15 results about "Potassium hexafluorophosphate" patented technology

The invention discloses a method for determining bedaquiline fumarate clean verification target residues, and relates to the technical field of instrument analysis of chemical pharmacy. The method comprises the following steps: preparing a sample wiping solution; determining the content of bedaquiline fumarate in the sample wiping solution by adopting a liquid chromatography; chromatographic conditions are as follows: a chromatographic column is a VP-ODS C18 column; mobile phases: a potassium hexafluorophosphate aqueous solution and acetonitrile, wherein the concentration of the potassium hexafluorophosphate aqueous solution is 0.01-0.03 mol / L; the elution mode is isocratic elution; the flow rate is 1 ml / min to 2 ml / min; the column temperature is 28-32 DEG C; the method has good specificity and sensitivity for determination of bedaquiline fumarate cleaning verification target residues, is simple and convenient to operate, rapid in determination, simple and easy to implement, and overcomes the defects that TOC, chemical titration methods, conductivity methods, pH methods and the like which are commonly used at present do not have specificity.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and determining nafamostat mesylate SM2 and related impurities thereof. The method is a high performance liquid chromatography, and comprises the following steps: by taking octadecylsilane chemically bonded silica as a chromatographic column filler, a potassium hexafluorophosphate solution as a mobile phase A and acetonitrile as a mobile phase B, separating nafamostat mesylate SM2 and related impurities thereof through linear gradient elution; and detecting by using detection wavelengths of 200 nm to 240 nm and 250 nm to 280 nm to obtain a chromatogram, so that effective determination of the nafamostat mesylate SM2 and the related impurities thereof is realized. The method provided by the invention adopts common buffer salt as a mobile phase, and has the characteristics of short analysis time, strong specificity, high sensitivity and good reproducibility.

The invention relates to a process for recovering an electrolyte and co-producing potassium hexafluorophosphate, which comprises the following steps: 1) taking the electrolyte, adding potassium fluoride and potassium carbonate solid, stirring for 0.5-1.5 hours at room temperature, and then stirring for 4-6 hours at 40-50 DEG C; 2) after stirring is finished, carrying out solid-liquid separation, and recovering the solvent from the obtained filtrate in a rectification manner; 3) performing solid-liquid separation to obtain a solid, adding acetonitrile, and stirring at 20-25 DEG C for 30-60 minutes; 4) after stirring, filtering and washing to obtain a lithium fluoride solid; and carrying out rotary evaporation on the obtained filtrate at 60-70 DEG C to obtain a crude potassium hexafluorophosphate solid. According to the process, a step-by-step extraction and hydrolysis process route is adopted, operation is easy, industrial production is easy to achieve, energy consumption and cost are reduced, and the potassium hexafluorophosphate solid is produced while the electrolyte is recycled; and guidance is provided for electrolyte recovery and potassium hexafluorophosphate synthesis in the future.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating, identifying and quantifying nafamostat mesylate Z1 and impurities thereof. And the nafamostat mesylate Z1 is 6-cyano-2-naphthol. According to the method, octadecylsilane chemically bonded silica is adopted as a chromatographic column filler, a potassium hexafluorophosphate solution is adopted as a mobile phase A, acetonitrile is adopted as a mobile phase B, an impurity Z1b, an impurity Z1c, nafamostat mesylate Z1, an impurity Z1h, an impurity Z1a, an impurity Z1g, an impurity Z1d, an impurity SM1, an impurity SM1i, an impurity Z1f and / or an impurity SM1j are sequentially separated through linear gradient elution, and the separated impurities enter a detector for detection; and finally, calculating the content of each impurity by adopting a correction factor-added principal component self-contrast method. The method can effectively separate 6-cyano-2-naphthol and related impurities thereof within 60 minutes, and has the advantages of high sensitivity, strong specificity, good durability and simplicity and feasibility in operation.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to an HPLC (High Performance Liquid Chromatography) method for separating and determining nafamostat mesylate X1 and impurities thereof. The impurities comprise an impurity NAA-SM2, an impurity NAA-SM2a, an impurity NAA-SM2f, an impurity NAA-X1d, an impurity NAA-X1b, an impurity NAA-X1e, an impurity NAA-X1f and isopropyl p-aminobenzoate. According to the method, octadecyl silane bonded silica gel is adopted as a chromatographic column filler, a potassium hexafluorophosphate solution is adopted as a mobile phase A, acetonitrile is adopted as a mobile phase B, and nafamostat mesylate X1 and impurities thereof are separated through linear gradient elution; and then calculating the content of each impurity by adopting an external standard method and / or a principal component self-contrast method multiplied by a correction factor according to a chromatogram. The method has the characteristics of good separation degree, good durability, high sensitivity and good reproducibility.

