54 results about "Linear gradient" patented technology

The invention belongs to the technical field of 3D printing, and particularly relates to a 3D printing control method based on multi-material gradient transition, which comprises the steps of model processing, multi-material distribution, path planning, dynamic parameter control, online monitoring and feedback optimization. According to the method, through dynamic mixing of a nonlinear gradient function and multiple materials, limitation of traditional discrete material switching is broken through, continuous smooth transition of material attributes is achieved, printing parameters are dynamically adjusted, and the forming consistency of gradient materials under complex working conditions is remarkably improved; local strengthening is carried out according to the thermodynamic property difference of a multi-material interface, interface embrittlement caused by a traditional single process is avoided, the curing degree is detected in real time through a spectrum sensor, the problem that the curing degree of a traditional light curing process is uncontrollable is solved by combining partitioned UV light intensity adjustment and control, and precise gradient forming of a soft and hard alternate structure is achieved.

The invention is suitable for the technical field of filters, and particularly relates to a manufacturing method of a linear gradient filter and the linear gradient filter. The manufacturing method of the linear gradient filter comprises the following steps that a glass wafer serves as a substrate, and a lower reflecting layer is plated on the surface of the glass wafer; wherein the lower reflecting layer is formed by alternately stacking a plurality of layers of low-refractive-index materials and a plurality of layers of high-refractive-index materials; coating a resonant cavity layer on one side, far away from the glass wafer, of the lower reflecting layer through a stepped coating process; plating a reflecting layer on one side, far away from the glass wafer, of the resonant cavity layer; and plating a long-wave-pass layer on one side, far away from the glass wafer, of the upper reflecting layer and in an area larger than the central wavelength to obtain the linear gradient filter. Compared with the prior art, the linear gradient filter provided by the invention is better in spectral resolution in a long wave band, smaller in energy difference of channels, excellent in wavelength selection performance and capable of being applied to spectrum applications such as a miniaturized infrared spectrometer and the like.

The invention provides a wafer detection method and system based on multichannel C scanning, and aims to solve the problems of multichannel sensitivity difference, Z-axis height deviation, splicing artifacts and the like in a traditional system. The maximum defect point and the defect-free point of the standard sheet are selected before detection, the gain of each channel is adjusted to a unified amplitude, and the echo amplitude is recorded, so that sensitivity calibration is realized; in the detection process, a laser displacement sensor is used for collecting wafer surface height data in real time, modeling is conducted in combination with an ARIMA + Kalman filtering or Gaussian process regression algorithm, the Z-axis focusing distance is dynamically adjusted through PID feedback, and signal attenuation caused by surface warping is compensated; during image splicing, channel response is optimized by adopting three gray mapping modes of linear self-adaption, Gamma self-adaption (automatic alignment channel mean value after reference gamma setting) and manual setting, sub-pixel level offset is calculated based on a two-dimensional cross-correlation function to realize coordinate alignment, and a 5% overlapping area is set at a channel junction. Gray transition is completed through linear gradient weight weighted averaging.

The invention provides a method for identifying polymers in ceftazidime / ceftazidime for injection. The method is characterized in that the ceftazidime / ceftazidime for injection is analyzed by adopting an RP-HPLC (Reverse Phase-High Performance Liquid Chromatography) method; the chromatographic conditions of the RP-HPLC are as follows: a 10-20 mmol / L ammonium formate solution with the pH value of 3.4-3.6 is used as a mobile phase A; methanol / acetonitrile in a ratio of 1: (1-2) is taken as a mobile phase B; linear gradient elution is carried out, and the flow velocity is 1.0-2.0 ml / min; the detection wavelength is 254 nm. The method can be used for effectively detecting the polymer in the ceftazidime / the ceftazidime for injection.

