78 results about "Isocratic elution" patented technology

The invention discloses a method for determining bedaquiline fumarate clean verification target residues, and relates to the technical field of instrument analysis of chemical pharmacy. The method comprises the following steps: preparing a sample wiping solution; determining the content of bedaquiline fumarate in the sample wiping solution by adopting a liquid chromatography; chromatographic conditions are as follows: a chromatographic column is a VP-ODS C18 column; mobile phases: a potassium hexafluorophosphate aqueous solution and acetonitrile, wherein the concentration of the potassium hexafluorophosphate aqueous solution is 0.01-0.03 mol / L; the elution mode is isocratic elution; the flow rate is 1 ml / min to 2 ml / min; the column temperature is 28-32 DEG C; the method has good specificity and sensitivity for determination of bedaquiline fumarate cleaning verification target residues, is simple and convenient to operate, rapid in determination, simple and easy to implement, and overcomes the defects that TOC, chemical titration methods, conductivity methods, pH methods and the like which are commonly used at present do not have specificity.

The invention relates to the technical field of plant extraction, and provides a plurality of phenolic compounds in senecio scandens, and a preparation method and application thereof. The method comprises the following steps: crushing senecio scandens, adding ethyl acetate, and performing ultrasonic heating, stirring and extracting to obtain an extracting solution; carrying out rotary evaporation and vacuum concentration on the extracting solution to obtain a crude extract; dissolving the crude extract by using absolute ethyl alcohol through ultrasonic heating, carrying out gradient elution through a macroporous adsorption resin chromatographic column, and collecting an ethanol water eluent; and concentrating the ethanol water eluent under reduced pressure, stirring with a reverse-phase filler, loading with a dry method, packing with a wet method, and sequentially performing isocratic elution with a reverse-phase chromatographic column and purification with a gel column. The dissolution efficiency of phenolic compounds in senecio scandens is improved through ultrasonic and mild heating, the problems that components are degraded due to high temperature in traditional reflux extraction and time and solvent are consumed in dipping extraction are solved, and target component residues are reduced; and then through gradient elution of a chromatographic separation column, isocratic elution of a reversed-phase chromatographic column and purification of a gel column, the problem that phenols are similar in structure and easy to co-elute is accurately solved.

The present application relates to the field of pharmaceutical analysis, and particularly relates to a method for determining the content of cetirizine hydrochloride and preservatives in cetirizine hydrochloride oral solution. The method provided by the present application uses octadecyl bonded silica as the filler of the chromatographic column, uses a mixed solution with specific composition and proportion as the mobile phase, adopts isocratic elution, uses a content volumetric pipette to prepare the test sample solution, injects the test sample solution and the mixed control solution into the liquid chromatograph respectively to perform liquid chromatography, thereby obtaining the chromatogram of the test sample solution and the chromatogram of the mixed control solution respectively; and then according to the external standard method, the content of cetirizine hydrochloride, the content of the hydroxy methylbenzoate preservative and the content of the hydroxy propylbenzoate preservative in the cetirizine hydrochloride oral solution are calculated by the peak area. The method has strong specificity, high accuracy, good precision, linear relationship and stability, and is conducive to the evaluation of sample quality.

The invention discloses a method for detecting phenyl sulfide in rectification residual liquid of 2, 4-dichlorophenol through high performance liquid chromatography, and belongs to the technical field of chemical detection and analysis. The method comprises the following steps: dissolving a to-be-detected 2, 4-dichlorophenol rectification residual liquid sample to prepare a to-be-detected sample, and preparing phenyl sulfide standard substance solutions with different concentrations; the method comprises the following steps: determining a to-be-detected sample and a phenyl sulfide standard substance solution by adopting a high performance liquid chromatograph, drawing a standard curve and a linear regression equation according to a detection result of the phenyl sulfide standard substance solution, and analyzing the phenyl sulfide in the sample by combining the linear regression equation and a chromatographic peak map of the to-be-detected sample, wherein the mobile phase comprises a phase A and a phase B, the phase A is an aqueous solution of phosphate buffer salt, the phase B is methanol, and an isocratic elution mode is adopted. According to the present invention, with the method, the accurate determination of the phenyl sulfide content in the 2, 4-dichlorophenol rectification residual liquid is achieved, the timely and accurate data guidance is provided for the 2, 4-D production process, and the target of production cost saving is ultimately achieved.

