provides a method for preparing 2, 6-diamino-3, 5-dinitropyridine, which comprises the following steps: (1) reacting 2, 6-diaminopyridine with an amino protection reagent to obtain an intermediate A; (2) in the presence of a dehydrating agent, carrying out double nitration reaction on the intermediate A and a nitration reagent to generate an intermediate B; (3) 2, 6-diamino-3, 5-dinitropyridine is obtained after the intermediate B is subjected to deprotection, and an amino protection reagent is selected from one or more of acetic anhydride, trifluoroacetic anhydride, di-tert-butyl dicarbonate, benzyl chloroformate and concentrated sulfuric acid; wherein the molar ratio of the amino protection reagent to the 2, 6-diaminopyridine is (2: 1)-(30: 1) by mole; and preferably, the ratio is 2: 1-12: 1.

The invention relates to a preparation method of trifluoromethylsulfonyl fluoride, which comprises the following steps: taking fluorosulfonyl difluoroacetic acid, fluorosulfonyl difluoroacetate or fluorosulfonyl difluoroacetyl fluoride as raw materials, and reacting with fluorine gas to obtain the product trifluoromethylsulfonyl fluoride. According to the method, the fluorosulfonyl difluoroacetic acid (ester or acyl fluoride) directly reacts with the fluorine gas, and complex multi-step reaction and separation and purification of intermediate products are not needed, so that the process flow is simplified, the production links are reduced, and the production efficiency is improved; the method has the advantages of low price of raw materials, mild reaction conditions, low requirements on equipment, realization of continuous production, and reduction of the equipment investment and the production cost; the preparation method is carried out under an anhydrous condition, does not need to use any organic solvent, and is environment-friendly and green; by controlling the reaction conditions, the yield of the trifluoromethylsulfonyl fluoride can reach 85%, the purity of the trifluoromethylsulfonyl fluoride can reach 99.9%, the requirements of different fields for high-purity products can be met, and the method has a good industrial application prospect.

The invention discloses bio-based polyamide with low water absorption and a preparation method thereof, and belongs to the technical field of polyamide preparation. The bio-based polyamide with the low water absorption rate is prepared from the following components in parts by weight: 30 to 50 parts of pentamethylene diamine, 15 to 30 parts of sebacic acid, 5 to 12 parts of citric acid, 5 to 10 parts of hexamethylenediamine, 2 to 5 parts of a hydrophobic auxiliary agent and 1 to 5 parts of a modified high-temperature-resistant additive, the hydrophobic additive is prepared from acetoxybenzoic acid, nonadecanoic acid, m-dimethoxybenzene, trifluoroacetic anhydride and methyl tert-butyl ether as raw materials, and the modified high-temperature-resistant additive is prepared from o-phenylenediamine, chloroacetic acid, vanillin, benzoyl bromide and thiourea as raw materials. The bio-based polyamide prepared from the substances has low water absorption and excellent thermal stability.

The invention discloses a method for microwave digestion of an express packaging material and application, and the method comprises the following steps: S1, crushing and grinding the express packaging material until the particle size is less than 100 [mu] m; s2, adding a composite acid-chitinase mixed solution into the digestion tank, and preliminarily contacting with the sample to weaken the structure of the sample; the composite acid-chitinase mixed solution comprises a composite acid mixed solution and a chitinase aqueous solution; the composite acid mixed solution comprises nitric acid, trifluoroacetic acid, hydrogen peroxide and formic acid; s3, placing the digestion tank treated in the step S2 on a turntable of a microwave digestion instrument, and carrying out pulse type microwave digestion; the microwave time is 25 minutes to 35 minutes; according to the method, pulse type microwaves are matched with the composite acid to digest the express packaging material, the digestion solution with high digestion completeness is obtained, HP-beta-CD and DTPA are used as double ligands to synergistically extract heavy metals such as lead and cadmium, the selectivity is good, and the efficiency is high.