The invention relates to the technical field of rock mechanics true triaxial tests, in particular to a rock cylinder sample true triaxial test analysis method which comprises the following steps: applying a point load to the cylindrical surface of a cylinder sample, performing integration by using a linear superposition principle, and calculating an analytical solution of an internal stress field in the circular surface of the rock cylinder sample; applying a symmetry plane load to the cylindrical surface of the cylinder sample, and calculating an internal stress field of the circular surface of the cylinder sample under the symmetry plane load by using an analytical solution; setting a constraint condition of a stress state similar region, calculating a relation function between symmetrical surface loads in a corresponding loading mode, and determining the relation function as a linear gradient loading mode; and performing finite element analysis on the cylindrical sample of the rock, and verifying the feasibility of the linear gradient loading mode determined by the analytical solution. According to the invention, true triaxial test analysis of the cylinder sample is realized, the internal stress state of a larger area of the sample is ensured to be similar, and the problems of boundary effect, friction effect, fluid channeling and the like of a cubic sample are avoided.

The invention belongs to the field of liquid chromatography-mass spectrometry detection, and discloses a liquid chromatography-mass spectrometry detection method for trace target objects in seawater, which comprises the following steps: firstly, configuring and precisely calibrating parameters such as flow velocity, column temperature, ion source voltage and the like for a liquid chromatography system, a chromatographic column, an automatic sampler and a tandem mass spectrometer; then, a methanol-water (containing 0.1% formic acid) system is adopted to implement linear gradient elution, polar difference component separation is considered, and analysis duration is compressed; a sample is subjected to solid-phase extraction, purification and concentration, then is automatically injected, is subjected to chromatographic separation and then enters an electrospray ion source; a mass spectrum end selects a dynamic multi-reaction monitoring (dMRM) mode, characteristic ion pairs are collected in a preset time window, and selective scanning and baseline noise suppression are achieved; and finally, utilizing retention time matching and internal standard correction to obtain a pg.L <-1 > magnitude quantitative result.

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 belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and determining a rupatadine fumarate starting material SM1 and impurities thereof. According to the method, phenylsilane bonded silica gel is adopted as a chromatographic column filler, mobile phases comprise a mobile phase A and a mobile phase B, the mobile phase A is a monopotassium phosphate solution, and the mobile phase B is acetonitrile; the method comprises the following steps: sequentially separating an impurity SM1a, rupatadine fumarate SM1, an impurity SM1o, an impurity SM1j, an impurity SM1g, an impurity SM1m, an impurity SM1i, an impurity SM1n, an impurity SM1k, an impurity SM1f, an impurity SM1b, an impurity SM1l and / or an impurity SM1e through linear gradient elution; the rupatadine fumarate SM1 and 12 known impurities can be separated within 62 minutes by the high performance liquid chromatography constructed by the invention, the analysis time is short, the sensitivity is high, the specificity is strong, and the reproducibility is good.

The provided method includes: determining an energy parameter and a co-volume parameter of a pure gas by a PR state equation, and determining a material parameter and a co-volume parameter of a mixed gas by a Waals one-fluid mixing rule and a combination rule; determining a Helmholtz free energy density and an equilibrium density of the pure gas by a Wertheim molecular association theory, and determining Helmholtz free energy and an equilibrium density of a (H2+N2) mixed gas with different components by a density mixing rule; determining an influence parameter of the pure gas by a gradient theory (GT), and determining an influence parameter of the mixed gas by the influence parameter of the pure gas and an interaction coefficient; simplifying a GT model; and obtaining the surface tension of the (H2+N2) / H2O system at different temperatures by combining the LGT model and the PR state equation.

The application provides a coating method for realizing a linearly graded filter and an angle adjusting device for an intermediate layer of the filter, and the coating method comprises the following operation steps: S1. correcting the uniformity of a plane; S2. establishing a database; S3. matching the product tilt angle through the angle and slope database; and S4. completing the preparation of the interval layer. The method utilizes the uniformity principle of an evaporation coating machine, changes the substrate tilt angle, changes the included angle between the normal line of the substrate and the single point-evaporation source connecting line, makes the included angles and distances of each point on the substrate present linear changes, and finally realizes the linear change of the film thickness in the substrate tilt direction.