The invention discloses a potassium ion battery based on a high-capacity and high-stability molybdenum sulfide composite electrode and a salt-regulated electrolyte. According to the method, electrostatic spinning is combined with a stepped heat treatment process, ammonium thiomolybdate, polyacrylonitrile and the like are used as precursors, a surfactant is introduced into the precursors to reduce the surface tension of a spinning solution, and then the molybdenum disulfide / carbon composite electrode material with the self-supporting structure is prepared. Meanwhile, the ethylene glycol dimethyl ether electrolyte which takes potassium hexafluorophosphate as a main salt and is added with potassium trifluoromethanesulfonate and potassium bis (fluorosulfonyl) imide in a specific proportion is adopted. The composite material has a synergistic effect with a specific electrolyte, so that the specific capacity and the cycling stability of the potassium ion battery are effectively improved.

The application provides a chromone-modified o-phenanthroline polypyridine Ru(II) series compound and a preparation method and application thereof, the preparation method synthesizes an intermediate A by taking 1,10-o-phenanthroline-5,6-diketone and 6-substituted-4-oxo-4H-benzopyran-3-formaldehyde as raw materials, then the intermediate A is heated to reflux in ethylene glycol solvent and cis-[Ru(2,2'-dipyridine)2Cl2]·2H2O at 120 DEG C for 6h, after the system is cooled to room temperature, an excess amount of a saturated aqueous solution of potassium hexafluorophosphate is added, after a precipitate is separated out, the filter cake is washed with clean water, and the final product is obtained after drying. The synthesis method is simple and easy to operate without steps such as column chromatography.

The invention discloses a method for measuring residual quantity of residual impurities DMAP and EDU in synthesis of antitumor drugs, and belongs to the technical field of drug analysis. According to the method, high performance liquid chromatography is adopted for detection; dimethyl sulfoxide is used as a solvent to dissolve the sample for detection; detection conditions of the high performance liquid chromatography are as follows: a chromatographic column is an octadecyl bonded silica gel column; the mobile phase A is a sodium perchlorate buffer solution or a potassium hexafluorophosphate buffer solution; the mobile phase B is acetonitrile; the detector is an ultraviolet detector; the detection wavelength for detecting the DMAP is 278 to 282 nm, and the detection wavelength for detecting the EDU is 198 to 202 nm; a gradient elution mode is adopted. The method is used for detecting DMAP and EDU residues in the raw material medicine, is high in sensitivity and accuracy, does not need a special column, can meet the control limit of the ICH guidance principle on genotoxic impurities and general impurities of the raw material medicine, provides reliable guarantee for impurity control of the raw material medicine, and further guarantees the safety of clinical medication.

The application belongs to the technical field of organic synthesis, and specifically provides a 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate, a preparation method and a condensation reagent. The preparation method of the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate comprises: making 2-chloro-4,6-dimethoxy-1,3,5-triazine and tetramethylurea undergo a nucleophilic substitution reaction to generate an intermediate; and making the intermediate and potassium hexafluorophosphate undergo an ion exchange reaction to generate the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate. The 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate according to the embodiment of the application can be used as a condensation reagent for forming an amide bond, and compared with condensation reagents such as HBTU and HATU which have two high-energy heteroatomic bonds of N-N and N-O, the thermal hazard of the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate is smaller, and the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate is suitable for industrial production. In addition, the preparation method according to the embodiment of the application has mild reaction, fewer reaction steps and low operation risk coefficient.

The invention relates to a high-voltage-resistant electrolyte, a preparation method and application of the high-voltage-resistant electrolyte and a potassium ion battery. The electrolyte comprises electrolyte sylvite and an electrolyte solvent, the electrolyte potassium salt is one or more of potassium hexafluorophosphate, potassium tetrafluoroborate, potassium bis (fluorosulfonyl) imide, potassium trifluoromethanesulfonate, potassium bis (trifluoromethane) sulfonyl imide, potassium nitrate and potassium perchlorate. The electrolyte provided by the invention is simple in manufacturing process and excellent in oxidation stability, and when the electrolyte is applied to the high-voltage potassium ion battery, a stable electrode-electrolyte interface can be formed by preferentially decomposing more anions under the condition that cyclic carbonate is not added as a film-forming cosolvent, so that the stability of the high-voltage potassium ion battery is improved. Therefore, the compatibility of the carbonic ester-based electrolyte with the positive and negative electrodes of the potassium ion battery is improved.

