62 results about "Hplc method" patented technology

The invention provides an online quality detection method of a nerve-soothing and brain-nourishing liquid based on multispectral fusion, and aims at solving the bottleneck problems of long offline time consumption, weak multi-index detection capability, poor dynamic adaptability and the like in the traditional detection technology, and realizing intelligent quality control of the whole process of the production technology. The device integrates an ultraviolet-visible spectrum module, a near-infrared spectrum module and a fluorescence spectrum module, constructs a multi-scale residual convolutional network to extract near-infrared spectrum characteristics, analyzes a fluorescence excitation-emission matrix through bidirectional LSTM, and cooperates with dynamic baseline correction of an ultraviolet spectrum, so that the icariin content detection precision is improved by 40% compared with that of a traditional HPLC method, the heavy metal residue detection lower limit reaches 0.05 ppm, and the detection accuracy is greatly improved. And an innovative solution is provided for intelligent production of traditional Chinese medicine preparations.

The invention relates to the technical field of high performance liquid chromatography detection, in particular to a liquid chromatography determination method and equipment for the content of m-tert-butylphenol, and the method comprises the following steps: determining a to-be-determined mixed solution of the prepared m-tert-butylphenol by using high performance liquid chromatography to obtain chromatographic data; the method comprises the following steps: preparing chromatographic data of standard control group solution samples of m-tert-butylphenol under different concentrations under two preset different wavelengths, and obtaining a nonlinear fitting relationship between the concentrations of m-tert-butylphenol and chromatographic peak areas; analyzing the chromatographic data deviation of the to-be-measured mixed solution, and obtaining the chromatographic peak area of the to-be-measured mixed solution after correction of the intermediate tert-butylphenol; and acquiring the concentration of the intermediate tert-butylphenol in the mixed solution to be measured corresponding to the corrected chromatographic peak area by utilizing a nonlinear fitting relationship. The invention aims to improve the measurement accuracy of the prepared m-tert-butylphenol.

This invention proposes an online quality detection method for An Shen Bu Nao Liquid based on multispectral fusion. Addressing the bottlenecks of traditional detection techniques, such as long offline processing time, weak multi-index detection capabilities, and poor dynamic adaptability, this method achieves intelligent quality control throughout the entire production process. The device integrates ultraviolet-visible spectroscopy, near-infrared spectroscopy, and fluorescence spectroscopy modules. It constructs a multi-scale residual convolutional network to extract ultraviolet-visible spectral features, uses a two-way LSTM to analyze the fluorescence excitation-emission matrix, and employs dynamic baseline correction of the ultraviolet spectrum. This improves the detection accuracy of icariin content by 40% compared to traditional HPLC methods, and achieves a heavy metal residue detection limit of 0.05 ppm, providing an innovative solution for the intelligent production of traditional Chinese medicine preparations.

The present invention belongs to the field of pharmaceutical chemical technology, and specifically relates to a method for analyzing chiral impurities of L-carnitine key intermediate L-carnitine. The method first uses (S)-2-(6-methoxy-2-naphthyl) propionyl chloride as a derivatization reagent to derive L-carnitine, and then uses high performance liquid chromatography to separate and detect the derivatized L-carnitine. The present invention proposes for the first time to use HPLC to determine the chiral purity of L-carnitine, which has simple steps and mild conditions, and is conducive to industrial promotion and application; the method of the present invention has strong specificity, high sensitivity, and good durability, and can be used for the accurate determination of the chiral purity of L-carnitine.

The invention discloses a characteristic chromatogram construction method of leech medicinal materials and related adulterants of the leech medicinal materials. The construction method comprises the following steps: establishing characteristic spectrums of the leech medicinal material and the related counterfeit species thereof through a high performance liquid chromatography, wherein the characteristic spectrums comprise the steps of respectively extracting and preparing test sample solutions from the leech medicinal material and the related counterfeit species thereof; the method comprises the following steps: preparing a test solution, preparing a reference solution, and respectively detecting the test solution and the reference solution by high performance liquid chromatography to obtain a corresponding characteristic chromatogram, so that the leech medicinal material and the related adulterants thereof can be quickly distinguished. The leech reference medicinal material is selected from leeches or leeches in the leech family; the leech medicinal material related adulterants are selected from poecilobdella manillensis, poecilobdella manillensis or poecilobdella japonica. The method is simple and convenient, has the advantages of being simple to operate, good in separation degree, high in precision, good in repeatability, good in stability and the like, and can rapidly and accurately distinguish the leeches from the leeches and the related adulterants of the leeches and the leeches by utilizing HPLC (High Performance Liquid Chromatography).

