43results about How to "Solving Separation Assay Problems" patented technology

The invention provides a method for determining related substances in Trelagliptin tablets, and relates to the field of analytical chemistry. The method comprises the steps that a high-performance liquid chromatography method is adopted, a sample solution is injected into a high-performance liquid chromatographic instrument, determination of the related substances in the Trelagliptin tablets is completed, and the chromatographic conditions are that a chromatographic column takes silica gel of which the surface is provided with electric hybrid particles as a filler, a mobile phase A is an acidic aqueous solution, a mobile phase B is an organic solvent, the sum of the volume percent of the mobile phase A and the volume percent of the mobile phase B maintains 100% all the time, and linear gradient elution is conducted. According to the method for determining the related substances in the Trelagliptin tablets, an Xselect C18 chromatographic column is adopted, optimization is conducted on the mobile phase gradient elution program, and the related substances in the Trelagliptin tablets can be effectively separated. The separation determination problem of the related substances in the Trelagliptin tablets is solved, and therefore it is guaranteed that the quality of the Trelagliptin tablets is controllable.

The invention belongs to the field of analytical chemistry, and specifically relates to a method for separating and measuring related impurities in acrivastine and a preparation thereof. According tothe method, octadecyl silane bonded silica gel is adopted as a solid phase, and a mobile phase consisting of aqueous solutions of acetonitrile, tetrahydrofuran and triethylamine is adopted for elutionfor solid-liquid separation; the related impurities include one or more of a double oxidation impurity I, a single oxidation impurity II, Z-type III, E-type IV and E-isomer V. According to the methodprovided by the invention, the related impurities in the acrivastine and the preparation thereof are separated and detected by high performance liquid chromatography, and can be totally separated anddetected within 18 minutes; the method has the advantages of high separation degree, strong specificity, high sensitivity, easiness in operation, simpleness and quickness, so as to guarantee that thequality of the acrivastine and the preparation thereof is controllable, and finally determines the safety and effectiveness of a product, and is of great significance to quality control on the acrivastine.

The invention belongs to the field of analytical chemistry, and discloses a method for separately testing a levocetirizine hydrochloride intermediate and related substances of the levocetirizine hydrochloride intermediate by liquid chromatography. The method comprises the following steps: a chromatographic column taking octadecylsilane chemically bonded silica as a filler uses a certain proportion of buffer salt solution-organic phase as a mobile phase to quantificationally test the content of the levocetirizine hydrochloride intermediate and the content of the related substances of levocetirizine hydrochloride intermediate, so that the quality of the levocetirizine hydrochloride intermediate is effectively controlled, and the controllable quality of levocetirizine hydrochloride is ensured. The method is high in specificity and accuracy, and simple and convenient to operate.

The invention belongs to the field of analytical chemistry and discloses a method of separating and measuring otioxetine hydrobromide and related substances thereof by liquid chromatography. The method can measure the contents of otioxetine hydrobromide and related substances thereof quantitively by taking an octyl alkyl silane bonded silica gel as a chromatographic column of filler and a buffer salt solution-organic phase in a certain proportion as a moving phase, so that the quality of the otioxetine hydrobromide is controlled effectively. The method is high in specificity, high in accuracyand simple to operate.

The invention belongs to the field of analytical chemistry, discloses a method for separation and determination of vortioxetine hydrobromide intermediate 1-bromo-2-iodo-benzene related substances by liquid chromatography. The method takes a chromatographic column with octadecylsilane bonded silica gel as a packing, takes a certain ratio of water-organic phase as a mobile phase, and can be used for quantitative determination of the contents of a vortioxetine hydrobromide intermediate and the related substances thereof, so as to effectively control the quality of the vortioxetine hydrobromide intermediate and ensure controllable quality of a vinpocetine hydrobromide final product. The method has the advantages of strong specificity, high accuracy and convenience in operation.

The invention belongs to the field of analytical chemistry and discloses a method for separating and determining maleic acid asenapine and impurities thereof by a liquid chromatography. The method adopts a chromatographic column taking octyl silane bonded silica gel as a filler, buffer salt solution-organic phase with certain proportion is used as a moving phase, the contents of the maleic acid asenapine and the impurities thereof can be quantitatively determined, and the quality of the maleic acid asenapine can be effectively controlled. The method has strong specificity, high accuracy and convenience in operation.

