Abrégé

The present invention relates to the field of drug analysis and testing, and provides a method for measuring the ethanol content in a methylergonovine maleate tablet. The present invention comprises the following steps: injecting a blank solution, a reference solution and a test solution into respective gas chromatographs; recording chromatograms; and measuring the residual ethanol content in the methylergonovine maleate tablet by calculating a peak area and according to an external standard method. The method of the present invention is rapid and efficient, involves low toxicity, has important significance in guiding enterprises to adjust process parameters and guaranteeing the medication safety of people, and involves short analysis time and low test costs. Few toxic and harmful reagents are used in the method, which conforms to the green industrialization development trend of the pharmaceutical industry in China.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/30 - Contrôle des paramètres physiques du fluide vecteur de la température
• G01N 30/32 - Contrôle des paramètres physiques du fluide vecteur de la pression ou de la vitesse
• G01N 30/68 - Détecteurs électriques à ionisation de flamme

Abrégé

The present invention relates to the technical field of calcium ion antagonist detection and provides a human plasma calcium ion antagonist-tandem mass spectrometry detection kit. The kit comprises a calibration material, a control material, an internal standard solution, an extraction agent, a QuEChERS purification material, a salting-out agent, a mobile phase A solution, a mobile phase B solution, a complex solution, a waterproof packaging bag, and a packaging box for separating and intensively packaging reagent bottles or tubes. The kit is high in sensitivity, high in specificity, and high in accuracy detection result, multiple CCBs with antihypertensive effects can be detected at the same time, and a CCBs direct detection method and kit are easy and convenient to operate and easy to popularize, so that the influence of a matrix effect and the instability of compound on an experimental result is reduced, thereby improving the clinical detection quality.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/72 - Spectromètres de masse
• G01N 30/86 - Analyse des signaux

Abrégé

The present invention relates to the technical field of separation and purification, and particularly, to a method for separating high-purity cepharanthine. The method comprises the following steps: A, grinding a Stephania erecta slice, Stephania delavayi, or a cepharanthine-containing Menispermaceae herb as raw materials into a powder by using a mortar, adding an extracting agent, extracting by 20 minutes of ultrasonication, and concentrating at a reduced pressure by rotary evaporation to remove the extracting agent; B, loading the extract obtained in step A on a silica gel column for chromatography, and eluting to obtain a crude cepharanthine product; C, filtering the crude cepharanthine product through a 0.45 μm membrane and purifying by preparative liquid chromatography; and D, concentrating the fraction obtained in step C at a reduced pressure by rotary evaporation at 35 °C to remove methanol, and lyophilizing to give a white solid, i.e., purified cepharanthine. The method features high cepharanthine purity, a simple and controllable separation process, and suitability for automation in industrial production.

Classes IPC  ?

• C07D 491/22 - Composés hétérocycliques contenant dans le système cyclique condensé, à la fois un ou plusieurs cycles comportant des atomes d'oxygène comme uniques hétéro-atomes du cycle, et un ou plusieurs cycles comportant des atomes d'azote comme uniques hétéro-atomes du cycle, non prévus dans les groupes , , ou dans lesquels le système condensé contient au moins quatre hétérocycles

Abrégé

The present invention relates to the field of drug analysis and detection, and provides a method for determining dissolution rates of eight representative components in Daochi pills, which comprises the following steps: preparing a mixed reference solution: taking 200 mL of degassed hydrochloric acid solution having a pH value of 1.0 as a dissolution medium, keeping the temperature at 37±0.5°C and the rotating speed at 80 r/min, lowering the solution into a container by means of a paddle, performing sampling after 180 min to obtain 2 mL of a product, and filtering same by using a 0.22 μm microporous filter membrane, so as to obtain the mixed reference solution; preparing a test solution; and precisely suctioning 1 μl of the mixed reference solution and 1 μl of the test solution, respectively, injecting same into an ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS) instrument, performing determination, and calculating content by means of an external standard method. According to the present invention, the dissolution rates of baicalin, berberine hydrochloride, aloe-emodin, calceolarioside B, harpagoside, geniposide, paeoniflorin, and forsythiaside A are determined by using a UPLC-MS/MS method, so that the medicine quality of Daochi pills is comprehensively evaluated, and a reference can be provided for quality control and efficacy verification of Daochi pills.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/72 - Spectromètres de masse
• G01N 30/86 - Analyse des signaux

Abrégé

A method for simultaneously measuring the content of 24 ingredients in Daochi Wan, comprising the following steps: preparing a mixed reference solution; preparing a test solution: precisely drawing 1 μL each of the mixed reference solution and the test solution, injecting same into an ultra-high performance liquid chromatography mass spectrometer, measuring, and calculating the content by using an external standard method. A UPLC-MS/MS method for simultaneously measuring 24 ingredients in Daochi Wan has strong specificity and many control ingredients. Different medicinal materials in a prescription are comprehensively measured and analyzed to conduct a more comprehensive assessment of drug quality. At the same time, the concept of convenient, efficient and resource-saving inspection and testing work is also reflected.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/72 - Spectromètres de masse
• G01N 30/86 - Analyse des signaux