The invention relates to the technical field of pharmaceutical analysis, in particular to a chromatographic method for determining optical isomers in a carbidopa raw material medicine and a preparation thereof by using an HPLC (High Performance Liquid Chromatography) method. The detection method is simple, convenient, rapid and accurate to operate, and specifically comprises the following steps: dissolving a proper amount of a sample with a solvent, diluting to a certain concentration, taking a certain volume of the sample, carrying out isocratic elution at a certain column temperature by adopting a high performance liquid chromatography, using a hand-type chromatographic column, a mobile phase A and a mobile phase B, and carrying out quantitative analysis by adopting a self-control method with correction factors. And calculating the isomer in the test solution. The method is good in specificity, solution stability, linearity, repeatability, intermediate precision and durability, and the detection result is accurate and reliable through verification.

The application is suitable for the field of in-vitro diagnosis equipment, and discloses a liquid chromatograph. The liquid chromatograph comprises a liquid phase fluid conveying assembly, a chromatographic column, a detector and a controller; the liquid phase fluid conveying assembly comprises a storage component, a first driving component and a second driving component independent of the first driving component, the first driving component is used for driving a first liquid phase fluid from a first container to the storage component and driving a second liquid phase fluid from a second container to the storage component, so that the first liquid phase fluid and the second liquid phase fluid are mixed in the storage component at a preset ratio to form a third liquid phase fluid of a single concentration and are stored in the storage component; and the second driving component is used for driving the third liquid phase fluid to flow through the chromatographic column from the storage component, so that the third liquid phase fluid elutes a test liquid adsorbed on the chromatographic column. The application can realize the function of isocratic elution by using the liquid phase fluid prepared on line from two liquid phase fluids.

The invention belongs to the technical field of analytical chemistry, and discloses a method for detecting creatinine in a creatine product, which comprises the following steps: (1) precisely weighing a sample, adding a buffer solution, carrying out vortex oscillation dissolution, volume metering, shaking up, centrifuging, and passing through a water phase filter membrane to obtain a creatine test solution; (2) a creatine test solution is taken, a liquid chromatograph is adopted for liquid phase detection, and the liquid chromatography conditions are as follows: an SCX chromatographic column is adopted, an ammonium dihydrogen phosphate solution is taken as a mobile phase for isocratic elution, an ultraviolet detector is adopted, and the content of creatinine is obtained according to a liquid phase detection result. According to the method, the situation that the detection result of the creatinine in the creatine product is virtually high can be remarkably reduced, accurate quantification of the creatinine byproduct creatinine is achieved, and a more perfect data basis is provided for quality control of the creatine product.

The invention provides a method for simultaneously determining ritocaine and prilocaine in blood plasma based on a liquid chromatography-tandem mass spectrometry (LC-MSMS) technology. The specific operation of the method comprises the following steps: adding an internal standard solution and an organic solvent into a plasma sample, and ensuring full extraction of lidocaine and prilocaine through vortex mixing. And separating by using a centrifugal technology, and collecting supernate as a pretreated sample to be detected. An Eclipse Plus C18 chromatographic column is adopted for isocratic elution, effective separation of lidocaine and prilocaine is achieved, and then a sample is subjected to mass spectrometric detection. A standard curve is drawn based on the mass spectrum peak area ratio, a regression equation is obtained, and the concentration of lidocaine and prilocaine in the sample to be detected is obtained through calculation. The method has the characteristics of simplicity and convenience in pretreatment operation, low plasma consumption, short analysis time and high sensitivity, and is suitable for detection of lidocaine and prilocaine in plasma and clinical pharmacokinetic research of the lidocaine cream.

