31 results about "Impurity profiling" patented technology

The invention relates to an application of a solid-phase extraction column in analysis of tacrolimus preparation ointment. In the preparation process of the test sample, the solid-phase extraction column with diol silane bonded silica gel as a filler is adopted for purification, and through the steps of suspension, activating, sample loading, leaching and elution, the tacrolimus and related substances thereof in the tacrolimus ointment sample are effectively separated. Moreover, the organic solvent is saved, the time consumption is short, the specificity is good, auxiliary materials do not interfere with tacrolimus impurity detection, and the impurity recovery rate also meets the requirements. The method is particularly suitable for effectively separating tacrolimus and related substancesfrom a complex matrix of tacrolimus ointment.

The invention relates to an impurity analysis method of a steroid compound, and especially relates to an impurity detection analysis method of norethisterone derivatives and intermediates thereof. The method comprises the following steps: (1) a chromatographic column with octadecylsilane chemically bonded silica as a filler is selected; a mobile phase gradient elution is carried out, and the mobile phase contains water, methanol and acetonitrile; the detection wavelength is 230-254nm; and (2) a proper amount of the test sample norethisterone derivatives or intermediates thereof are selected, methanol is precisely weighed for dissolving and diluting the test sample to form a sample solution of a certain concentration, the solution is uniformly shaken, and a high performance liquid chromatography analysis is carried out at a proper flow velocity and a proper column temperature, in order to record a chromatogram. The method can be used for rapidly and accurately realizing impurity analysis of norethisterone derivatives, and is especially suitable for the impurity analysis of norethisterone enanthate, and simultaneously can be used for impurity analysis of norethisterone derivative intermediates, and can be used for effectively tracing impurities generated in the synthesis process.

The invention discloses a ketorolac impurity C and a preparation method and application thereof. According to the method, the ketorolac impurity C is prepared by taking pyrrole as an initial raw material through a series of reactions such as substitution, oxidation and alkaline hydrolysis, and the ketorolac impurity C is one of important impurities of ketorolac drugs or preparations thereof and can be used for toxicological and pharmacological researches such as in-vivo absorption and metabolism of ketorolac, and can also be applied to research on stability and quality control of ketorolac preparations. The preparation method of the ketorolac impurity C has the advantages of simplicity in operation, safety in reaction and high purity and yield, and can be widely applied to the fields of impurity analysis, toxicological research, safety detection, stability judgment and the like of ketorolac bulk drugs and preparations thereof.

The invention provides a method for analyzing peptide fragment impurities in high-purity polypeptide based on data mining. The operation method for analyzing the peptide fragment impurities in the high-purity polypeptide comprises the following steps: during peptide fragment impurity analysis, based on a data dependence acquisition strategy, optimizing a detection data set and an identification data set while analyzing; adopting an onion peeling strategy to sequentially identify high-abundance impurity peptide fragments, wherein the subsequent analysis is no longer specific to the identified peptide fragments, the precious window period is saved, and the non-identified second-high-abundance peptide fragment impurities are identified; and finally, carrying out selective enrichment on peptide fragment ions which are pre-judged to be ultralow in abundance for multiple times, and then identifying. Therefore, the identification number of peptide fragment impurities in the high-purity polypeptide is remarkably increased.

The present invention relates to an automatic detection method and apparatus, and particularly is a fast evaluation method and apparatus applied to seed cotton impurities in a seed cotton purchasing link. In an existing seed cotton purchasing process, a seed cotton impurity analytical engine is mainly used for performing an impurity separating test on seed cotton to detect a percentage of impurities, in which an impurity detection procedure is complicated and is slow in speed. As a result, a phenomenon of seed cotton transport vehicle queuing is serious. The fast evaluation method and apparatus proposed in the present invention are used for resolving a problem that a speed of detecting a percentage of impurities in seed cotton is slow in a purchasing process. The fast evaluation apparatusin the present invention comprises a pneumatic cotton delivery apparatus, a seed cotton large-impurity cleaning apparatus, a pushing apparatus, a seal capping apparatus, a conveying apparatus and an online imaging detection apparatus. The evaluation method and apparatus resolve technical problems that a procedure of detecting a percentage of impurities in seed cotton in a purchasing process is complicated and slow in speed and the like, and provides a real-time basis for seed cotton transaction settlement.

The invention relates to a gas chromatography detection method in a caprolactam production process. The method uses gas chromatography to detect an intermediate product at a quality control point in caprolactam production, and the gas chromatography uses a strongly polar chromatographic column stationary liquid selected from at least one of bonded polyethylene glycol and cross-linked polyethyleneglycol. According to the gas chromatography detection method in the caprolactam production process, the separation effect is high, and the impurity detection capacity is good. The impurity analysis capability of each control point in the caprolactam production process is improved, and caprolactam production enterprises can be better guided to carry out lean production control.