The invention belongs to the field of analytical chemistry, relates to a method for the simultaneous determination of palonosetron hydrochloride and four impurities. In particular, a high performance liquid chromatography method is employed for the simultaneous separation and determination of palonosetron hydrochloride and four process impurities A-D (including a degradation product). The column used in the method employs octadecyl silane bonded silica gel as a filler, and the method employs an inorganic salt buffer system supplemented with a certain proportion of an ion pair reagent and an organic solvent as the mobile phases for gradient elution. The method can simultaneously fully separate the process impurities and degradation products of palonosetron hydrochloride, has the advanategs of simpleness, feasibility, good reproducibility and strong specificity, and can effectively determinw palonosetron hydrochloride bulk drugs and medicine and the content of the relevant materials in the preparation.

The invention belongs to the field of analytical chemistry and discloses a method for separating and detecting lurasidone hydrochloride intermediate 3-(1-piperazinyl)-1,2-benzisothiazole and related substances through liquid chromatography. According to the method, octyl silane bonded silica gel serves as a chromatographic column of filler, ion-pairing reagent-buffer salt solution-organic phase in a certain proportion serves as a mobile phase, and the content of the lurasidone hydrochloride intermediate and the related substances of the intermediate can be measured, so that purity of reactants in the production process of lurasidone hydrochloride is effectively controlled, side reactions and impurities are reduced, the yield of the product is increased, and the quality of the product is improved. The method is high in specificity, high in accuracy and easy and convenient to operate.

The invention discloses a pharmaceutical analysis method for efficiently determining gangliosides GM1 and impurities thereof, and belongs to the technical field of pharmaceutical analysis. According to the method, a chromatographic column taking octadecylsilane chemically bonded silica as a filler is used as a stationary phase, and a mixed solution of a buffer salt solution and an organic phase isused as a mobile phase, so that the gangliosides GM1 related substances and content can be effectively separated and determined.

The invention belongs to the field of analytical chemistry, and discloses a method for separating and determining oxiracetam and a midbody of the oxiracetam by utilizing liquid chromatography. The method is characterized in that octadecyl silane bonded silica gel is used as a chromatographic column of filler, an organic phase with a given ratio of ion to reagent is adopted as a mobile phase, the content of each midbody in the oxiracetam can be quantitatively determined, so that the quality of the oxiracetam can be effectively controlled. According to the method, the exclusiveness is strong, the accuracy is high, and the operation is simple and convenient.

The invention belongs to the field of analytical chemistry, and the invention discloses a method for separating and detecting a relevant substance of a lurasidone hydrochloride intermediate 3-(1-piperazinyl)-1,2-benzisothiazole by using a gas chromatographic technique. A methylpolysilicone medium polar capillary chromatographic column and a hydrogen flame ionization detector are adopted by the method; the content of the relevant substance of the lurasidone hydrochloride intermediate can be quantitatively measured; thus, the purity of a reactant in the process of synthesizing the lurasidone hydrochloride is effectively controlled; the occurrences of side reactions and the generation of impurities are reduced; the yield of a product is improved. The method provided by the invention is quick in separation and detection, high in specificity and high in accuracy, and is simple and convenient to operate.

The invention discloses a method for separating and determining a lurasidone hydrochloride intermediate (1R,2R)-1,2-cyclohexanedimethanol and related substances thereof by using gas chromatography. The method employs a polysiloxane nonpolar capillary chromatographic column and a hydrogen flame ionization detector, can quantitatively determine the contents of the lurasidone hydrochloride intermediate and the related substances thereof, so purity of reactants in the process of synthesis of lurasidone hydrochloride is effectively controlled, occurrence of side reactions and generation of impurities are reduced, and product yield is improved. The method provided by the invention is fast in separation and detection, good in specificity, high in accuracy, and easy and simple to operate.

