1034 results about "Gradient elution" patented technology

The invention discloses a liquid chromatography-tandem mass spectrometry detection method and system, and the method comprises the steps: designing a multi-dimensional gradient elution program according to the physicochemical properties of a target compound, and obtaining a chromatographic separation spectrogram; performing efficient ionization on the target compound according to the chromatographic separation spectrogram to obtain an ionization signal; according to the ionization signal, fragmenting the target ions, and obtaining a fragment ion spectrogram through fragment ion screening; according to the fragment ion spectrogram, a multivariable data analysis algorithm based on machine learning is adopted, a standard curve of a target compound and an interferent database are combined, quantitative analysis is carried out, and a quantitative result is generated through a dynamic interference correction technology in combination with principal component analysis and a partial least square method. By utilizing the embodiment of the invention, the sensitivity, the accuracy and the real-time performance of detection can be improved through multi-dimensional gradient elution, dynamic ionization and fragmentation parameter optimization in combination with an analysis means of machine learning.

The invention discloses a liquid chromatography-mass spectrometry data peak shape recognition processing method and related equipment, and relates to the field of data processing. The method comprises the following steps: acquiring liquid chromatography-mass spectrometry data; extracting morphological characteristic data of a chromatographic peak based on the extracted ion current chromatogram time sequence; calculating and extracting a signal complexity index of the ion current chromatogram time sequence; adjusting peak shape identification parameters according to the signal complexity index, wherein the peak shape identification parameters comprise a noise threshold value and a peak width range; distinguishing the chromatographic peak into a normal peak or an abnormal peak by using the adjusted peak shape identification parameter; searching a liquid phase method optimization scheme matched with the morphological characteristic data of the abnormal peak in a preset optimization database, wherein the liquid phase method optimization scheme comprises gradient elution time adjustment, mobile phase proportion optimization or chromatographic column replacement suggestion; and sending the liquid phase method optimization scheme to a user. According to the invention, various abnormal peak shapes can be automatically and accurately identified, and the reliability and accuracy of identification are guaranteed.

The invention provides a content detection method for a salvia miltiorrhiza medicinal material, a salvia miltiorrhiza clear paste and a musk heart-dredging dropping pill. According to the method, a high performance liquid chromatography method is adopted, octadecylsilane chemically bonded silica is used as a chromatographic column filler, acetonitrile is used as a mobile phase A, 0.02%-0.1% trifluoroacetic acid is used as a mobile phase B, gradient elution is carried out, and rosmarinic acid and salvianolic acid B in the salvia miltiorrhiza medicinal material are synchronously and quantitatively detected. And synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid and salvianolic acid B in the salvia miltiorrhiza clear paste, and synchronously and quantitatively detecting tanshinol, protocatechuic aldehyde, caffeic acid, salvianolic acid E, rosmarinic acid, alkannic acid, salvianolic acid B, arenobufagin and bufalin in the musk Tongxin dropping pill. The method is used for monitoring the content of specific components, can also judge the transfer rate in the medicine production process, and facilitates traceability in the production link. In addition, the method is relatively low in equipment requirement and suitable for industrial popularization.

The invention belongs to the technical field of traditional Chinese medicine detection, and discloses a detection method for a characteristic spectrum of Uighur medicine Kspecific heat extracting tablets and application of the detection method. The detection method provided by the invention comprises the following steps: preparing a test sample solution by taking a 75% methanol solution as a solvent, and determining the test sample solutions prepared from different batches of test samples by adopting ultra-high performance liquid chromatography to obtain a characteristic spectrum; the chromatographic conditions of the ultra-high performance liquid chromatography are as follows: a chromatographic column is a C18 chromatographic column, a mobile phase A is acetonitrile, a mobile phase B is a 0.1 vol% phosphoric acid solution, and the flow velocity is 0.25-0.35 mL / min; the detection wavelength is 0 to 18 minutes, and the wavelength is 327 nm; the time is 18 to 28.5 min, and the wavelength is 254 nm; when the time is 28.5 to 37.6 minutes, the wavelength is 242 nm; after 37.6 to 70 minutes, the wavelength is 210 nm; the sample size is 1 microliter, the column temperature is 20-40 DEG C, and gradient elution is carried out. The invention provides a more scientific identification and quality control method for the Kespecific heat tablets.