The invention discloses a scanning type hyperspectral imaging device and method based on a linear gradient filter. The device sequentially comprises an imaging objective lens, a gradient filter assembly, a telecentric imaging lens group and a camera along the incident direction of a light path, during working, the one-dimensional linear displacement table drives the gradient filter assembly to perform linear scanning motion in the direction perpendicular to the optical axis, so that light in an imaging view field penetrates through band-pass filtering areas with different central wavelengths on the gradient filter in a time-sharing manner. The filtered monochromatic or narrow-band light is projected to a photosensitive target surface of the camera through the telecentric imaging lens group, and multiple frames of spectral images with different wavebands are continuously acquired. Collected sequence images are processed and reconstructed to form a hyperspectral three-dimensional data cube containing spatial information and spectral information. The system has the advantages of high imaging speed, high luminous flux, compact system structure, low cost and the like, and is suitable for hyperspectral data acquisition scenes with higher real-time requirements.

The invention discloses a pH value real-time regulation and stabilization method and system for online column separation, and belongs to the technical field of ion exchange chromatographic separation.The method comprises the steps that a proton disturbance signal is applied to a chromatographic column, an outflow response signal of the chromatographic column is detected, and a parameter map representing the dynamic buffer capacity characteristic of the chromatographic column is obtained; the parameter atlas and the target pH gradient are input into a physical transmission model based on convection, diffusion and adsorption coupling equations, and the physical transmission model outputs a predistortion pH gradient program used for compensating dynamic buffer capacity characteristics; according to a fluid proportion requirement which is defined by a pre-distortion pH gradient program and changes along with time; according to the method, dynamic buffer capacity characteristics can be obtained through a proton disturbance test, a pre-distortion pH gradient program is constructed, and closed-loop iterative optimization is combined, so that interference of the dynamic buffer capacity of the chromatographic column on proton transfer is effectively counteracted, a post-column effluent pH curve is accurately matched with a target linear gradient, and the problems of pH nonlinear distortion and a platform area are eliminated.

The invention relates to the technical field of preparation of natural products, in particular to a high-efficiency preparation method of active ingredients of semen cassiae seeds, anthraquinone compounds are purified by adopting linear gradient countercurrent chromatography, and two gradient mobile phases are adopted: n-hexane / ethyl acetate / methanol / water (5: 5: 5: 5, v / v) and (5: 5: 8: 2, v / v); n-hexane / ethyl acetate / methanol / water (5: 5: 5.5: 4.5, v / v) and (5: 5: 7: 3, v / v) are solvent systems for internal circulation separation; n-hexane / ethanol / water (1: 1: 0.2, v / v) is used as a solvent system of an off-line two-dimensional separation mode, and the separated substances are detected and analyzed through high performance liquid chromatography to obtain nine anthraquinone compounds.

The invention discloses a method for detecting related substances in an enconazole solution, and relates to the technical field of medicine detection. High performance liquid chromatography is adopted, octadecylsilane chemically bonded silica is used as a chromatographic column of a filler, a 0.025 mol / L monopotassium phosphate buffer solution (the pH value is adjusted to 2.6-3.0 by phosphoric acid) is used as a mobile phase A, acetonitrile is used as a mobile phase B, linear gradient elution is carried out, and the flow velocity of the mobile phase is 0.8-1.2 ml / min; the column temperature of the chromatographic column is 27-33 DEG C; the detection method can be used for effectively separating and determining the related substances of the enconazole solution, under the chromatographic conditions of the invention, each impurity peak is completely separated, the linear relationship between the concentration and the peak area within a limit range is good (r is greater than or equal to 0.999), and the recovery rate is 90.0-110.0%. The analysis method is easy and convenient to operate, good in specificity, high in accuracy, stable, reliable and suitable for determining the related substances of the enconazole solution.

The invention provides an analysis method of polymyxin B sulfate related substances, which comprises the following steps: dissolving polymyxin B sulfate for injection in water-acetonitrile (80: 20) to obtain a test solution; the method comprises the following steps: dissolving a polymyxin B standard substance in water-acetonitrile (80: 20), and uniformly shaking to obtain a standard substance solution; detecting the test solution and the standard solution by adopting a high performance liquid chromatography, wherein the detection adopts linear gradient elution; wherein the mobile phase A is a sodium sulfate solution; and the mobile phase B is acetonitrile. According to the technical scheme, a high performance liquid chromatography method is adopted, automatic operation can be achieved, repeatability is good, accuracy is high, sensitivity is high, component content and related substance inspection are combined into one method, the component content in a sample can be effectively detected, related substance inspection can also be considered, the detection time needed during quality control is shortened, and the analysis efficiency is improved.