The invention belongs to the technical field of analysis and detection, and provides a visual detection method for chemical components in radix ophiopogonis. The method comprises the following steps: embedding a radix ophiopogonis root sample to be detected, and slicing to obtain a sliced sample; carrying out matrix spraying on the slice sample to obtain a sprayed slice; carrying out matrix-assisted laser desorption ionization mass spectrometry imaging on the sprayed slice to obtain a visual result; the matrix sprayed by the matrix is a 2, 5-dihydroxy benzoic acid solution, and the concentration of the 2, 5-dihydroxy benzoic acid is 20-40 mg / mL; the 2, 5-dihydroxybenzoic acid solution also contains trifluoroacetic acid, and the volume concentration of the trifluoroacetic acid is 0.05-0.15%; the solvent is an acetonitrile aqueous solution (the volume ratio of acetonitrile to water is (6-8): (4-2)). According to the method, clear in-situ analysis is carried out on the chemical components in the radix ophiopogonis by utilizing matrix-assisted laser desorption ionization mass spectrometry imaging, so that the spatial distribution and content difference of the components in the radix ophiopogonis are obtained, and the result is more visual due to spatial presentation.

The invention belongs to the technical field of organic conjugated compounds, and particularly relates to an amidinourea-containing water-soluble arylacetylene illuminant and a preparation method and application thereof.The preparation method of the amidinourea-containing water-soluble arylacetylene illuminant comprises the following steps that (1) in the nitrogen atmosphere, an amidinourea-containing water-soluble arylacetylene illuminant is obtained; the method comprises the following steps: reacting a guanidyl monomer, an alkyne compound, a catalyst and a mixed solvent to obtain a reaction solution; (2) extracting the reaction liquid, drying an organic phase, performing rotary evaporation under reduced pressure to obtain a crude product, and separating and purifying the crude product to obtain an amidinourea-based aromatic acetylene compound; and (3) mixing the amidinourea-based aromatic acetylene compound with dichloromethane, adding trifluoroacetic acid, stirring, carrying out reduced pressure rotary evaporation, washing with an organic solvent, and drying to obtain the amidinourea-containing water-soluble aromatic acetylene illuminant. The water-soluble arylacetylene illuminant containing the amidinourea group is excellent in activity, good in water solubility, stable in chemical property, high in sensitivity and high in selectivity.

The embodiment of the invention provides a bromo-ethyl difluoroacetate-mediated novel amide dehydration cyaniding method, which comprises the following steps of: heating and reacting 0.2 mmol and 1.0 equivalent weight of amide compound and 0.6 mmol and 3.0 equivalent weight of bromo-ethyl difluoroacetate for 24 hours under an oil bath condition of 90 DEG C to generate an experimental reactant; concentrating the experimental reactant under reduced pressure to obtain a residue; and purifying the residue by silica gel rapid column chromatography to obtain the target product nitrile compound. According to the scheme, the process reaction conditions are mild, a strict anhydrous and anaerobic environment is not needed, the harsh requirements on equipment and operation are greatly reduced, and the production safety and practicability are improved. Acetone is used as a solvent, so that high-efficiency reaction can be realized, the solvent after reaction is convenient to recycle and recycle, the production cost and the environmental burden are remarkably reduced, and the remarkable green chemical engineering characteristic is embodied.

The invention relates to a synthetic method of a compound 4-hydroxy-2-trifluoromethylpyrimidine, which comprises the following steps: by taking a compound ethyl trifluoroacetate and a compound 3-aminopropanamide as raw materials, firstly converting the raw materials into a compound 3-(2, 2, 2-trifluoroacetamido) propanamide, and then carrying out ring closing reaction to obtain the target compound 4-hydroxy-2-trifluoromethylpyrimidine. The synthetic route has the advantages of short steps, simple operation, low cost, mild reaction conditions, simple post-treatment and ideal yield, and is suitable for process amplification.

The invention belongs to the technical field of electrolysis, and discloses a method for preparing p-hydroxyanisole through electrolytic oxidation of anisole. The method comprises the following steps: S1, adding anisole, an acylation reagent, an organic alkali proton trapping agent and an alkaline amine group-containing solvent into a single-chamber electrolytic bath together, starting electrification, carrying out electrolysis, and obtaining a product liquid containing p-methoxytrifluoroacetic acid phenyl ester in the single-chamber electrolytic bath after electrolysis is finished; the organic base proton trapping agent is at least one of N, N-diisopropylethylamine, tributylamine and tripropylamine; and S2, adding a saturated sodium bicarbonate aqueous solution into the product liquid containing p-methoxytrifluoroacetic acid phenyl ester in the step S1 to hydrolyze p-methoxytrifluoroacetic acid phenyl ester, and extracting to obtain p-hydroxyanisole. The selectivity of para-position and ortho-position products of methoxyl on anisole is regulated and controlled, so that the selectivity of p-hydroxyanisole prepared by the method is higher.