The invention discloses a construction method and an identification method of characteristic chromatograms of a senecio scandens medicinal material as well as decoction pieces, standard decoction and formula granules thereof, and relates to the technical field of traditional Chinese medicine identification. The construction method of the specific chromatogram comprises the following steps: extracting a to-be-detected sample with methanol to obtain a test solution; the method comprises the following steps: dissolving 5-caffeoylquinic acid, chlorogenic acid, caffeic acid, 4-caffeoylquinic acid, rutin, hyperoside, isoquercitrin and 4, 5-dicaffeoylquinic acid with methanol to obtain a reference solution; and a liquid chromatograph is adopted for determination. A chromatographic column of the liquid chromatograph takes phenyl-methyl polysiloxane as a stationary phase, acetonitrile as a mobile phase A and 0.05 vol%-0.3 vol% formic acid aqueous solution as a mobile phase B for gradient elution. The information of the characteristic chromatogram constructed by the method is rich, and the quality of the senecio scandens medicinal material, decoction pieces, standard decoction and formula granules can be quickly and comprehensively reflected.

The invention relates to the field of pharmaceutical analytical chemistry, in particular to a method for determining tandospirone and salt intermediates thereof, high performance liquid chromatography is adopted, and chromatographic conditions include that a chromatographic column with octadecylsilane chemically bonded silica as a filler is adopted, and gradient elution is performed by a mobile phase A and a mobile phase B; wherein the mobile phase A consists of a first water phase and acetonitrile; the mobile phase B is composed of a second water phase and acetonitrile; the first water phase is a water solution containing monopotassium phosphate and sodium hexanesulfonate, and the pH value of the first water phase is 3.0-3.8; the second water phase is an aqueous solution containing monopotassium phosphate and sodium hexanesulfonate, and the pH value of the second water phase is 1.8-2.6. The testing method disclosed by the invention has good specificity, accuracy and repeatability, and can be used for monitoring the quality of the tandospirone raw material medicine.

The invention discloses a construction method of a gout compound decoction fingerprint as well as the fingerprint and application thereof, and belongs to the technical field of analysis and detection. The construction method of the fingerprint spectrum comprises the following steps: taking a test solution prepared from the gout compound decoction; the test solution is subjected to HPLC-SPD detection, so that the fingerprint spectrum of the gout compound decoction is obtained, and the HPLC detection conditions are that a C18 chromatographic column is used, a C18 chromatographic column is used, a C18 chromatographic column is used, a C18 chromatographic column is used, and a C18 chromatographic column is used for detecting the fingerprint spectrum of the gout compound decoction. An aqueous solution containing 0.1%-0.2% of phosphoric acid is used as a mobile phase A, and acetonitrile is used as a mobile phase B for gradient elution; the flow velocity is 0.8-1 mL / min, the column temperature is 25 DEG C, the sample injection volume is 5-10 [mu] L, and a diode array detector is 190-400 nm full-wave band scanning. The chemical components in the gout compound decoction are comprehensively and systematically analyzed, and a basis is provided for quality control and in-depth study of a pharmacodynamic material basis.

The invention relates to the technical field of medicine analysis and traditional Chinese medicine detection, in particular to a construction method, a detection method and application of a specific chromatogram of a szechuan lovage rhizome perfume extract. Wherein the conditions of the liquid chromatographic analysis are as follows: gradient elution is carried out by adopting an aqueous solution of a mobile phase A acetonitrile and a mobile phase B phosphoric acid for 0-5 minutes, the volume percent of the mobile phase A is maintained to be 4% and 5-12 minutes, the volume percent of the mobile phase A is increased to 16% from 4% and 12-19 minutes, the volume percent of the mobile phase A is maintained to be 16% and 19-29 minutes, the volume percent of the mobile phase A is increased to 40% from 16% and 29-31 minutes, and the volume percent of the mobile phase A is maintained to be 4% and 12-19 minutes. The volume percentage of the mobile phase A is increased to 55% from 40%, 31-37 min, and the volume percentage of the mobile phase A is maintained to be 55%. The method can be used for quantitatively determining the water-soluble components of the szechuan lovage rhizome perfume extract, and can also be used for identifying the true and false.