The invention discloses a decomposition method for analyzing trace impurities of a metal organic compound, which comprises the following steps of feeding a dry sampling bottle and a sampling device which are accurately weighed into an inert atmosphere operation box, taking the metal organic compound by using the sampling device, and putting the metal organic compound into the sampling bottle, accurately weighing a sampling bottle and the total weight of the metal organic compounds in the sampling bottle, then sequentially connecting the sampling bottle, a buffer bottle, an absorption bottle and a drying bottle in the inert atmosphere operation box, slowly introducing ultrapure water into the sampling bottle in the form of water vapor, and after complete decomposition, preparing a corresponding to-be-detected solution by absorbing a nitric acid or hydrochloric acid solution with the mass percentage of 5% for substance in the bottle and detecting. The water vapor is adopted to decompose the metal organic source to form the soluble hydroxide, and the method has the advantages of easiness in operation, good safety, short detection time, no environmental pollution, good analysis result repeatability, wide applicability and the like.

The invention discloses an ultra-high performance liquid chromatography analysis method for dihydralazine sulfate and related substances thereof. Waters UPLC AcQuity H-Class is used, a reversed-phaseC18 column is adopted, a monopotassium phosphate-phosphoric acid buffer solution is used as a mobile phase A, and methanol is used as a mobile phase B, and then gradient elute treatment is performed.According to the method, the known impurity content can be effectively controlled through a main component self-contrast method with correction factors, and the separation degree between a main peak and adjacent impurity peaks and the separation degree between the main peak and each impurity peak are both larger than 1.5. The method is simple, convenient to operate, good in reproducibility and accurate in impurity analysis and positioning, and a reliable analysis method can be provided for controlling the quality of dihydralazine sulfate and tablets thereof.

The invention discloses an impurity analysis instrument for chemical detection, and relates to the technical field of chemical detection, in particular to an impurity analysis instrument for chemical detection, which comprises an analyzer shell, wherein support legs are fixed below the analyzer shell; a display screen embedded in the outer wall of the analyzer shell; a feeding pipe arranged above the analyzer shell, wherein the upper part of the feeding pipe is connected with a quantitative box, and the feeding pipe is communicated with the quantitative box; a metal detection head fixedly arranged on the outer wall of the feeding pipe; and an analysis box. According to the impurity analysis instrument for chemical detection, the quantitative box is arranged, industrial impurities are put into the quantitative box by opening a protective cover, the industrial impurities in the quantitative box can be conveniently observed under the action of a dial gauge, and the protective cover is closed after the industrial impurities are put to a proper amount, so that the quantitative function is achieved; and the situation that needed detection data cannot be accurately obtained due to the fact that too many industrial impurities are put is avoided, and practicability is high.

The invention discloses a method for cleaning a gas chromatographic column for analyzing trace impurities in high-purity carbonic ester. The method aims to solve the problem that measurement accuracy is influenced by chromatographic column residues in analysis of trace impurities in high-purity carbonic ester, a sample injection cleaning method is adopted, the method is a chromatographic method for keeping sample analysis, and a cleaning agent is injected into a chromatograph for operation, and then one-time non-injection operation is executed. The cleaning agent is an organic solvent capable of dissolving the carbonic ester to be detected, is extremely high in content and lower in boiling point, and does not easily cause component residues; and meanwhile, trace impurity residues can be dissolved out, and the trace impurity residues can be completely eliminated through sample injection-free operation. The method does not need to disassemble and assemble an instrument, is simple to operate and short in time consumption, does not damage the chromatographic column, and has a cleaning elimination rate of trace impurity residues greater than 99%.

The invention discloses a method for determining the impurity content of recycled plastic. The method comprises the steps of sample pretreatment, sample detection, impurity analysis and generation of a quantitative estimation model. According to the method for determining the impurity content of the regenerated plastic, physical detection and chemical instrument detection are combined, the content of visible impurities in the regenerated plastic can be analyzed and detected, and the content of invisible impurities can also be analyzed and detected. According to the method, qualitative analysis and quantitative analysis are carried out on the impurity content in the recycled plastic, the impurity components and content in the same recycled plastic can be generally known, an impurity quantitative estimation model can be generated according to the impurity analysis result of the recycled plastic, and the impurity content of the same recycled plastic sample can be estimated.