The invention discloses a method for detecting a pitavastatin calcium intermediate and related substances thereof. According to the method, liquid chromatography is adopted for detection, and chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a chromatographic column of a filler; a PDA detector; the detection wavelength is 240 nm; the column temperature is 25-35 DEG C; the flow velocity is 0.8 to 1.2 ml / min; carrying out linear gradient elution by adopting a mobile phase A and a mobile phase B; the mobile phase A is a mixed solution of water, trifluoroacetic acid and ammonia water in a volume ratio of 1000: 1: 0.5; and the mobile phase B is acetonitrile. According to the method, effective separation and quantitative detection of various related substances of YPF-SM-A can be realized, effective separation among chromatographic peaks can be realized, the conditions of intermediates and related substances can be accurately qualitatively and quantitatively determined, and the method is simple, convenient, feasible and low in detection cost; the method can be used for conventional analysis and quality control of YPF-SM-A and related substances, and meets the requirements of research, development and production.

The invention discloses an on-chip optical system based on linear gradient device design, which is used for generating a coherent optical pattern with a sparse lattice structure. The cross section of the on-chip device sequentially comprises a waveguide layer, a bottom cladding layer and a substrate layer from top to bottom, a plurality of input waveguides are used, a linear gradual change device is coupled with an on-chip system, input light is guided into an interference area, and an optical lattice structure with specific symmetry is generated. Through the disclosed calculation method, a specified coherent lattice structure can be obtained by calculating a corresponding light beam configuration scheme. According to the method, while the periodicity and symmetry of the crystal lattice are kept, the movement of the crystal lattice pattern on a two-dimensional plane can be realized by regulating and controlling the phase of the input light beam through the phase modulator. Compared with a traditional method, the system has the advantages of being compact in structure, high in interference efficiency, flexible and adjustable in pattern and the like, and is suitable for application of biosensing, quantum calculation, microscopic imaging and the like.

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.

This invention belongs to the field of pharmaceutical analysis technology, specifically relating to a method for separating and detecting rifabutin and its impurities. The impurities include impurity B, impurity D, impurity E, impurity F, impurity G, impurity I, impurity J, impurity K, and impurity Z. 3b Impurity Z 3c Any one or more of the following. This method is a reversed-phase high-performance liquid chromatography (RP-HPLC) method. The chromatographic column uses octadecyl-bonded silica gel as the packing material, and a linear gradient elution is performed using mobile phases A and B. The chromatogram is obtained by detection using a detector. Mobile phase A is a mixture of phosphate buffer solution and organic solvent, and mobile phase B is a mixture of acid aqueous solution and organic solvent. This method can completely separate and detect rifabutin and its 10 impurities within 60 minutes, and features good resolution, robustness, high sensitivity, and good reproducibility.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and determining a linezolid intermediate Z4 and impurities thereof. The impurities comprise any one or more of an impurity Z2, an impurity Z3b, an impurity Z4b, an impurity Z3, an impurity Z4d, an impurity Z3c and an impurity Z4c. The self-built high performance liquid chromatography is used for separating and determining the linezolid intermediate Z4 and impurities thereof. A mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is a mixed solution of a buffer salt solution and acetonitrile; the mobile phase B is a mixed solution of methanol and acetonitrile; in a stationary phase, octadecylsilane chemically bonded silica is used as a filler of a chromatographic column, and linear gradient elution is carried out. Then, according to a chromatogram, the content of each impurity is calculated by adopting a main component self-contrast method with a correction factor. The method disclosed by the invention has the characteristics of good separation degree, good durability, high sensitivity and good reproducibility.