The invention provides a method for determining related substances in Trelagliptin tablets, and relates to the field of analytical chemistry. The method comprises the steps that a high-performance liquid chromatography method is adopted, a sample solution is injected into a high-performance liquid chromatographic instrument, determination of the related substances in the Trelagliptin tablets is completed, and the chromatographic conditions are that a chromatographic column takes silica gel of which the surface is provided with electric hybrid particles as a filler, a mobile phase A is an acidic aqueous solution, a mobile phase B is an organic solvent, the sum of the volume percent of the mobile phase A and the volume percent of the mobile phase B maintains 100% all the time, and linear gradient elution is conducted. According to the method for determining the related substances in the Trelagliptin tablets, an Xselect C18 chromatographic column is adopted, optimization is conducted on the mobile phase gradient elution program, and the related substances in the Trelagliptin tablets can be effectively separated. The separation determination problem of the related substances in the Trelagliptin tablets is solved, and therefore it is guaranteed that the quality of the Trelagliptin tablets is controllable.

The invention belongs to the field of analytical chemistry, and discloses a method for separating and determining a memantine hydrochloride starting material 1, 3-Dimethylaminamantine and related substances thereof by using a gas chromatography. The method adopts a capillary chromatographic column filled with 100% dimethyl polysiloxane anda hydrogen flame ionization detector, and canquantitatively determine the content of the memantine hydrochloride starting material and the related substances thereof, so that the purity of reactants in the process of synthesizing memantine hydrochloride is effectively controlled, side reactions and impurities are reduced, and the product yield is improved. The method is high in specificity, high in accuracy and simple and convenient to operate.

The invention belongs to the field of analytical chemistry and discloses a method for separating and determining etoricoxib and related substances thereof by using liquid chromatography. The method can be used for quantitatively determining the contents of etoricoxib and related substances thereof by using phenyl silane bonded silica gel as a chromatographic column of fillers and using a certain proportion of buffer salt solutions-organic phases as mobile phases, thus effectively controlling the quality of etoricoxib. The method has strong specificity and high precision and is simple and convenient to operate.

The invention relates to a method for separating and measuring the impurity-diglycol acid (natrium) (DGA) in carboxymethyl chitosan by a liquid chromatography method. A high-efficiency liquid chromatography method for separating and measuring the impurity DGA in carboxymethyl chitosan products adopts a chromatographic column taking C18 as stuffing, takes mixed solutions prepared by buffer salts with the PH value being 1.5-3.5 and organic phases according to a certain mixture ratio as a flowing phase, and performs detection and quantization by an ultraviolet detector. The method can effectively separate and measure the impurity DGA in the carboxymethyl chitosan and solves the problem of separation and measurement of the impurity DGA in the carboxymethyl chitosan, thereby ensuring the controllable quality of the carboxymethyl chitosan.

The invention discloses a method for measuring nebivolol hydrochloride impurities by a liquid phase chromatography method. Cellulose three(3, 5-dimethylphenyl amino formate is taken as a chiral chromatographic column of a filling material, and a mixed solution of a buffer salt solution and an organic phase according to certain ratio is taken as a mobile phase. The method can rapidly and accurately separate and measure the two optical isomers.

The invention belongs to the field of analytical chemistry. The invention discloses a method for rapidly separating and detecting the optical purity of a brivaracetam starting material (R)-4-propyl-dihydrofuran-2-one by using gas chromatography. According to the method, a cyclodextrin chiral capillary chromatographic column and a hydrogen flame ionization detector are adopted, so that the opticalpurity and the isomer content of the brivaracetam starting material can be quantitatively determined, and the stability of the optical isomer of the brivaracetam starting material is indicated. The method disclosed by the invention is strong in specificity, high in accuracy, good in durability and simple and rapid to operate.

The invention belongs to the field of analytical chemistry. The invention discloses an analysis method for separating and determining a vortioxetine hydrobromide intermediate and its isomers by usingliquid chromatography. The method uses a chromatographic column filled with phenyl bonded silica gel as a filler and a certain proportion of a buffer salt solution-organic phase as a mobile phase, andcan quantitatively determinethe content of the vortioxetine hydrobromide intermediate and isomers thereof so that the mass of a vortioxetine hydrobromide starting material is effectively controlled,side reactions are reduced, and therefore it is guaranteed that the quality of a vortioxetine hydrobromide final product is controllable. The method is strong in specificity, high in accuracy and simple and convenient to operate.