Abrégé

The present invention relates to the technical field of traditional Chinese medicine detection, and specifically relates to a content measurement method for six alkaloid components in a small meridian-activating pill, comprising: preparing a mixed reference solution; preparing a test solution; respectively and precisely suctioning 15 μl of the mixed reference solution and 15 μl of the test solution, injecting the mixed reference solution and the test solution into a liquid chromatograph, measuring, and calculating the content by means of an external standard method. In the present invention, an HPLC method is established for simultaneously measuring the content of six alkaloid components in the small meridian-activating pill, the method is simple and convenient, and has high specificity, and monoester and diester alkaloids are controlled at the same time, such that quality control of herbal medicine Aconitum is facilitated, the safety and effectiveness of clinical medication are ensured, and reference is provided for quality control and quality evaluation of products.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/86 - Analyse des signaux

Abrégé

Disclosed is a method for detecting benzenesulfonate genotoxic impurities in a cisatracurium besilate injection, the method comprising the following steps: taking a mixed control solution, a blank solution and a test solution, respectively injecting same into a liquid chromatography-mass spectrometer, recording a chromatogram, and respectively calculating the content of methyl benzenesulfonate, ethyl benzenesulfonate, propyl benzenesulfonate and isopropyl benzenesulfonate in a cisatracurium besilate injection on the basis of peak area by means of an external standard method. The method for simultaneously determining the content of four benzenesulfonate genotoxic impurities in a cisatracurium besilate injection using liquid chromatography-mass spectrometry is simple and accurate, has high sensitivity, meets the detection requirements, is suitable for routine detection of genotoxic impurities in a cisatracurium besilate injection, and provides a reference and basis for the revision of genotoxic impurity inspection items in the quality standard thereof, thereby effectively improving the drug quality, and reducing the risk of clinical medication.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/72 - Spectromètres de masse

Abrégé

The present invention relates to the technical field of inhibitor detection, and provides a tandem mass spectrometry detection kit for a human urine anti-hepatoma tyrosine kinase inhibitor, comprising calibrators, quality control products, an internal standard solution, an extractant, a QuEChERS purification material, a salting-out agent, a mobile phase A solution, a mobile phase B solution, a reconstituted solution, a waterproof packaging bag, and a packaging box for separating and collectively packaging reagent bottles or tubes. By combining a QuEChERS technology and a high performance liquid chromatography-mass spectrometry technology, the dosage of a sample is small, the result is accurate, reliable, and sensitive, and the present invention is suitable for simultaneously detecting a plurality of TKIs having an anti-hepatoma effect; moreover, the kit has the advantages of being simple and convenient to operate, and easy to popularize, and can avoid an experimental error caused in a reagent preparation process, thereby improving the clinical detection quality.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• B01J 20/281 - Absorbants ou adsorbants spécialement adaptés pour la chromatographie préparative, analytique ou de recherche
• G01N 30/72 - Spectromètres de masse

Abrégé

The present invention relates to the technical field of inhibitor detection, and provides a tandem mass spectrometry detection kit for a human plasma anti-hepatoma tyrosine kinase inhibitor. The kit of the present invention comprises a calibrator, a quality control product, an internal standard solution, an extractant, a QuEChERS purification material, a salting-out agent, a mobile phase A solution, a mobile phase B solution, a reconstitution solution, a waterproof packaging bag, and a packaging box for separating and centrally packaging reagent bottles or tubes. The present invention has high sensitivity, high specificity and high accuracy of detection results, can also simultaneously detect a plurality of TKIs having an anti-liver cancer effect, and has a method and kit for directly detecting TKIs which are simple and convenient to operate and easy to popularize, so as to reduce the influences of matrix effects and compound instability on experimental results, thereby improving the quality of clinical detection.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/04 - Préparation ou injection de l'échantillon à analyser
• G01N 30/06 - Préparation
• G01N 30/72 - Spectromètres de masse
• G01N 30/86 - Analyse des signaux

Abrégé

The present invention relates to the technical field of sterility detection in sterile drug substances, and in particular to a method for fast sterility detection of sterile drug substances. The method comprises: after 48 hours of culture, aseptically adding 1-10 mL of a culture broth from each of an anaerobic bacterium collector and a fungus or aerobic bacterium collector into an anaerobic bacterium culture flask containing hemolysin or a standard aerobic culture flask in an automatic microorganism culture/detection system, and cultivating in the automatic microorganism culture/detection system for 5 days; and continuing the anaerobic bacterium collector and the fungus or aerobic bacterium collector cultivation for 14 days at 30-35 °C or 20-25 °C. On the basis of no changes in the existing method for sterility detection in sterile drug substances and minimized changes in system applicability, the period for sterile detection is reduced to 7 days.

Classes IPC  ?