The invention relates to a content determination method of a traditional Chinese medicine composition fingered citron drink. The traditional Chinese medicine composition is prepared from the following medicinal raw materials: fingered citron, orange peel, malt, liquorice, Chinese date, purple perilla, citron, almond and donkey-hide gelatin. The content determination method comprises the following steps: preparing a reference solution and a test solution; detecting the reference substance solution and the test solution by high performance liquid chromatography; a mobile phase adopted by the high performance liquid chromatography is an acetonitrile and formic acid aqueous solution, and the elution mode is gradient elution. According to the content determination method, the content of various components can be simply, conveniently and rapidly determined, and richer chemical information and more comprehensive basis are provided for quality evaluation of the components.

The invention discloses a method for determining pesticides in water by liquid chromatography and tandem mass spectrometry, which comprises the following steps: acquiring retention time data of different pesticide compounds in a liquid chromatography system, recording retention behavior characteristics of each pesticide compound under optimized chromatographic conditions by adjusting the composition proportion of a mobile phase and a gradient elution program, and determining the retention behavior characteristics of each pesticide compound under optimized chromatographic conditions. Obtaining a standardized retention time spectrum library data set; establishing a quantitative relation model between molecular structure parameters and chromatographic retention time by adopting a multiple linear regression algorithm through key parameters such as molecular weight, polar surface area and lipid-water partition coefficient in the molecular structure parameter matrix, and obtaining a structure-retention correlation prediction model; and constructing a classification prediction model between molecular structure parameters and environmental durability by adopting a support vector machine algorithm through activity index data in the biological activity prediction result, and determining the environmental durability grade of the pesticide compound according to molecular stability parameters and degradation half-life characteristic values.

The invention discloses a system and a method for rapidly measuring trace F <-> and Cl <-> in water based on chromatographic gradient elution. The system comprises a water storage tank, an anion trapper, an eluent generator, a six-way sample injection valve, a guard column, an analytical column, a suppressor, a conductivity detector and a chromatographic workstation, an outlet of the water storage tank is communicated with an inlet of the leacheate generator through the anion trapper, an outlet of the leacheate generator is communicated with an inlet of the guard column through the six-way sample injection valve, and an outlet of the guard column is communicated with the conductivity detector through the analytical column and the suppressor. The chromatographic work station is connected with the leacheate generator, the six-way sample injection valve, the suppressor and the conductivity detector, and the system and the method can realize rapid measurement of strongly corrosive anions F <-> and Cl <-> in water and rapid elution of other anions, so that the measurement time of each sample is reduced by at least 40% or more.

The invention provides a traditional Chinese medicine formula granule spectrum similarity evaluation system, and relates to the technical field of traditional Chinese medicine, and the system comprises: a spectrum acquisition module, which is used for separating active components with similar polarity in a compound salvia miltiorrhiza formula granule test solution by gradient elution based on chromatographic conditions to obtain a characteristic spectrum; and the analysis processing module is used for carrying out analysis processing on overlapped chromatographic peaks in the characteristic spectrum, distinguishing characteristic signals corresponding to main active components and trace components, and realizing separation and identification of characteristic peaks of different components in the mixture so as to obtain a characteristic peak analysis result. According to the method, the standard characteristic chromatogram database is constructed through gradient elution and deconvolution processing, and the accuracy and standardization of quality evaluation of the traditional Chinese medicine formula granules are improved.

The invention discloses a method for rapidly determining the content of breast milk oligosaccharide in dairy products, which comprises the following steps: sampling and pretreating different types of dairy products according to sample states, carrying out ultrasonic extraction, refrigerated centrifugal degreasing and centrifugal ultrafiltration protein purification on the obtained sample, and reducing the purified sample solution by using sodium borohydride to obtain a sample solution to be detected; reducing the breast milk oligosaccharide standard substance by sodium borohydride to obtain a standard solution to be detected; determining the standard substance solution and the to-be-detected sample solution by adopting ultra-high performance liquid chromatography-tandem mass spectrometry, establishing a standard curve, and carrying out quantitative analysis on the to-be-detected sample solution; the chromatographic conditions are as follows: an ACQUITY UPLC BEH Amide hydrophilic interaction chromatographic column is adopted; the mobile phase A is 20 mmol / L ammonium formate; the mobile phase B is acetonitrile; and gradient elution.