The present application relates to a method and system for additive manufacturing of continuous gradient materials with nonlinear composition transitions, which can solve the problem that traditional functional gradient materials with linear composition changes are prone to brittle phases and insufficient performance in composition-sensitive intervals. The method includes: determining the gradient step size according to the part size, and calculating the composition change rate of each layer based on the printing layer thickness and height; preparing full-composition functional gradient materials by linear transition, and identifying the brittle phase generation interval in combination with microstructure characterization methods; designing a nonlinear composition transition method for sensitive intervals to suppress element segregation and brittle phase generation, and optimize interface bonding strength and comprehensive performance. The composition of the gradient material prepared by this application is continuously controllable in any direction, and there is no sudden interface in the composition distribution. The strength, high-temperature oxidation resistance and thermal fatigue life are significantly better than those of traditional linear gradient materials, and it is suitable for high-performance demand scenarios such as aerospace, nuclear energy heat dissipation and biological implants.

The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for separating and determining rupatadine fumarate Z3 and impurities thereof by an HPLC (High Performance Liquid Chromatography) method. The method comprises the following steps: preparing a system applicability solution, a contrast solution and a sample solution by taking methanol as a solvent, and carrying out gradient elution by taking octadecylsilane chemically bonded silica as a chromatographic column filler, a phosphate solution as a mobile phase A and acetonitrile as a mobile phase B; the method comprises the following steps: sequentially separating an impurity Z2, an impurity Z2e, an impurity SM1, an impurity Z3c, an impurity Z3b, rupatadine fumarate Z3, an impurity Z3d, an impurity Z3a and / or an impurity Z1 through linear gradient elution, and detecting in a detector with the detection wavelength of 270nm. According to the HPLC method provided by the invention, rupatadine fumarate Z3 and eight related impurities can be separated within 40 minutes, and the HPLC method has the characteristics of short analysis time, high sensitivity, strong specificity and good reproducibility.

The application provides an image processing method based on a feathering mask and related components, and the technical scheme points are as follows: obtaining an inferred image sub-block and a position thereof; initializing a full-one mask for each sub-block; respectively calculating linear gradient weight maps in horizontal and vertical directions; multiplying the three to generate a target feathering mask with four-side gradient attenuation; and finally, weighting each sub-block and the corresponding mask, and then adding to a canvas according to the position to obtain a fusion image. Compared with the prior art, the application makes the corresponding pixel points of adjacent sub-blocks in the overlapping area satisfy a weight complementary relationship, reduces the condition that a traditional simple average or fixed weight fusion produces obvious joint lines at the splicing position, and thus improves the visual continuity of the fusion image.

This invention provides a wafer inspection method and system based on multi-channel C-scanning, aiming to address issues such as multi-channel sensitivity differences, Z-axis height deviation, and stitching artifacts in traditional systems. Before inspection, the maximum defect point and defect-free point on a standard wafer are selected, the gain of each channel is adjusted to a uniform amplitude, and the echo amplitude is recorded to achieve sensitivity calibration. During inspection, a laser displacement sensor is used to collect wafer surface height data in real time. Modeling is combined with ARIMA+Kalman filtering or Gaussian process regression algorithms, and the Z-axis focus distance is dynamically adjusted through PID feedback to compensate for signal attenuation caused by surface warping. For image stitching, three grayscale mapping methods are used to optimize channel response: linear adaptive, gamma adaptive (automatically aligning channel means after a reference γ is set), and manual setting. Coordinate alignment is achieved by calculating sub-pixel offsets based on a two-dimensional cross-correlation function. A 5% overlap area is set at the channel junction, and grayscale transitions are achieved through linear gradient weighted averaging.

The invention provides a method for improving quality control of busulfan injection, which comprises the following steps: injecting a test solution of the busulfan injection into a high performance liquid chromatograph to separate and detect related substances in the busulfan injection by using an electric fog detector; a mobile phase A and a mobile phase B are adopted as eluents for gradient elution, the mobile phase A is a formic acid aqueous solution with the volume concentration of 0.02%-0.08%, the mobile phase B is acetonitrile, linear gradient elution is adopted when the elution time is controlled to range from 0 min to 10 min, the volume percent of the mobile phase A is reduced to 15% from 98%, and meanwhile the volume percent of the mobile phase B is increased to 85% from 2%. The method disclosed by the invention can be used for separating and detecting a main component busulfan and impurities methanesulfonic acid and RRT0.91, and has good separation degree, accuracy and sensitivity.