The invention discloses a method for separating and determining a dotenorad key intermediate and related compounds thereof by HPLC (High Performance Liquid Chromatography), which belongs to the field of analytical chemistry, and is used for separating and detecting the dotenorad key intermediate (3, 5-dichloro-4-methoxyphenyl) (1, 1-benzo [d] thiazole-3 (2H)-yl) ketone and related compounds A-F thereof by liquid chromatography. A chromatographic column with phenylsilane bonded silica gel as a filler is adopted, a phosphoric acid aqueous solution is used as a mobile phase A, acetonitrile is used as a mobile phase B, gradient elution is carried out, detection and analysis are carried out, and the content of each compound is calculated. According to the present invention, the dotenorad key intermediate and the related impurity compounds thereof can be effectively separated, and the method has advantages of high sensitivity, high separation degree, good repeatability, good durability, simple operation and stable and reliable result, and has important significance on the realization of the dotenorad drug quality control.

The invention discloses a prismatomeria tetrandra fingerprint spectrum construction method and application thereof. Belongs to the technical field of medicine. The construction method comprises the following steps: taking scopoletin, coumarin, methyl isoalizarin-1-methyl ether and methyl isoalizarin reference substances, and dissolving the reference substances in a solvent to prepare a reference substance solution; taking a prismatomeris tetrandra sample, adding an extraction solvent for extraction, and filtering an extracting solution to prepare a test solution; respectively carrying out high performance liquid chromatography detection on the reference substance solution and the test solution, and constructing the fingerprint spectrum of the prismatomeria tetrandra. Compared with the prior art, the method has the beneficial effects that the fingerprint spectrum of the prismatomeria tetrandra is established by adopting an HPLC (High Performance Liquid Chromatography) method and is used for identifying and controlling the quality of the prismatomeria tetrandra medicinal material, so that a standard for comprehensively and effectively controlling the quality of the prismatomeria tetrandra medicinal material is expected to be established.

The invention belongs to the technical field of detection and analysis, and provides an HPLC detection method for taurocholic acid in snake gall bulbus fritilariae liquid, which comprises the following steps: collecting chromatograms of a test sample and a reference substance through HPLC, and judging whether a co-outflow phenomenon exists or not; if the co-outflow phenomenon occurs, interference proportion analysis is carried out, and main interferents are identified; the judged main interferents are removed; carrying out retention analysis to obtain a taurocholic acid retention rate, judging whether the taurocholic acid retention rate accords with expectation or not based on the taurocholic acid retention rate, and if not, judging whether a trailing signal is triggered or not; if the trailing signal is triggered, performing cause analysis to determine the cause of triggering the trailing signal; when the optimal methanol proportion is obtained, a comprehensive detection signal is triggered; if the comprehensive detection signal is triggered, performing comprehensive adaptation analysis of the HPLC detection method to obtain an adaptation index, and evaluating the comprehensive performance of the HPLC detection method according to the adaptation index; and the accuracy of HPLC taurocholic acid detection is effectively improved.

The present invention belongs to the technical field of drug detection, and in particular to a HPLC method for simultaneously qualitatively and quantitatively detecting LXH‑2103 and its impurities. Prepare a test solution, an impurity reference solution and a control solution, inject a blank solution, a test solution, an impurity reference solution and a control solution into a liquid chromatograph respectively, record a chromatogram, calculate the content of LXH‑2103 in the test solution by peak area normalization method, and calculate the content of impurities in the test solution by peak area according to an external standard method; wherein, the impurity is one or more of LXH‑ZZ1, LXH‑ZZ2, LXH‑ZZ3, LXH‑ZZ4 or LXH‑ZZ5. The present invention has good separation between the main peak and each impurity peak, high precision, good stability and good reproducibility, and provides analytical means for LXH‑2103 quality control.

To provide a method for optimizing a safflower seed extraction process based on an ant colony optimization method and back propagation neural network.SOLUTION: A method for optimizing a safflower seed extraction process includes: extracting safflower seeds by ultrasonic waves, and conducting a single-factor experiment in which ultrasonic output, ethanol concentration, solid-liquid ratio, and extracted temperature are selected as affectors in the single-factor experiment; calculating the extraction ratio of CS and FS by using a HPLC method, and determining the optimal value of the affectors on the basis of the extraction ratio; and calculating the total evaluation value by using an entropy weighting method, and obtaining the optimal process parameter by using an ant colony optimization method and back propagation neural network model. Specific steps of the ant colony optimization method and back propagation neural network include a step of constructing a back propagation neural network, and a step of constructing the optimal neural network model of the ant colony optimization method.SELECTED DRAWING: Figure 4