The invention belongs to the technical field of detection methods, and particularly relates to a liquid chromatography detection method for an idedecalciferol intermediate and impurities thereof. According to the liquid chromatography detection method for the eldecalciferol intermediate and the impurities thereof, a liquid chromatography method is combined with an electrospray detector for detection; chromatographic conditions are as follows: an amylose-tri (3-chlorphenyl carbamate) covalently bonded silica gel chromatographic column is adopted; and carrying out gradient elution by taking water as a mobile phase A and acetonitrile as a mobile phase B. The method for detecting the eldecalciferol intermediate and the impurities of the eldecalciferol intermediate is good in specificity, high in sensitivity and accuracy, good in repeatability and stability and high in analysis speed, the content of the eldecalciferol intermediate and the impurities of the eldecalciferol intermediate can be rapidly and accurately detected, and the blank of detection of the eldecalciferol intermediate and the impurities of the eldecalciferol intermediate in the prior art is filled.

The invention discloses a CAD detection method for phosphoric acid and phosphorous acid in an alendronate sodium oral solution, and belongs to the technical field of pharmaceutical analysis. The method comprises the following steps: preparing a reference stock solution and a test solution; then setting high performance liquid chromatography detection conditions; a Shodex VN-504D chromatographic column is adopted, a CAD detector is adopted as a detector, a mixed solution of a mobile phase A and a mobile phase B is adopted as a mobile phase, the mobile phase A is ammonium formate, the mobile phase B is an acetonitrile solution, and gradient elution is performed by adopting the mobile phase; and respectively measuring the reference stock solution and the test solution, injecting into a liquid chromatograph, and recording a chromatogram. A CAD detector is adopted, the detection sensitivity is obviously improved, the quantitative concentration can reach 0.24 mu g / mL, and the detection concentration can reach 0.10 mu g / mL. The method is high in specificity, high in sensitivity, good in durability, rapid, simple, effective and reliable.

The invention relates to the field of water quality monitoring of a secondary loop of a nuclear power plant, in particular to a synchronous detection system and method for ammonia and hydrazine. The method comprises the following steps: removing impurities in a sample by utilizing filtration and reverse chromatography; the sample is quantified to 240-260 [mu] L; carrying out gradient elution on the sample by using a methanesulfonic acid solution as an eluent; wherein in the first stage, the concentration of a methanesulfonic acid solution is controlled to be 13-18 mmol / L, and a sample is washed; in the second stage, the concentration of the methanesulfonic acid solution is controlled to be 55-70 mmol / L, and the sample is Drawing a low-concentration curve based on the 10-500 [mu] g / L standard solution, and drawing a high-concentration curve based on the 500-3000 [mu] g / L standard solution; and measuring the ionic conductivity values of NH4 < + > and N2H5 < + >, automatically selecting a corresponding concentration curve according to the peak area of the ionic conductivity values, and calculating the concentration of ammonia and hydrazine. According to the invention, the synchronous detection of ammonia and hydrazine concentration is realized, the analysis process is simplified, the use of toxic and harmful substance phenol and the generation of toxic and harmful waste liquid of yellow azo compound are solved, the measurement accuracy is improved, and the relative measurement error can be controlled within + / -2.0%.

The invention relates to a method for detecting six second-line antituberculous drugs by high performance liquid chromatography. The method comprises the following steps: providing an internal standard stock solution and a standard stock solution of six second-line antituberculosis drugs; preparing an internal standard working solution and a standard curve working solution by utilizing the diluent; preparing a solution of a product to be detected by using the Tianlongitudinal sample extraction liquid TZ-002; a liquid chromatograph is used for detection, and the conditions are as follows: a mobile phase A is a Tianlongitudinal sample releasing agent TZ-D004; a mobile phase B is acetonitrile; a mobile phase C is water; and gradient elution. According to the method, the plasma concentration of the second-line antituberculous drug taken by a tuberculosis patient is measured by applying the reversed-phase high-performance liquid chromatography, the cost is relatively low, the analysis time is short, the sensitivity is high, and the accuracy is high. The kit can be used for simultaneously detecting the blood concentration of six second-line antituberculosis drugs such as isopropylthioamide, levofloxacin, linezolid, moxifloxacin, deramanib and bedaquiline in human serum, and is expected to provide a more reliable basis for clinicians to adjust the dosage of the antituberculosis drugs.