The invention provides a method for determining the content of two sesquiterpenoids in a turmeric extract, and belongs to the technical field of medicine detection.The quality detection method comprises the steps that the turmeric extract is taken to be prepared into a test solution, then acetonitrile (A) and 0.08-0.12 wt% phosphoric acid aqueous solution (B) are subjected to isocratic elution with the ratio of 65-75: 25-35, then an external standard one-point method or a standard curve method is used for determining the content of the two sesquiterpenoids in the turmeric extract, and the content of the two sesquiterpenoids in the turmeric extract is determined. And calculating the content of aryl turmerone and beta-turmerone in the turmeric extract. The method for determining the content of the two sesquiterpene compounds in the turmeric extract is innovatively established, accurate quantitative analysis of the target sesquiterpene component is realized for the first time by optimizing chromatographic separation conditions and detection parameters, the detection blank of an existing standard system is filled, and the method has a wide application prospect. And a key technical support is provided for constructing a turmeric extract multi-dimensional quality control system.

The invention discloses a method for detecting lactic acid in displacement liquid, which comprises the following steps: (1) pretreating the displacement liquid, namely pretreating a sample by using an alkaline solution, standing, adding a proper amount of acid solution for neutralization, filtering by using a filter membrane, and taking a subsequent filtrate to obtain a test solution; and (2) detecting the test solution by adopting a high performance liquid chromatography under the chromatographic conditions that a mobile phase is a phosphoric acid aqueous solution, and isocratic elution is carried out. The mobile phase is simple to prepare, various reagents are not needed, the detection cost is saved, the experimental error is reduced, and the lactic acid in the displacement liquid can be accurately analyzed. The phosphoric acid water is used as a mobile phase, the pH value of the phosphoric acid water is about 2, the activity of silicon hydroxyl in the chromatographic column can be just inhibited, long-time use of the chromatographic column is facilitated, the sample peak shape can be improved, and trailing can be reduced.

The invention relates to the related technical field of measurement of the content of fluticasone propionate emulsifiable paste, in particular to a method for detecting the content of paste by adopting a high performance liquid chromatography, and particularly relates to a method for measuring the content of fluticasone propionate emulsifiable paste by adopting the high performance liquid chromatography, in particular to a method for detecting the content of fluticasone propionate emulsifiable paste by adopting the high performance liquid chromatography. Comprising the following steps: preparing a mobile phase from a diammonium hydrogen phosphate buffer solution (the pH value is 2.0-5.0), methanol and acetonitrile by adopting an octadecyl silane bonded silica gel column; and carrying out isocratic elution. According to the method disclosed by the invention, the diammonium hydrogen phosphate buffer solution-methanol-acetonitrile with a specific ratio is adopted as a mobile phase, and a chromatographic system in which an octadecyl silane bonded silica gel column and a guard column are connected in series is combined, so that the interference of oily auxiliary materials in a cream matrix is effectively eliminated, and the detection specificity and the separation effect are remarkably improved; besides, key chromatographic parameters such as column temperature, flow velocity and detection wavelength are optimized, and a scientific test sample pretreatment process is matched, so that the accuracy and reliability of a content measurement result are guaranteed.

The invention discloses a method for separating and preparing megastigmatrienone isomers, and belongs to the technical field of isomer separation and preparation. The technical problem to be solved is that in the prior art, mg-level separation preparation of a megastigmatrienone single-configuration isomer cannot be rapidly realized. The key point of the technical scheme is as follows: the method comprises the following steps: (1) mixing megastigmatrienone with methanol to obtain a mixed solution; (2) separating the mixed solution by adopting a reversed-phase preparative chromatography to obtain an isomer of megastigmatrienone; wherein the chromatographic conditions in the reversed-phase preparative chromatography in the step (2) are as follows: a chromatographic column is a reversed-phase semi-preparative chromatographic column, the sample size is 100-800 [mu] L, the flow velocity is 0.1-0.8 mL / min, the detection wavelength is 308 nm, an eluent is methanol-THF-H2O in a ratio of 37.5: 7.5: 55, and isocratic elution is performed.