The invention belongs to the field of analytical chemistry, and concretely relates to a method for separating and determining diflucortolone as well as 6 beta diflucortolone and 16 beta diflucortolonethereof. A stationary phase adopted by the method is an octylsilanebonded silica gel. The method comprises the concrete steps of injecting a diflucortolone sample solution into a chromatographic instrument, adopting a mixed solution of a potassium hexafluorophosphatebuffer salt system and an organic solvent as a moving phase for eluting, and detecting in a detector. The method can be used for separating and content-determining of the diflucortolone as well as the 6 betadiflucortolone and the 16 beta diflucortolone thereof at the same time, achieves better effects on tailing factors and theoretical pedal number, has excellent separating property and durability, and is simple, convenient, feasible, good in reproducibility, efficient, fast, and high in specificity.

The invention discloses a method for measuring related substances in succinic acid Trelagliptin raw materials and relates to the field of analytic chemistry. According to the method, high performance liquid chromatography is adopted, a sample solution is injected into a high performance liquid chromatograph, and the related substances in the succinic acid Trelagliptin raw materials are measured; according to chromatographic conditions, a 100-5C18 chromatographic column of the Kromasil company is adopted as a chromatographic column, a flowing phase A and a flowing phase B are both a mixed solution of an acid aqueous solution and an organic solvent, the sum of the volume percentage of the flowing phase A and the volume percentage of the flowing phase B is kept 100% all the time, and linear gradient elution is performed. According to the method, the 100-5C18 chromatographic column of the Kromasil company is adopted, the gradient elution program of the flowing phases is optimized, and the related substances in the succinic acid Trelagliptin raw materials can be effectively separated. The method solves the separation and measurement problem of the related substances in the succinic acid Trelagliptin raw materials, and therefore it is guaranteed that the mass of the succinic acid Trelagliptin raw materials is controllable.

The invention belongs to the field of analytical chemistry, relates to a method for separating and measuring bilastine and technical impurities in a preparation of bilastine, and specifically relates to a method for separating and measuring bilastine and six technical impurities A-F (including a degradation product) in the preparation of bilastine by adopting high performance liquid chromatography. An adopted chromatographic column takes octylsilane bonded silicone as a filler, and adopts an inorganic salt buffer system with an ion-pairing agent added and an organic solvent, wherein the inorganic salt buffer system and the organic solvent is according to a certain ratio, as a moving phase for gradient elution. According to the method, the technical impurities A-F of bilastine and the degradation product can be totally separated. The method is simple to operate and good in reproducibility. The content of a raw medicine of bilastine and relevant materials in the preparation can be effectively measured, and the method is good in specificity.

The invention belongs to the field of analytical chemistry and discloses a method for separating and determining etoricoxib and related substances thereof by using liquid chromatography. The method can be used for quantitatively determining the contents of etoricoxib and related substances thereof by using phenyl silane bonded silica gel as a chromatographic column of fillers and using a certain proportion of buffer salt solutions-organic phases as mobile phases, thus effectively controlling the quality of etoricoxib. The method has strong specificity and high precision and is simple and convenient to operate.

The invention belongs to the field of analytical chemistry and relates to a method for separating and determining a linezolid raw material (S)-1-acetamido-2-acetoxyl-3-chloropropane X3 and its process impurities X2, in particular to a method for separating and determining a linezolid raw material X3 and its process impurities X2 by adopting a high performance liquid chromatography. A chromatographic column adopted in the method uses octadecyl silane bonded silica gel as a filler, water added with an ion-pairing agent and acetonitrile which are in certain proportion are adopted as mobile phases. The method can completely separate the linezolid raw material (S)-1-acetamido-2-acetoxyl-3-chloropropane X3 and the its process impurities X2, is simple, convenient, feasible, good in reproducibility and strong in specificity and can effectively determine the related substance content in the linezolid raw material (S)-1-acetamido-2-acetoxyl-3-chloropropane X3.