The application discloses a method for constructing a characteristic map of a traditional Chinese medicine and the characteristic map, wherein the method adopts an HPLC method to determine the content of an effective component, imperatorin, in Zhikang capsules, and constructs a high performance liquid chromatography characteristic map of the Zhikang capsules; 10 characteristic peaks are determined as the characteristic map, which are respectively from dragon's blood, rhubarb and Bai Zhi; the components from the dragon's blood are dracorhodin B (peak 2) and pterostilbene (peak 4); the components from the rhubarb are peak 1 (aloe-emodin), peak 3, peak 6 (emodin), peak 9 and peak 10; and the components from the Bai Zhi are imperatorin (peak 5), peak 7 and peak 8; the method covers polyphenols, anthraquinones and furanocoumarins and other main components, and constructs a quality evaluation system of the Zhikang capsules; the method has good specificity, precision, repeatability and solution stability, and can be used for standardizing the production of the Zhikang capsules and guaranteeing the uniformity and stability of the internal quality of products to provide comprehensive quality control.

The invention discloses a beta-alanine identification method, which comprises: S1, sample solution preparation: adding water to a sample, and carrying out ultrasonic treatment to completely dissolve the sample so as to obtain a sample solution; s2, preparing a standard solution: adding water into a beta-alanine standard substance, and performing ultrasonic treatment to completely dissolve the beta-alanine standard substance to obtain the standard solution; s3, HPLC (High Performance Liquid Chromatography) determination: taking the standard solution as a reference substance, and identifying the sample solution by adopting an HPLC method; wherein a chromatographic column is Ultimate OAA, a mobile phase liquid A and a mobile phase liquid B are used for elution, and the mobile phase liquid A is 10mM monopotassium phosphate; the mobile phase liquid B is methanol. The specific mobile phase combination and the specific chromatographic column are adopted, beta-alanine can be rapidly identified, the method has the advantages of being easy and convenient to operate, good in specificity, high in accuracy, low in detection cost and the like, product quality can be better controlled, and quality controllability is achieved.

The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for detecting N-fluorenylmethoxycarbonyl protected histidine and enantiomers thereof, which comprises the following steps: (1) preparing a system applicability solution; (2) injecting the system applicable solution into a high performance liquid chromatograph, and separating by adopting a chiral chromatographic column which takes amylose-tri (3, 5-dimethyl phenyl carbamate) covalently bonded porous silica gel microspheres as a stationary phase; (3) carrying out gradient elution by adopting a binary mobile phase system containing a mobile phase A and a mobile phase B; (4) obtaining a chromatogram map; and (5) calculating the contents of the N-fluorenylmethoxycarbonyl protected histidine and the enantiomer according to the chromatogram. The invention discloses a method for detecting Fmoc-His (Trt)-OH and an enantiomer thereof by an HPLC (High Performance Liquid Chromatography) method. The method has the advantages of very high sensitivity and separation degree, good repeatability and durability, simplicity in operation and stable and reliable result.

The invention relates to the technical field of analysis and detection, and discloses a method for detecting ethanolamine in a Nicodil bulk drug, which comprises the following specific steps: (1) carrying out derivatization reaction on ethanolamine in the Nicodil bulk drug by using 9-fluorenylmethyl chloroformate as a derivatization reagent to obtain a sample containing an ethanolamine derivatization product; and (2) preparing a test solution from the sample containing the ethanolamine derivatization product, and detecting the test solution by high performance liquid chromatography. According to the method, the chloroformic acid-9-fluorenylmethyl ester is used as a derivatization reagent, the pre-column derivatization HPLC method is established to measure the ethanolamine in the Nicodil bulk drug by optimizing derivatization conditions and methodology verification, the conditions are mild, the operation is simple, and the sensitivity is high.

The invention discloses a method for determining the dissolution rate and the dissolution curve of purinol tablets. The dissolution rate of the allopurinol tablets is detected by high performance liquid chromatography instead of an ultraviolet spectrophotometer method used at present. According to the method, a chromatographic column is used as a silica gel bonded octadecylsilane column, an acid solution-organic phase is used as a mobile phase, and an isocratic elution mode is adopted for detection. According to the method for detecting the dissolution rate and the dissolution curve of the allopurinol tablet through the high performance liquid chromatography, detection can be easily and conveniently completed, specificity is high, accuracy is high, repeatability is good, application and linearity are achieved, and the dissolution rate of the allopurinol tablet and the dissolution amount of the dissolution curve can be efficiently and rapidly detected.