The invention relates to the technical field of substance detection, and particularly discloses an HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride and application. According to the HPLC-ELCD method for simultaneously detecting calcium gluconate, zinc gluconate and lysine hydrochloride, a cation exchange chromatographic column is adopted for isocratic elution of a sample to be detected, and a mobile phase is a methanesulfonic acid-oxalic acid solution; the mobile phase is a methanesulfonic acid-oxalic acid solution, the concentration of methanesulfonic acid is 0.002 mol / L to 0.004 mol / L, and the concentration of oxalic acid is 0.12 g / L to 0.18 g / L. The method disclosed by the invention is high in separation efficiency, good in selectivity, high in detection sensitivity and strong in operability.

The invention relates to the technical field of polypeptide detection, in particular to a method for detecting the content of a semeglutide polymer. A liquid chromatography method is adopted, wherein a chromatographic column is G2000 SWxl; carrying out isocratic elution for 40 minutes; the detection wavelength is 280 nm; the column temperature is 26-30 DEG C; the mobile phase is formed by mixing a phosphate solution of sodium chloride and isopropanol according to the volume ratio of 50: 50. The selected mobile phase has no influence on the retention performance of the chromatographic column, the separation degree of the polymer and the main peak is greater than 1.5, and the requirement on an instrument is lower; accurate and reliable experimental results can be obtained by determining the polymer in the semeglutide through the method.

The application discloses a method for detecting enantiomers in (S)-(1-hydroxypropan-2-yl) tert-butyl carbamate by high performance liquid chromatography. Specifically, the test product is dissolved in a diluent, and detection is performed by using a high performance liquid chromatograph, wherein a CHIRALPAK IG is used as the chromatographic column, the specification of the chromatographic column is an inner diameter of 4.6 mm, a length of 250 mm, and a filler particle size of 5 microns; a mobile phase is water-acetonitrile-tetrahydrofuran, and the volume ratio is 900:75:25; and isocratic elution is adopted. The method is simple and rapid, does not need derivatization treatment, has high sensitivity, good sample solubility, and accurate results, and is suitable for quality control of (S)-(1-hydroxypropan-2-yl) tert-butyl carbamate.

This invention belongs to the field of testing and analysis technology, and discloses a method for rapidly extracting and detecting the content of various terpenoids and sterols in rubber grass. The specific steps are as follows: Step 1: Preparation of standard solutions of terpenoids and sterols. Detection is performed using a general-purpose high-performance liquid chromatograph, eliminating the need for large-scale precision mass spectrometry equipment, resulting in lower purchase and maintenance costs. The operation process is simple and easy to learn, meeting the needs of high-throughput rapid detection of batch samples. A single sample test only takes 35-60 minutes, significantly improving detection efficiency. It can simultaneously complete the qualitative identification and content determination of five target components, including lupeol and taraxasterol. The method has good repeatability and high accuracy, with excellent linearity of the standard curve, and stable and reliable detection results. By optimizing the extraction solvent, temperature, time, and isocratic elution chromatographic conditions, the target components are fully extracted and separated effectively, allowing for accurate acquisition of the content data of each component.

The invention discloses a method for determining isomers in an oseltamivir phosphate product by using high performance liquid chromatography. The chromatographic condition is that a Waters Symmetry C8 chromatographic column is used, a mobile phase is phosphate buffer solution-methanol-acetonitrile, the volume ratio is 620: 245: 135-700: 245: 135, isocratic elution is performed, the concentration of the phosphate buffer solution is 0.040 mol / L to 0.075 mol / L, the pH value is 6.25 to 6.40, the column temperature is 43 to 47 DEG C, the flow velocity is 1.1 to 1.3 ml / min, the detection wavelength is 207 nm, and the sample size is 60 microliters. According to the method, the isomer in the oseltamivir phosphate product can be rapidly and accurately detected, the content of the isomer can be calculated, the operation is simple, the reproducibility is good, the quality control of an oseltamivir phosphate preparation and an intermediate product thereof can be well realized, and a guarantee is provided for synthesis and preparation process optimization.