The invention belongs to the technical field of agricultural chemistry, and particularly relates to a naphthoquinone compound with tobacco black shank resisting activity as well as a preparation method and application of the naphthoquinone compound. The naphthoquinone compound is prepared by the following steps: by taking honeysuckle branches as raw materials, extracting with high-concentration methanol, high-concentration acetone / water or high-concentration ethanol / water, merging extracting solutions, filtering, and concentrating under reduced pressure to obtain extract; packing the extract by using a silica gel dry method and carrying out silica gel column chromatography; carrying out gradient elution by using a chloroform-acetone solution; and further separating and purifying the 7: 3 part of the eluent by high performance liquid chromatography to obtain the required naphthoquinone compound. The invention further discloses application of the compound, and activity tests show that the compound has a good inhibiting effect on tobacco black shank. The compound disclosed by the invention is novel in structure, has relatively good black shank resisting activity, can be used as a lead compound for resisting tobacco black shank, and is used for research and development of biological pesticides for preventing and treating tobacco black shank.

The invention provides a method for analyzing and identifying chemical components of a calculus-eliminating prescription, which comprises the following steps: S1, preparing a test solution: performing ultrasonic treatment on a calculus-eliminating prescription extract by using methanol, centrifuging, taking supernate, diluting, filtering, and taking subsequent filtrate to obtain the test solution; s2, analyzing the test sample solution by adopting UHPLC-QE-MS (Ultra High Performance Liquid Chromatography-Quantitative Enhanced-Mass Spectrometry), wherein the detection conditions of the UHPLC-QE-MS are as follows: a chromatographic column is an octadecylsilane chemically bonded silica chromatographic column; the column temperature is 20-40 DEG C; the flow rate is 0.1 to 0.5 ml / min; the mobile phase A is 0.03-0.20% v / v formic acid aqueous solution, the mobile phase B is acetonitrile, gradient elution is carried out, and the gradient elution procedure is 0-1 min, 5% B-> 5% B; in 1-14 minutes, 5% B is changed into 60% B; and after 14-15 minutes, 60% B is converted into 95% B. The detection method disclosed by the invention can identify 68 compounds in the calculus eliminating sample at one time, and is rapid, simple, convenient, high in sensitivity and good in specificity.

The invention relates to the field of quality detection of traditional Chinese medicine preparations and specifically provides a method for constructing a characteristic spectrum of nardostachys radix and a preparation thereof and a quality detection method. In the characteristic spectrum construction method, chromatographic conditions include: using acetonitrile and an aqueous solution containing formic acid as mobile phases for gradient elution, the gradient elution program includes: 0-5 min-40 min-50 min, and the volume percentage of acetonitrile in the mobile phase is: 10%-10%-35%-50%. Under the specific elution program, 9 common characteristic peaks are obtained, and good separation of the common characteristic peaks is achieved. The obtained characteristic spectrum has a stable baseline, good characteristic peak shape, good separation effect, and strong characteristic component specificity. The method provides a basis for quality detection and control of nardostachys radix and a preparation thereof, achieves characterization of the overall components of nardostachys radix and a preparation thereof, and has stable reproducibility.

The invention provides a method for quantitatively detecting a nitrosamine impurity in a macassavir raw material medicine and an intermediate TG9, and relates to the technical field of medicine detection, the method comprises the step of detecting the nitrosamine impurity in the macassavir raw material medicine or the intermediate TG9 sample by adopting a high performance liquid chromatography and mass spectrometry combined method, the mobile phase A is a formic acid solution, and the mobile phase B is a formic acid methanol solution; gradients, such as segmented gradients of the raw material medicines, are respectively designed for the intermediate and the raw material medicines through a dynamic gradient elution program, so that TG801, TG901 and TG1001 realize baseline separation; an acidic mobile phase is adopted, formic acid acetonitrile is added into the solution, protonation competition of nitrosamine impurities is inhibited, the ionization efficiency and stability are improved, the sensitivity is high, and the LOQ of the method is 0.033 ng / g. The technical problem that in the prior art, a method for quantitatively detecting three nitrosamine impurities in a macassavir raw material medicine and an intermediate TG9 does not exist is solved.

The invention provides a preparation method of an artemisia capillaris decoction reference sample. The invention also provides a construction method of the high performance liquid characteristic chromatogram of the artemisia capillaris decoction reference sample. According to the invention, the characteristic chromatogram of the artemisia capillaris decoction is constructed by adopting the high performance liquid chromatography for the first time, the blank of quality control of the artemisia capillaris decoction is filled through the method of the characteristic chromatogram, meanwhile, the quality condition of the prescription is comprehensively reflected, the quality control of the artemisia capillaris decoction is more perfect, and a means is added for the quality standard aspect of the artemisia capillaris decoction. According to the method disclosed by the invention, gradient elution is adopted for determination by adopting a high-performance liquid chromatography, and the method has the advantages of simplicity in operation, good separation degree, high precision, good repeatability, good stability and the like. Under specific detection conditions, the identification of the artemisia capillaris decoction characteristic spectrum method can be realized by taking a chlorogenic acid chromatographic peak as a reference substance S peak.