The application relates to a coating equipment and a linear gradient filter film thickness uniformity correction method, and solves the problem that the film thickness uniformity of a linear gradient filter prepared by using an existing deposition method of electron beam evaporation cannot be corrected. A revolution correction plate is arranged below a workpiece disc, the revolution correction plate rotates with the workpiece disc around the center of a rotating disc, the workpiece disc has self-rotation motion, the film thickness distribution of Ta2O5 and SiO2 is corrected to the middle linearity by the revolution correction plate, at this time, the film thickness distribution of Ta2O5 and SiO2 after being corrected by the revolution correction plate has not reached the final target, and the difference from the final target is respectively corrected for the second time by a first fixed correction plate and a second fixed correction plate, so that the film thickness distribution of Ta2O5 and SiO2 finally reaches the final target, and the film thickness distribution of Ta2O5 and SiO2 is corrected to the film thickness distribution state required by the linear gradient filter by the combination of the revolution correction plate and the fixed correction plate.

The present disclosure is directed to methods of purifying a dulaglutide composition. For example, the methods comprise loading the dulaglutide composition in-line with a buffer B solution onto a hydrophobic interaction chromatography (HIC) column in a downflow direction, washing the HIC column with a buffer mixture of a buffer A solution and the buffer B solution in the downflow direction, and eluting dulaglutide from the HIC column. A linear gradient of a percentage of the buffer A and buffer B solutions is used for eluting dulaglutide, which is then followed by an isocratic hold based on a UV absorbance reading of an eluate. The methods further comprise maintaining the isocratic hold until a front side cut is made, and then dropping the buffer B solution for dulaglutide to elute from the HIC column.

The invention relates to a separation and quality control detection method for related substances in deoxycholic acid, which adopts a high performance liquid chromatography method, a chromatographic column takes octadecyl bonded silica gel as a filler, 0.010 mol / L dipotassium phosphate solution as a mobile phase A and acetonitrile as a mobile phase B, linear gradient elution is carried out, and the related substances are subjected to separation and quality control detection. Wherein the related substance is pyridine. The quality control detection method for related substances in deoxycholic acid provided by the invention comprises the following steps: preparing a pyridine reference substance solution with a certain concentration, determining the peak area of pyridine in a reference substance and a test solution by using a high performance liquid chromatography, and calculating the content of pyridine by using an external standard method. Therefore, the content of pyridine in deoxycholic acid can be accurately and quantitatively determined.

The invention belongs to the technical field of chemical analysis, and particularly relates to a method for separating and determining related substances in a rupatadine fumarate intermediate Z2. The related substances comprise any one or more of an impurity SM1, an impurity Z1, an impurity Z2a and an enantiomer thereof, an impurity Z2b and an enantiomer thereof, and an impurity Z2e and an enantiomer thereof. According to the self-built high performance liquid chromatography, octadecyl silane bonded silica gel is adopted as a chromatographic column filler, a phosphate solution is adopted as a mobile phase A, acetonitrile is adopted as a mobile phase B, and related substances in the rupatadine fumarate intermediate Z2 are separated through linear gradient elution; then detecting in a detector to obtain a chromatogram; and calculating the content of each impurity by adopting a correction factor-added principal component self-contrast method. The analysis method has the characteristics of short separation time, high sensitivity, strong specificity, good reproducibility, strong durability and simplicity and feasibility in operation.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating, detecting and determining an initial raw material SM3 and impurities thereof of ibrutinib. The impurities comprise one or more of propionyl chloride, 3-chloropropionyl chloride and benzoyl chloride. A mobile phase is a phosphate buffer solution as a mobile phase A, acetonitrile is a mobile phase B, a chromatographic column adopts octadecylsilane chemically bonded silica as a filler, and linear gradient elution of high performance liquid chromatography is carried out after pre-column derivatization. And then, according to a chromatogram, an external standard method is adopted to calculate the impurities according to a peak area. The method has the characteristics of good separation degree, good durability, high sensitivity and good reproducibility.