An electrolyte, comprising: an amount of potassium hexafluorophosphate; at least one cyclic carbonate, the at least one cyclic carbonate optionally comprising at least one of ethylene carbonate and propylene carbonate; and at least one organic phosphate, the at least one organic phosphate optionally comprising at least one of trimethyl phosphate and triethyl phosphate. An electrical cell, comprising: the electrolyte according to the present disclosure, and an electrode, the electrode contacting the electrolyte. A method, comprising: any one or more of separating, disposing, or at least partially neutralizing any one or more of HF, HPO2F2, H2PO3F, an organofluorophosphate, a monofluorophosphate, an organophosphate, and a phosphonate evolved from operating an electrical cell that includes as an electrolyte any one or more of LiPF6, NaPF6, and KPF6.

This invention discloses a method for synthesizing tri(p-tolyl)thionium hexafluorophosphate, comprising the following steps: di(4-chlorophenyl) sulfoxide is mixed uniformly with a solvent, and p-tolyl magnesium bromide is slowly added under an inert atmosphere. After stirring for 10 min, trimethylchlorosilane is added dropwise. After the reaction is complete, a 25 wt.% hydrobromic acid aqueous solution is added dropwise to quench the reaction. After extraction and vacuum concentration, tri(p-tolyl)thionium bromide is obtained. A potassium hexafluorophosphate aqueous solution is added to the tri(p-tolyl)thionium bromide and stirred. After the reaction is complete, the mixture is filtered, and the filter cake is recrystallized to obtain tri(p-tolyl)thionium hexafluorophosphate. This invention uses inexpensive and readily available raw materials, employs mild activation conditions, has high production safety, and achieves a yield of up to 71.34% for the obtained tri(p-tolyl)thionium hexafluorophosphate.

The invention relates to the technical field of photovoltaic power generation, in particular to a blade coating preparation method of a perovskite solar cell using potassium hexafluorophosphate, and the method can effectively passivate defects of a perovskite film and inhibit ion migration through the introduced potassium hexafluorophosphate, thereby fundamentally reducing the hysteresis effect of a device, the potassium ions can be embedded into octahedral gaps of perovskite crystal lattices, the hexafluorophosphate ions can fill up iodine vacancy defects, the potassium ions and the hexafluorophosphate ions jointly inhibit migration of iodine ions in the perovskite crystal lattices, the photoelectric conversion efficiency of a finally prepared device is improved to 22.50% from 21.07%, the hysteresis factor is reduced to 4.1% from 11.8%, the film crystallization quality and the device stability are remarkably improved, and the performance of the device is improved. And an effective scheme is provided for large-area and industrial production of high-performance perovskite solar cells.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and detecting nafamostat mesylate Z2 and impurities thereof by an HPLC (High Performance Liquid Chromatography) method. The impurities comprise an impurity Z1, an impurity Z1b, an impurity Z1c, an impurity Z1d, an impurity Z1f, an impurity Z1g, an impurity Z1h, an impurity Z2b, an impurity Z2e and / or an impurity Z2f. According to the method, octadecyl silane bonded silica gel is adopted as a chromatographic column filler, a potassium hexafluorophosphate solution is adopted as a mobile phase A, an organic solvent is adopted as a mobile phase B, and nafamostat mesylate Z2 and related impurities are separated through gradient elution; a detector is used for detection, and each component is quantified by adopting a limit method or a principal component self-contrast method multiplied by a correction factor. The method can effectively separate and measure the nafamostat mesylate Z2 and related impurities thereof, and has important significance on quality control of the nafamostat mesylate Z2 and subsequent nafamostat mesylate preparation products.

The invention discloses a method for detecting related substances of trazodone hydrochloride sustained release tablets, and belongs to the technical field of pharmaceutical analysis. According to the detection method, high performance liquid chromatography is adopted, and the chromatographic condition is that an octadecyl bonded silica gel column is used as a chromatographic column; the column temperature is 25-35 DEG C, and the flow velocity is 0.8-1.2 ml / min; the sample size is 5-15 [mu] l, and the detection wavelength is 252-256 nm; the mobile phase A is a potassium hexafluorophosphate buffer solution; the mobile phase B is acetonitrile; and carrying out gradient elution. Compared with trazodone hydrochloride sustained-release tablet imported drug registration standards and United States Pharmacopoeia related substance detection methods of trazodone hydrochloride bulk drugs, the method abandons a tailing-sweeping agent triethylamine suitable for an alkaline sample, adjusts the pH value of a mobile phase to be acidic, improves the peak shape and increases retention of trazodone hydrochloride and impurities through a chaotropic agent potassium hexafluorophosphate buffer solution, and improves the quality of trazodone hydrochloride sustained-release tablets. The method has the advantages of moderate impurity retention, good separation effect, excellent peak shape, long service life of the chromatographic column and reduction of the analysis cost. The method has the advantages of strong specificity, high sensitivity, high accuracy and good durability.