An UPLC can offer the advantages of improved resolution, shorter analysis time, reduced solvent consumption, and easy connectivity to a mass spectrometer. One of our unique approaches is to use four small linear pumps to achieve gradient elution. We use four binary pumps to achieve continuous gradient elution. We designed an on-line degassing to greatly reduce interference from gas bubbles, thereby maintaining stable pressure. The range of flow speed is controlled from 300 nl / min to 100 ul / min. This portable UPLC can withstand pressures of 15,000 psi or higher. Its size is 30 cm×30 cm×30 cm, and it weighs less than 20 kg. This portable UPLC is equipped with an LED detector, which reduces both cost and system size and has higher sensitivity than a spectrophotometer. We also have the option to easily switch to a conventional detector with a discharge light source and a grating spectrophotometer.

The invention discloses an analysis method for determining multiple components of white spirit by high performance liquid chromatography-tandem mass spectrometry, and relates to the technical field of white spirit analysis and detection, and the analysis method comprises the following steps: firstly, preparing an ethyl carbamate precursor substance standard stock solution and a mixed standard intermediate solution, and diluting the mixed standard intermediate solution step by step to obtain a mixed standard working solution; then determining chromatographic and mass spectrometry conditions, wherein BEH Ami chromatographic column is adopted as the chromatographic condition, and 0.1% formic acid water-acetonitrile is adopted as a mobile phase for gradient elution; a mass spectrum condition adopts a multi-reaction monitoring mode under an electrospray positive ion mode; drawing a quantitative calibration curve; finally, preparing a to-be-detected sample for content determination. According to the analysis method for determining the multiple components of the Baijiu through the high performance liquid chromatography-tandem mass spectrometry, through chromatographic condition optimization and mass spectrometry parameter innovation, the detection efficiency is improved, peak area data of urea, citrulline and arginine can be synchronously obtained through single sample injection, the analysis time is short, and quantification is accurate.

The invention discloses a method for determining related substances in a fluralamoxidectin drop, the related substances comprise an impurity A, an impurity B, an impurity C, an impurity D, an impurity G and an impurity J. The method is carried out by adopting a high performance liquid chromatography method, and the chromatographic conditions are as follows: an ammonium dihydrogen phosphate buffer solution with the pH value of 4.5-5.2 is taken as a mobile phase A, the mobile phase B is taken as a mobile phase C, and the mobile phase C is taken as a mobile phase D; acetonitrile is used as a mobile phase B for gradient elution, and the concentration of the ammonium dihydrogen phosphate buffer solution is 0.02 mol / L-0. 1 mol / L; the flow velocity is 0.7 mL / min to 1.3 mL / min; the column temperature is 40-50 DEG C; and the detection wavelength is 242 nm. According to the method, related substances in the fluralamoxidectin drops can be simultaneously determined under the same chromatographic condition, simultaneous detection and separation of various impurities are realized, the detection time is shortened, the method can be used for quality research and quality control of fluralamoxidectin drop products, and the drug safety risk is reduced.

The invention discloses a method for detecting related substances in imaric acid dihydrochloride by HPLC (High Performance Liquid Chromatography), and belongs to the technical field of chemical engineering and pharmacy, the related substances in the imaric acid dihydrochloride are detected by high performance liquid chromatography, a phosphate buffer solution (0.05 mol / L of monopotassium phosphate solution, and pH adjusted to 2.5 by phosphoric acid) is used as a mobile phase A, acetonitrile is used as a mobile phase B, gradient elution is carried out, the flow rate is 1.0 ml / min, the detection wavelength is 250nm, and the detection wavelength is 250nm. The column temperature is 40 DEG C, and the detection wavelength is 235nm; the method can be used for effectively separating and quantitatively detecting imatamide, demethylated imaric acid dihydrochloride, ortho-imaric acid, meta-imaric acid, p-hydroxymethyl benzamide, an intermediate B, p-hydroxymethyl benzoic acid, an imaric acid dimer, p-cyanobenzyl alcohol, p-chloromethyl benzamide, p-toluic acid and p-chloromethyl benzoic acid in the imaric acid dihydrochloride. The method disclosed by the invention is simple and convenient to operate, strong in specificity, high in sensitivity and accuracy, good in linearity and capable of effectively controlling the quality of a p-imaric acid dihydrochloride product.