This invention belongs to the field of responsive material production technology, specifically relating to a high-viscosity fluoropolymer solution and its applications. The preparation method of the high-viscosity fluoropolymer solution is as follows: (meth)acrylate naphthyl ester, fluorinated methacrylate, and vinylcarbazole are dissolved in a solvent and stirred to obtain a clear and transparent solution. Then, an initiator is added, and the mixture is heated to 60-90℃ under magnetic stirring for 16-24 hours to polymerize. After the reaction is completed, a transparent high-viscosity polymer solution with a viscosity range of 800-8000 Pa·s is obtained. After the high-viscosity fluoropolymer solution forms a film on the substrate, it forms an anti-counterfeiting coating that can be stimulated by ultraviolet light and trifluoroacetic acid, exhibiting excellent multi-stimulus responsiveness. The preparation method of this anti-counterfeiting coating is simple, has good film-forming properties, long service life, and low cost. It can be industrially produced and provides dual anti-counterfeiting capabilities, showing great application prospects in anti-counterfeiting, information encryption, and other fields.

The invention relates to the technical field of medicine detection, and provides a method for determining the content of diethylenetriamine pentaacetic acid in a lutetium [177Lu] radiopharmaceutical preparation, which comprises the following steps: testing by adopting a high performance liquid chromatography-electrospray detector method, taking porous graphite carbon as a filling agent in a chromatographic column, and eluting by adopting a gradient mode, so as to determine the content of the diethylenetriamine pentaacetic acid in the lutetium [177Lu] radiopharmaceutical preparation. The mobile phase A is an aqueous solution of formic acid, trifluoroacetic acid or perfluorovaleric acid, and the mobile phase B is an acetonitrile solution of formic acid, trifluoroacetic acid or perfluorovaleric acid. According to the detection method, the separation degree of the DTPA reaches 1.5 or above, verification is carried out according to the 9101 Analytical Method Verification Guidance Principle of Chinese Pharmacopoeia 2020 edition, and the method has good system applicability, specificity, accuracy, stability and reliability and can be used for measuring and controlling the content of the DTPA.

The application relates to the field of biological medicine, and discloses an active oxygen response thione aldehyde linker as well as a preparation method and application thereof. The thione aldehyde linker structure is a thione aldehyde structure with a p-hydroxyphenyl as a center. The thione aldehyde carbon atom is connected with two -CH2CH2COOH groups through a sulfur atom. The preparation method of the active oxygen response thione aldehyde linker comprises the following steps: dissolving 3-mercapto propionic acid and p-hydroxybenzaldehyde in ethyl acetate, adding trifluoroacetic acid as a catalyst, stirring and reacting at room temperature, and after the reaction is completed, the thione aldehyde linker is obtained through separation and purification. The thione aldehyde linker can respond to the increased ROS level in a tumor microenvironment, is broken under a high ROS condition, and thus realizes the release of a drug molecule connected therewith, which is beneficial to realizing the specific release of the drug at a tumor site.

The invention relates to the field of macromolecules, and discloses a method for refining polyetherketoneketone and a polyetherketoneketone refined product. The method comprises the following steps: (1) treating a polyetherketoneketone complex by adopting a pretreatment agent; (2) the polyether ketone ketone crude product and a mixed chain supporting solution are mixed and washed, a first product is obtained, the mixed chain supporting solution comprises a main chain supporting agent and a cosolvent, the main chain supporting agent comprises one or more selected from parachlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid, the cosolvent comprises one or more selected from N, N-dimethylformamide and dimethyl sulfoxide, and the main chain supporting agent comprises one or more selected from dichlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid. The solvent is one or more of water, N-methyl pyrrolidone and N-methyl formamide; (3) adding a mixed aqueous solution into the first product to remove at least part of metal ions to obtain a second product; and (4) washing the second product for multiple times by using an organic solvent, and washing and drying to obtain the refined polyether ketone ketone. The content of aluminum ions in the polyetherketoneketone prepared by the method is low.