The invention discloses a method for measuring degraded impurities in orlistat capsules and relates to the field of analytical chemistry.According to the method, a high performance liquid chromatographic method is adopted, an impurity mixed reference substance solution and a sample solution are injected in a high performance liquid chromatograph, and measurement of the degraded impurities in the orlistat capsules is completed.According to the chromatographic conditions, silica gel solid sphere particles are used as filler of a chromatographic column; a mobile phase A is an acidic water solution, a mobile phase B is an organic solvent, the sum of the percent by volume of the mobile phase A and the percent by volume of the mobile phase B is kept 100% all the time, and linear gradient elution is carried out.According to the method, the Cortecs C18 (Waters, 150 mm*4.6 mm, 2.7 micrometers) chromatographic column is adopted, and by optimizing the mobile phase gradient elution procedure, all the degraded impurities and process impurities hard to separate nearby a main peak can be separated under the same chromatographic conditions, and the degraded impurities in the orlistat capsules can be effectively detected.

The invention belongs to the field of analytical chemistry, and concretely relates to a method for separating and determining diflucortolone as well as 6 beta diflucortolone and 16 beta diflucortolonethereof. A stationary phase adopted by the method is an octylsilanebonded silica gel. The method comprises the concrete steps of injecting a diflucortolone sample solution into a chromatographic instrument, adopting a mixed solution of a potassium hexafluorophosphatebuffer salt system and an organic solvent as a moving phase for eluting, and detecting in a detector. The method can be used for separating and content-determining of the diflucortolone as well as the 6 betadiflucortolone and the 16 beta diflucortolone thereof at the same time, achieves better effects on tailing factors and theoretical pedal number, has excellent separating property and durability, and is simple, convenient, feasible, good in reproducibility, efficient, fast, and high in specificity.

The invention relates to the technical field of pharmaceutical analysis, in particular to a method for analyzing ethyl gatetanecarboxylate and related impurities by using high performance liquid chromatography. A chromatographic column adopted by the method takes octadecyl bonded silica gel as a filling agent, a buffer salt solution and an organic solvent are adopted for gradient elution, the flow velocity is 0.9-1.1 ml / min, and the column temperature is 18-22 DEG C; the detection wavelength is 220 nm or 250 nm; the method can effectively separate and accurately quantify seven known impurities possibly existing in the starting material ethyl gatetanecarboxylate of moxifloxacin hydrochloride within 42 minutes, the separation effect of the other two known impurities possibly existing in the starting material and the seven known impurities is good, and the method has no interference on impurity identification and quantitative detection. The problem of separation and determination of known impurities in ethyl gatetanecarboxylate, which cannot be solved in the prior art, is provided; the analysis method is high in sensitivity; the specificity is high; the reproducibility is good; the operation is simple and feasible.

The invention belongs to the field of analytical chemistry, and discloses a method for separating and determining a compound A[(2RS)-1-ethyl pyrrolidinone-2-yl-methylamine] and imidazole in an amisulpride final product {4-amino-N-[[(2RS)1-ethyl pyrrolidinone-2-yl] methyl]-5-(ethyl sulfonyl)-2-methoxybenzamide} by using a gas chromatographic method. According to the method, a capillary chromatographic column filled with polyethylene glycol and a hydrogen flame ionization detector are adopted, and the content of impurities A[(2RS)-1-ethyl pyrrolidone-2-yl-methylamine] and imidazole in a final product of amisulpride can be quantitatively determined, so that the purity of reactants in the process of synthesizing amisulpride is effectively controlled, side reactions and impurities are reduced, and the product yield is improved. The method is high in specificity, high in accuracy and simple and convenient to operate.

The invention belongs to the field of analytical chemistry and discloses a method for separating and determining imidafenacin and related substances thereof by using liquid chromatography. The method can be used for quantitatively determining the contents of imidafenacin and related substances thereof by using phenyl silane bonded silica gel as a chromatographic column of fillers and a certain proportion of buffer salt solutions-organic phases as mobile phases, thus effectively controlling the quality of imidafenacin. The method has strong specificity and high precision and is simple and convenient to operate.