The invention discloses a method for determining chemical components in a medicine for treating vitiligo and a method for establishing a fingerprint spectrum. Comprising the following steps: S1, preparing a to-be-detected solution and a reference substance solution: grinding Bailing tablets, dissolving the Bailing tablets in a solvent, and extracting to prepare the to-be-detected solution; dissolving a paeoniflorin reference substance in a solvent to prepare a reference substance solution; wherein the extraction solvent is a methanol-water mixed solution; s2, respectively obtaining chromatograms of the to-be-detected solution and the reference substance solution under the same detection conditions by adopting ultra-high performance liquid chromatography, and carrying out qualitative analysis and / or quantitative analysis on chemical components in the chromatograms of the to-be-detected solution; wherein the detection conditions are as follows: the wavelength of a detector is 201 + / -2nm; the elution conditions are as follows: acetonitrile is used as a phase A, water is used as a phase B, and elution is performed through a gradient elution procedure. According to the method, the chemical components in the medicine for treating the leucoderma can be accurately determined, so that the establishment of the fingerprint spectrum database of the medicine for treating the leucoderma can be better realized.

The invention relates to the technical field of medicine research of Cichorium glandulosum, in particular to a Cichorium glandulosum extract, a compound separated from the Cichorium glandulosum extract and an extraction method and application thereof.The Cichorium glandulosum extract comprises Cichorium glandulosum lactone A, Cichorium glandulosum lactone B, Cichorium glandulosum picroside and Cichorium glandulosum. And dissolving the crude extract with a solvent, separating, carrying out gradient elution, carrying out gradient elution on the obtained eluate through ODS column chromatography, and carrying out gradient elution on the obtained eluate through high performance liquid chromatography separation to obtain the cichorium glandulosum extract. According to the invention, the cichorium glandulosum extract and the compound separated from the cichorium glandulosum extract are extracted by taking the whole herb of cichorium glandulosum as a raw material for the first time, and the inhibition effect of the compounds, namely cichorium glandulosum lactone A, cichorium glandulosum lactone B, cichorium glandulosum picroside and cichorium glandulosum, separated from the cichorium glandulosum extract on RAW264.7 cells is disclosed for the first time. Therefore, the compound can be applied to preparation of anti-inflammation or / and inflammation treatment medicines.

The utility model relates to a two-dimensional liquid phase system which comprises a hydrophilic interaction chromatographic column, a reversed-phase chromatographic column, a detector, an automatic sample injector, a first pump assembly, a second pump assembly, a sample temporary storage unit and a switching valve, the first pump assembly is communicated with the hydrophilic interaction chromatographic column and is used for pushing a sample loading solution and carrying out gradient elution on the hydrophilic interaction chromatographic column; the second pump assembly is communicated with the reversed-phase chromatographic column and is used for carrying out gradient elution on the reversed-phase chromatographic column; wherein the switching valve comprises a first double-four-way valve and a second double-four-way valve which are communicated with each other; the switching valve has at least two connection states through position switching: state 1: the switching valve communicates a liquid inlet of the detector with a liquid outlet of the hydrophilic interaction chromatographic column; and state 2: the switching valve communicates the liquid inlet of the detector with the liquid outlet of the reversed-phase chromatographic column, and communicates the first port of the sample temporary storage unit with the liquid inlet of the hydrophilic interaction chromatographic column. The system can realize one-time analysis of a multi-component target object with relatively large polarity difference.

The invention provides a method for detecting related substances of dihydroxypropyl arginine hydrochloride, which is characterized in that a high performance liquid chromatography method is adopted, a chromatographic column is a reversed-phase, cation exchange and hydrophilic interaction mixed type chromatographic column, and a mobile phase is used for gradient elution. The detection method provided by the invention can effectively separate and detect main components, starting materials and process impurities in dihydroxypropyl arginine hydrochloride, has the advantages of high sensitivity, good degree of separation, simple operation, fast appearance time, short detection time, good method reproducibility and stability, and strong specificity, meets the requirements of product quality control, and is suitable for industrial production. The method has the advantages of high sensitivity and high precision, is favorable for ensuring the safety and effectiveness of the product, reduces the production cost, and has remarkable technical advantages and application value.