The present invention relates to the technical field of drug quality control, and in particular to a method for detecting kanamycin in amikacin sulfate injection. The detection method comprises the following steps: S1 dilutes the amikacin sulfate injection with water, and obtains a test solution by derivatization treatment with an acetonitrile solution containing phenyl isothiocyanate and triethylamine; S2 prepares linear solutions of kanamycin sulfate of different concentrations, and obtains a reference solution by derivatization treatment; S3 elutes the test solution and the reference solution by HPLC, and then enters UV detection and detection to calculate the kanamycin content; the mobile phase used for the elution is 0.08-0.12 mol / L sodium acetate solution (pH value is 6.5±0.2)-methanol, and the volume ratio of the two is 65-75:25-35. The detection method of the present invention has low cost, can effectively separate the components to be tested, has high method sensitivity, good specificity, high precision, good accuracy, and accurate and reliable test results.

The invention belongs to the technical field of medicine detection, and particularly relates to an HPLC (High Performance Liquid Chromatography) method for simultaneously detecting LXH-5 and impurities thereof. Respectively injecting the blank solution, the reference solution and the test solution into a liquid chromatograph, recording chromatograms, calculating the content of LXH-5 in the test solution according to a peak area normalization method, calculating the content of impurities LXH-3 and / or LXH-4 in the test solution according to the peak area according to an external standard method, and determining the content of the impurities LXH-3 and / or LXH-4 in the test solution according to the external standard method. And calculating according to a main component self-contrast method to obtain the content of other impurities in the test solution. The method disclosed by the invention is good in stability, high in precision, good in reproducibility and good in degree of separation between a main peak and each impurity peak, and provides an analysis means for quality control of LXH-5, so that the quality of an LXH-1211 final product is more effectively controlled.

The application belongs to the technical field of medicine detection, and particularly relates to a detection method of Fuyanxiao preparation, which is made of seven medicinal materials of Oxalis corniculata L., Patrinia, Radix Trichosanthis, Radix et Rhizoma Rhei, Cortex Moutan, Atractylodes and Liriodendron, and the detection method is to use HPLC method, acetonitrile as mobile phase A, 0.2% phosphoric acid aqueous solution as mobile phase B for gradient elution to determine the fingerprint and / or characteristic spectrum. The establishment of the detection method is beneficial to comprehensively monitor the product quality, and further helps to guarantee the medicine quality and clinical efficacy.

A computer implementation method for predicting the HPLC retention time of one or more compounds using a machine learning model is disclosed. In particular, the use of a machine learning model to identify a suitable set of HPLC method parameters for separating two or more compounds in a composition is disclosed. Related systems and products are also described.

This invention belongs to the field of chromatographic detection and analysis, and discloses a reversed-phase chromatographic analysis method for the purity of enterokinase protein. High-performance liquid chromatography (HPLC) is used to detect enterokinase in the sample solution. In this HPLC method, the chromatographic column is selected from reversed-phase chromatographic packing material C18 or C8, with a particle size of 3.5~5 μm and a pore size of 120~1000 Å. The mobile phase is selected as follows: an aqueous solution of heptafluorobutyric acid (HFA) is used as mobile phase A, and an acetonitrile solution of HFA is used as mobile phase B. This invention improves the separation of the main peak and subsequent impurities in the enterokinase stock solution by screening suitable mobile phase systems and column types. It also optimizes chromatographic parameters such as the proportion of modifier in the mobile phase, column temperature, sample loading, mobile phase gradient, and wavelength, ultimately achieving effective separation of the main peak and subsequent impurities in the enterokinase stock solution. Furthermore, the analysis time is short and the repeatability is good, providing an effective analytical method for the quality control of enterokinase stock solution.

The application discloses a method for determining the content of carvacol in compound fertilizer, and the method comprises gas phase determination and liquid chromatography, and the gas chromatography method for determining the content of carvacol in compound fertilizer comprises the following steps: S1, sample pretreatment; S2, matrix purification; S3, chromatographic analysis; and S4, quantitative calculation; in the application, a silica gel SPE column is used to replace a traditional diatomite column in the GC method, the polarity impurity adsorption is enhanced through ethyl acetate-hexane gradient activation, sodium chloride salting-out and EDTA complex metal ions are introduced in the HPLC method, the number of miscellaneous peaks in the GC chromatogram is reduced, the separation degree of the carvacol peak is improved, and the service life of the HPLC column is prolonged; the GC method is operated under the conditions of temperature control ultrasonic at 35±2 DEG C and full light avoidance; the HPLC method adopts room temperature methanol-water system extraction, and the recovery rate of the GC method is improved; the HPLC method avoids the 60 DEG C concentration requirement of acetonitrile extraction, and the light stability is improved.