The invention discloses a method for detecting the content of fumaric acid vonoprasan in a fumaric acid vonoprasan tablet, which comprises the following steps: carrying out ultrahigh liquid chromatography detection on a sample to be detected, and determining the content of fumaric acid vonoprasan in the sample to be detected on the basis of a detection result, a mobile phase adopted in the ultrahigh liquid chromatography detection comprises a phosphate buffer solution and methanol, and the volume ratio of the phosphate buffer solution to the methanol is (50-70): (30-50); the elution mode is isocratic elution. According to the detection method, an isocratic elution mode is adopted, the treatment mode is simple, the detection operation time is short, and consumed resources are fewer; the phosphate buffer solution and the methanol in a specific ratio are used as mobile phases, so that the method has the advantages of strong qualitative specificity, accurate quantification, high sensitivity, good method stability, short operation time, high efficiency, rapidness, high detection efficiency and the like, and can realize effective detection of the content of the Vonoprazan fumarate in the Vonoprazan fumarate tablets.

The invention discloses a method for detecting 3-chloroaniline in a trazodone hydrochloride tablet, the detection method is a high performance liquid chromatography, an octadecylsilane bonded silica gel packed column is used, a phosphoric acid aqueous solution with a volume fraction of 0.1 + / -0.02% is used as a mobile phase A, acetonitrile is used as a mobile phase B, gradient elution is carried out, and the elution procedure is as follows: 0-7th minutes, 0-7th minutes, 0-7th minutes, 0-7th minutes, 0-7th minutes, 0-7th minutes, 0-7th minutes, 0-7th minutes, 0-7th minutes, 0-7th minutes and 0-7th the mobile phase A and the mobile phase B with the constant volume fraction are used for isocratic elution, and the volume fraction of the mobile phase B is 2-10%; the volume fraction of the mobile phase B is increased for gradient elution for 12 minutes, and the volume fraction of the mobile phase B is 68%; performing isocratic elution for 17 minutes by keeping the volume fraction of the mobile phase B to be 68%; reducing the volume fraction of the mobile phase B to 5% for gradient elution for 18 minutes; and finally, keeping the volume fraction of the mobile phase B at 5%, performing isocratic elution for 25 minutes, and ending. In the elution process, the total volume fraction of the mobile phase A and the mobile phase B is 100%. Qualitative and quantitative analysis of 3-chloroaniline can be completed only by using high performance liquid chromatography.

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 invention relates to the technical field of pharmaceutical analysis, and particularly discloses a method for detecting related substances in a key parent nucleus of cefcapene pivoxil hydrochloride. Detection is carried out according to the following high performance liquid chromatography conditions: a chromatographic column is GL Sciences InertSustaiin C18, 4.6 mm * 250 mm, 5 [mu] m, and the column temperature is 25 DEG C; a mobile phase is ammonium acetate solution-acetonitrile-tetrahydrofuran; the detection wavelength is 255 nm to 275 nm, the column temperature is 20 DEG C to 30 DEG C, and isocratic elution is carried out. By adopting the method provided by the invention, various impurities such as D-CPC, 7-ADCA, N-acetyl-D-7-ACA, 7-ACA, D-7-ACA lactone, cephalosporin C and the like in the key mother nucleus of the cefcapene pivoxil hydrochloride are effectively detected, and the condition of the impurities in the key mother nucleus of the cefcapene pivoxil hydrochloride is accurately, qualitatively and quantitatively detected. Therefore, the clinical safety of the cefcapene pivoxil hydrochloride product is improved.