The invention discloses a method for detecting the purity of pimpinolide. The invention belongs to the technical field of traditional Chinese medicine purity detection. The method comprises the following steps: (1) preparation of a test solution: precisely weighing 1.75-3.0 mg of a pimpinolide test sample, putting the test sample into a 1mL or 3mL volumetric flask, fixing the volume to a scale byusing a 50% acetonitrile-water mixed solution, uniformly shaking, passing through a 0.22 mu m microfiltration membrane or centrifuging, and taking the supernatant for later use; (2) detecting the testsolution by using ultra-high performance liquid chromatography and gradient elution, wherein the detection conditions are as follows: a chromatographic column is a reversed-phase C18 column; the column temperature of the chromatographic column is 20-45 DEG C; a mobile phase: the mobile phase A is methanol or acetonitrile; the mobile phase B is water; wherein the flow rate is 0.2 mL/min to 0.5 mL/min; the detector is a diode array detector, and the detection wavelength of the diode array detector is 254-330nm; wherein the sample size of the pimpinolide test solution is 0.2 mu L-1. 0mu L. The invention further discloses a detection method of the pimpinolide. The method provided by the invention has the characteristics of accuracy, sensitivity and quickness, provides reliable guarantee for impurity analysis of the pimpinolide, and also saves time and material cost.

The invention discloses an impurity generated in production of indapamide as well as a synthesis method and application. The synthesis method of the indapamide impurity D comprises the following stepsof: reacting an initial raw material A with thionyl chloride, and carrying out reduced pressure distillation to obtain a compound B, carrying out acylation reaction on the compound B and C, and recrystallizing petroleum ether and ethyl acetate to obtain a compound D. The invention provides a simple synthesis method of the indapamide impurity D. The synthesized indapamide impurity D can provide impurity contrast monitoring for reaction, and the problem of impurity analysis and control of indapamide is solved. And a strong support is provided for large-scale industrial production of indapamide.

The present invention relates to an omeprazole process impurity and a preparation method thereof, the omeprazole process impurity has a structure represented by a formula I: wherein X<-> is CH3SO4<->or HSO4<->. Separation, confirmation and preparation of the omeprazole process impurity are beneficial to impurity analysis of an omeprazole intermediate and an omeprazole bulk drug, and improvement of a synthesis process of the omeprazole intermediate and the omeprazole bulk drug, so that further improvement of the quality standard and control of the omeprazole bulk drug is facilitated; the quality level of the raw material medicine is improved, and guarantee is provided for the medication safety of people.

The invention provides a sitagliptin key intermediate impurity as well as a preparation method and application thereof, which belong to the technical field of medicinal chemistry. The compound with the structure as shown in the formula I provided by the invention is an impurity component generated in the production process of a key intermediate acetyl Meldrum's acid derivative 5-(1-hydroxy 2-(2, 4, 5-trifluorophenyl)ethylene)-2, 2-dimethyl-1, 3-dioxepin-4, 6-diketone) (II) for synthesizing sitagliptin. The impurity can be used as a reference substance to be applied to impurity analysis of keyintermediates in a sitagliptin production process so as to promote quality control of the key intermediates and further effectively control the quality of sitagliptin drugs. The invention provides thepreparation method of the sitagliptin key intermediate impurity, the synthesis method of the impurity reference substance of the sitagliptin key intermediate is established through pyrolysis, the method is a basis for researching impurity composition and quality control of sitagliptin, and the method is strong in operability and simple.

The invention discloses a method for separating and analyzing impurities in NF3, which adopts gas chromatography with double blowback or double cutting systems, takes high-purity helium as carrier gas, configures a helium discharge ionization detector, and comprises the step of emptying main components by using a blowback switching valve after the impurities flow out of a pre-column. According tothe method for separating and analyzing the impurities in the NF3, the impurities are separated, the analysis time is short, and the separation effect is remarkable. A large amount of NF3 can be prevented from entering the detector, and the detector is effectively protected.

The invention discloses an ultra-high performance liquid chromatography analysis method of clozapine. The method comprises the following steps: carrying out gradient elution by using a Waters UPLC (Ultra Performance Liquid Chromatography) AcQuity H-Class, adopting an Agilent Rapid Response HD column and taking methanol-potassium dihydrogen phosphate-water as a mobile phase. According to the method, all known impurities in the clozapine raw material and the preparation thereof can be analyzed at the same time, the content of the known impurities can be effectively controlled through a main component self-control method with correction factors, and the separation degree between a main peak and adjacent impurity peaks and the separation degree between all impurity peaks are larger than 1.5. The method is simple, short in time and accurate in impurity analysis, and a reliable analysis method is provided for clozapine.

The invention relates to a preparation method of a zagrel impurity. The method includes the steps of: adding methyl 4-bromomethylcinnamate and sodium methoxide into a proper amount of methanol according to a mass ratio of 5:1, and blending the substances into a dilute solution; performing stirring for 2-16h under a room temperature condition to enable full reaction of the mixture, thus obtaining amixed solution containing ozagrel impurity; concentrating the ozagrel impurity by vacuum rotary evaporation method; and carrying out purification treatment on the ozagrel impurity by column chromatography process. The method provided by the invention can simply and directly acquire an ozagrel impurity reference substance, also provides convenience for impurity analysis and research of ozagrel crude drugs and preparations thereof, and provides a detection method and judgment basis for production and medication safety of ozagrel.