• C12Q 1/04 - Détermination de la présence ou du type de micro-organismeEmploi de milieux sélectifs pour tester des antibiotiques ou des bactéricidesCompositions à cet effet contenant un indicateur chimique
• G01N 21/64 - FluorescencePhosphorescence

Abrégé

The present invention relates to the field of drug analysis and detection, and provides a method for determining the salt forming rate in a raw material, i.e., methylergonovine maleate. The method of the present invention comprises the following steps: respectively injecting a system suitability solution, a blank solution, a reference solution and a test solution into an ion chromatograph, recording a chromatogram, calculating the content of maleic acid in the bulk drug methylergonovine maleate by using a peak area according to an external standard method, and substituting the content into formula (1) to calculate the salt forming rate of the raw material, i.e., methylergonovine maleate. The method of the present invention has high specificity and sensitivity, is simple to operate and has an accurate result.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/64 - Détecteurs électriques

Abrégé

The present invention relates to the field of drug analysis and detection, and provided is a method for detecting a residual solvent in a pingyangmycin hydrochloride bulk drug. The method of the present invention comprises the following steps: respectively heating a blank solution, a mixed control solution, and a test sample solution and balancing same, injecting same into a gas chromatograph using a headspace sample injection method, recording the chromatogram, and calculating the content of the residual solvent on the basis of the peak area according to the external standard method. The method of the present invention is simple and accurate, and has a high sensitivity. The method of the present invention meets the residual solvent detection requirement, is suitable for daily detection of the residual solvent in the pingyangmycin hydrochloride bulk drug, and provides a reference and basis for the revision of the residual solvent check item in the quality standard of the product. Therefore, the method of the present invention effectively improves the quality of the bulk drug, and reduces the clinical medication risk.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/68 - Détecteurs électriques à ionisation de flamme

Abrégé

The present invention relates to the field of pharmaceutical analysis and testing, and provides a method for efficiently measuring trace copper elements in a bleomycin A5 hydrochloride raw material at low consumption, comprising the following steps: (1) preparing a test solution and a blank solution; (2) preparing a standard copper solution; (3) sequentially introducing the standard copper solution prepared in step (2) into an atomic absorption spectrometer by means of a flame method, measuring an absorbance value of the standard copper solution, performing linear regression on copper concentration by means of the absorbance value of the standard copper solution, and simulating a linear regression equation; and (4) introducing the test solution prepared in step (1) into the atomic absorption spectrometer, measuring an absorbance value of the test solution, and calculating the content of copper elements in a sample according to a relationship between an absorbance value and concentration. The present invention is fast, simple, stable, interference-free, accurate in results, fewer in used reagents, low in test costs, and is suitable for the quality monitoring of large-batch products of an enterprise.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne
• G01N 30/06 - Préparation
• G01N 30/74 - Détecteurs optiques

Abrégé

A method for testing the dissolution rate of Siji Sanhuang tablets, relating to the technical field of traditional Chinese medicine testing. The method comprises the following steps: (1) the preparation of a test solution; (2) the preparation of a control solution; and (3) the determination of the dissolution rate, wherein the chromatographic condition is that the chromatographic column is Waters HSS C18 (1.7 μm, 2.1×100 mm); gradient elution is performed with acetonitrile as a mobile phase A and 0.1% aqueous trifluoroacetic acid as a mobile phase B; the test wavelength is 254 nm; the column temperature is 30-40°C, and the flow velocity is 0.2-0.3 ml·min-1. The contents of geniposide, berberine hydrochloride, baicalin, and oroxindin are determined by means of a highly-efficient liquid chromatography method. The method is simple and convenient to operate and accurate in result, and is thus suitable for testing the dissolution rate of Siji Sanhuang tablets.

Classes IPC  ?

• G01N 30/02 - Chromatographie sur colonne

Abrégé

A method for detecting the bacterial filtration efficiency of a mask, which belongs to the technical field of mask detection. The method comprises the following steps: (1) pretreating a sample; (2) preparing a bacterial suspension for test; (3) atomizing the Staphylococcus aureus suspension into an aerosol for spraying, vertically spraying the aerosol passing through a pipeline to a mask fixed on a sampler at a flow rate of 1 mL/min for 1 min, then stopping the spraying, spraying with sterile air for 1 min, enabling the aerosol to enter an impingement liquid collector through the mask, collecting the aerosol penetrating through the sample in each collector by using 20 mL of sterile peptone water, and controlling the flow rate of the gas passing through the sampler at 28.3 L/min; (4) counting the bacteria in the peptone water in the collectors with an electronic bacterial counter by means of a sterile operation to respectively obtain the number of bacteria in the peptone water with the mask sample added thereto, namely, the bacterial penetration value, and the number of bacteria in the peptone water without the mask, namely, the positive control value; and (5) calculating a result according to a formula.

Classes IPC  ?

• G01N 15/10 - Recherche de particules individuelles
• C12Q 1/14 - StreptocoquesStaphylocoques
• C12R 1/445 - Staphylococcus aureus