The invention discloses a method for detecting sodium hydrogen sulfite in a compound amino acid injection, which adopts high performance liquid chromatography for detection, and the chromatographic conditions are as follows: a chromatographic column adopts a hydrogen-type sulfonated crosslinked styrene-diethylbenzene copolymer as a filler; a mobile phase is a sulfuric acid aqueous solution; the elution mode is isocratic elution; and the detector is an ultraviolet detector. By adopting the high performance liquid chromatography detection method, the sodium hydrogen sulfite in the compound amino acid injection can be directly, conveniently, quickly, qualitatively or quantitatively detected, and the technical problems of low detection efficiency, complicated operation and the like in the prior art are solved; moreover, an ultraviolet detector is adopted for direct determination, so that the use of a derivative reagent is avoided, and the method has the advantages of environmental protection and convenience. The method provided by the invention has the advantages of strong specificity, high sensitivity, good linear relationship, high accuracy and good repeatability, and can be used for accurately judging the storage state and production quality of the compound amino acid injection.

The invention relates to a preparation method for purifying and salifying quinidine. The preparation method comprises a purification method of quinidine and a salifying method of quinidine. The purification method of the quinidine comprises the following steps: weighing an initial raw material which is total alkali obtained after quinine is separated and removed from a peruvian bark extract, adding dichloromethane into the initial raw material, stirring until the dichloromethane is completely dissolved, and separating and purifying a dissolved solution by using column chromatography so as to complete purification of the quinidine, the salifying method of the quinidine comprises the following steps: firstly, preparing a sulfuric acid methanol solution, then adding methanol, the purified quinidine and water into a reaction kettle, regulating the pH value of the solution in the reaction kettle to 6-7 by using the sulfuric acid methanol solution, then drying twice to obtain a quinidine sulfate dihydrate crude product, and finally obtaining the quinidine sulfate dihydrate. And refining to obtain a quinidine sulfate dihydrate refined product. In order to solve the problem that a gradient elution process used in a column chromatography process in an original quinidine purification method is complex in operation, an isocratic elution process is adopted, and the whole process does not involve the change of the proportion of an organic solvent, so that the operation is simplified.

The invention provides a method for detecting the content of urea in a water sample by using high performance liquid chromatography. The method comprises the following steps: preparing a urea standard solution; performing filter membrane filtration pretreatment on the to-be-detected water sample; carrying out high performance liquid chromatography analysis according to optimized chromatographic conditions, and calculating the urea content by adopting a standard curve method; wherein the chromatographic conditions are as follows: a C18 type reversed-phase chromatographic column is adopted, a mixed solution of acetonitrile and ultrapure water is adopted as a mobile phase, isocratic elution is performed, and the detection wavelength is 190-200nm. According to the method, the mobile phase and the chromatographic column are improved, the urea content in the water sample is directly and accurately detected, operation is easy and convenient, the detection time is short, good specificity and stability are achieved, the detection limit is lower than 0.6 microgram / L, the recovery rate ranges from 95% to 105%, the relative standard deviation is smaller than 2%, and the method can be effectively applied to detection and analysis of the urea content in various environment water samples.

The invention belongs to a pharmaceutical analysis and detection method. The invention provides a method for determining the content of caffeic acid in rabdosia amethystoides, which comprises the following steps: determining the content of caffeic acid in rabdosia amethystoides by adopting a high performance liquid chromatography, and the conditions of the high performance liquid chromatography are as follows: a chromatographic column is a C18 column; the column temperature of a chromatographic column is 15-45 DEG C; the sample size is 5-25 [mu] L; a mobile phase is phosphoric acid aqueous solution-acetonitrile; the elution condition is isocratic elution; the number of theoretical plates should not be less than 5000 in terms of caffeic acid peaks; the flow velocity of the mobile phase is 0.5-2 mL / min; and the detection wavelength is 330 nm. According to the present invention, the high performance liquid chromatography is adopted to achieve the determination of the caffeic acid content in the rabdosia amethystoides, the determination method is simple and accurate, and the verification results show that the determination method has high repeatability, high stability and high credibility, and can provide the reference basis for the quality evaluation of the rabdosia amethystoides.