The present invention belongs to the technical field of quality detection of traditional Chinese medicine preparations, and specifically relates to a characteristic spectrum of a pumpkin seed medicinal material and a preparation, and further discloses a method for constructing the characteristic spectrum, as well as a quality detection method for the pumpkin seed medicinal material and the preparation. The characteristic spectrum construction method of the pumpkin seeds and preparations described in the present invention is based on the HPLC method to establish a characteristic spectrum method for pumpkin seed raw medicinal materials and pumpkin seed water-extracted pharmaceutical preparations, and through the optimization of the detection method, the chromatographic conditions are easy to achieve, and the sample processing method is simple to prepare. The validation results of the analytical method show that the method is easy to operate, the results are accurate, the method has good reproducibility, can comprehensively display the chemical composition of pumpkin seeds, and broaden the use of pumpkin seeds.

The present invention provides a high performance liquid chromatography (HPLC) detection method for index components in a Qinzhu Liangxue mixture. The HPLC method is used to detect nine components in the traditional Chinese medicine composition, namely, liquiritin, cimicifugin, 5-O-methylvisamin glycoside, liquiritigenin, baicalin, ethyl p-hydroxybenzoate, paeonol, baicalein and wogonin, so as to more comprehensively characterize the quality of the traditional Chinese medicine composition.

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

The application relates to the technical field of drug detection, in particular to an HPLC detection method for enantiomers in letimovir injection, which comprises the following steps: preparing letimovir sample solution; preparing control sample solution; and detecting by adopting a reversed-phase high performance liquid chromatography system, wherein the high performance liquid chromatography conditions are as follows: a chromatographic column filled with ovomucoid bonded silica gel; a mobile phase A: 0.01 mol / L phosphate solution with a pH value of 3.8-4.2; a mobile phase B: a mixed solution of methanol and acetonitrile, wherein the volume ratio of the methanol to the acetonitrile is 90:10; a flow rate of 0.35-0.45 ml / min; a column temperature of 32-38 DEG C; and a detection wavelength of 250-260 nm. The letimovir and isomers thereof can be effectively separated by the application, the separation capacity is high, the chromatographic medium performance is stable, and the operation process is simple.

The invention provides a deoxycholic acid intermediate detection method, which comprises: dissolving a deoxycholic acid intermediate in a diluent to obtain a sample solution, and detecting the sample solution through an HPLC method. The detection method provided by the invention can effectively separate deoxycholic acid intermediates and impurities so as to effectively control the quality of deoxycholic acid products, and the method completely meets acceptance standards in the aspects of specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, durability, solution stability, system precision, system applicability and the like and has good performance.

A computer-implemented method for predicting the HPLC retention time of one or more compounds using a machine learning model is disclosed. In particular, the present invention discloses the use of a machine learning model for identifying a set of HPLC process parameters suitable for separating two or more compounds in a composition. Related systems and articles are also described.

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 present invention belongs to the field of analysis of traditional Chinese medicine preparations, and specifically relates to a method for determining the contents of seven active ingredients in the classic ancient prescription Xiangsha Liujunzi Decoction. This method utilizes high-performance liquid chromatography (HPLC) under the same experimental conditions to simultaneously separate and determine the contents of liquiritin, apigenin, naringin, hesperidin, nobiletin, costunolide, and dehydrocostuslactone in Xiangsha Liujunzi Decoction. Experimental results demonstrate that the HPLC method established herein for simultaneously determining the contents of multiple different index components in a preparation is simple, rapid, accurate, reliable, and exhibits good repeatability and stability, making it suitable for use as a quality control method for the preparation.

The invention provides a method for determining impurities in ceftriaxone sodium for injection, which is characterized in that an RP-HPLC method is adopted, and a system applicable solution is prepared by taking 1g of ceftriaxone sodium for injection, putting the ceftriaxone sodium into a 10ml measuring flask, dissolving with a phosphate buffer solution with the pH value of 7.0, diluting to a scale, uniformly mixing, sealing, placing in a drying oven with the temperature of 20-50 DEG C for less than 20 hours, and diluting with water to prepare a solution containing 2mg per 1ml; chromatographic conditions comprise that a mobile phase A is an ammonium formate solution, and a mobile phase B is mobile phase A / acetonitrile; performing linear gradient elution; the detection wavelength is 254 nm; the sample injection volume is 5 microliters. The method has good specificity and is suitable for quality control of polymer impurities.