The application relates to the technical field of pharmaceutical analysis and detection, in particular to a high-performance liquid chromatography detection method for formic acid and acetic acid in polidexide. The application adopts a chromatographic column with octadecylsilane-bonded silica gel as a filler, uses a 0.1% phosphoric acid aqueous solution as a mobile phase, and realizes the simultaneous separation and accurate quantification of two impurities (formic acid and acetic acid) introduced in the polidexide production and storage process through specific isocratic elution detection parameters. The method has strong specificity, good precision, high sensitivity, excellent linear relationship and high accuracy. The detection method provided by the application is simple in operation and controllable in parameters, fully meets the requirements of drug quality control and registration declaration, and can be widely applied to the quality detection of polidexide raw materials and preparations.

The invention discloses a detection method of lysophosphatidylcholine, which can realize good separation of lysophosphatidylcholine and other components in a preparation sample by optimizing a chromatographic column, adjusting a mobile phase and using isocratic elution, greatly shortens the operation time of a single needle, and improves the detection efficiency.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for chiral resolution of a clodinafop-propargyl enantiomer. According to the present invention, the high performance liquid chromatography-mass spectrometry technology is adopted to separate the clodinafop-propargyl enantiomer, the chromatographic column is the polysaccharide derivative chiral chromatographic column, the mobile phase A is the organic solvent, the mobile phase B is pure water, the volume ratio of the mobile phase A to the mobile phase B is 40: 60-100: 0, isocratic elution is performed, the column temperature is 30-35 DEG C, and the flow rate is 0.5-0.8 mL / min. The invention provides the method for effectively separating the chiral propargyl enantiomer, and the method has the advantages of high sensitivity, simplicity in operation, high separation speed and the like.

This invention belongs to the technical field of bactericide residue analysis and determination in plant-derived foods, specifically relating to a method for detecting isobutylethoxyquinoline and its metabolites in plant-derived foods. The method includes extraction with acetonitrile under citrate conditions, followed by purification with C18 (25 mg), PAX (25 mg), and XFM64 (nitrogen-doped multi-walled carbon nanotubes, 10 mg) adsorbents. Chromatographic separation is performed using a C18 column with methanol-2 mmol / L ammonium acetate (containing 0.1% formic acid) as the mobile phase, isocratic elution at a flow rate of 0.40 mL / min, electrospray ionization (ESI+), and detection in multiple reaction monitoring (MRM) mode. This invention is simple to operate, has high pretreatment efficiency, and its precision and recovery rate meet the regulatory residue limit monitoring requirements. It is suitable for the simultaneous determination of isobutylethoxyquinoline and its metabolites in plant-derived foods.

The invention discloses a method for detecting vitamin B12 and impurities thereof, and belongs to the technical field of medicine analysis and detection. The method comprises the following steps: introducing a sample to be detected into high performance liquid chromatography for detection; high performance liquid chromatography detection conditions are as follows: a chromatographic column takes hydrophilic octadecylsilane chemically bonded silica as a filler; the mobile phase comprises a mobile phase A and a mobile phase B, the mobile phase A is a buffer solution, and the mobile phase B is methanol; the pH value of the buffer solution is 3-4; the column temperature is 55-65 DEG C; the flow velocity of the mobile phase is 0.15 to 0.25 mL / min; the sample injection volume is 15-25 [mu] L; the detection wavelength is 361nm; the elution mode is isocratic elution; the volume ratio of the mobile phase A to the mobile phase B in isocratic elution is (80-90): (10-20). The method has good specificity, accuracy, precision and durability, can realize single detection of vitamin B12 and impurities thereof, and is simple, convenient and feasible.