486 results about "Gradient elution" patented technology

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 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.

This invention discloses an analytical method for benzothiazole contaminants, comprising the following steps: detection by high performance liquid chromatography (HPLC), with the following chromatographic conditions: a phenylhexyl column as the stationary phase, mobile phase A being water, mobile phase B being acetonitrile, and gradient elution; wherein the benzothiazole contaminants are at least one of 2-aminobenzothiazole, 2-hydroxybenzothiazole, benzothiazole, 2-methylbenzothiazole, 2-mercaptobenzothiazole, 2,5-dimethylbenzothiazole, 2-cyanobenzothiazole, ethyl 2-carboxylate benzothiazole, 2-chlorobenzothiazole, 2-bromobenzothiazole, 2-methylthiobenzothiazole, phenylthiocyanate, N-tert-butyl-2-benzothiazole sulfenamide, 2-(2-hydroxyphenyl)-benzothiazole, N-cyclohexyl-2-benzothiazole sulfinamide, dibenzothiazole disulfide, and N,N-dicyclohexyl-2-benzothiazole sulfonamide.

The invention relates to the technical field of pharmaceutical analysis, and particularly discloses a high performance liquid chromatography-mass spectrometry tandem method (HPLC-MS / MS) for detecting a genotoxic impurity L-alanine isopropyl ester in an emtricitabine-propofol tenofovir tablet. By optimizing chromatographic column selection, a mobile phase gradient elution procedure and mass spectrometric detection parameters, the method realizes exclusive, sensitive and accurate detection of the L-isopropyl alanine. The methodological verification result shows that the detection limit is 1.00 ng / mL, the quantification limit is 2.00 ng / mL, the linear range is 2.00-100.00 ng / mL (the correlation coefficient r is equal to 0.9994), the recovery rate is stabilized between 92% and 98%, and the precision and repeatability are good. The detection method has the advantages of high sensitivity and strong selectivity, is suitable for quality control of emtricitabine propofol tenofovir tablets, meets the control requirements of ICH M7 guide on genotoxic impurities, and has good practicability and popularization value.

This invention relates to a method for establishing and detecting the fingerprint spectrum of the traditional Chinese medicine composition Taohongyin. The raw materials of the traditional Chinese medicine composition include: chicken gizzard lining, papaya, hawthorn, chrysanthemum, tangerine peel, peach kernel, and wolfberry. The fingerprint spectrum establishment method includes the preparation of a reference solution and a test solution; detection of the reference solution and the test solution using high-performance liquid chromatography (HPLC); the mobile phase used in the HPLC is acetonitrile and phosphoric acid aqueous solution, and the elution method is gradient elution.

This invention discloses a method and application for extracting soluble collagen from bones unearthed from archaeological sites, belonging to the field of archaeological sample processing technology. Specifically: 1) After pretreatment, the blocky ancient bone sample is dried at low temperature and ground into bone powder; the bone powder is added to an acidic solution for ultrasonic treatment, centrifuged, and the supernatant is filtered to obtain the sample to be loaded onto a column; 2) The sample to be loaded onto the column is subjected to chromatographic separation, using a gradient elution with equilibration buffer and elution buffer, and a UV detector is used to monitor protein peaks, collecting the target protein solution that elutes within 20-30 minutes; 3) Finally, the target protein solution is concentrated and purified using an ultrafiltration tube to obtain soluble collagen. This invention can obtain a sufficient amount of collagen from ancient deteriorated bone samples, significantly improving sample utilization and providing reliable technical support for bioarchaeological research.

The invention relates to a spleen-tonifying, appetite-stimulating and digestion-promoting traditional Chinese medicine preparation UPLC detection method and a fingerprint spectrum, and belongs to the technical field of medicine detection. The invention aims to solve the technical problems that the existing quality control method of the spleen-tonifying, appetite-promoting and digestion-promoting pills lacks comprehensive and objective analysis on the spleen-tonifying, appetite-promoting and digestion-promoting pills, and the problems of low precision, poor reproducibility, low efficiency and the like during detection of related components in the prior art are solved. According to the technical scheme, the UPLC detection method is characterized in that a mixed standard substance of gallic acid, 5-hydroxymethylfurfural, chlorogenic acid, sinapine thiocyanate, sinapic acid, hyperoside, 3, 6-dimustard acyl sucrose, hesperidin, naringenin, nobiletin and hesperetin is taken as a contrast, an acetonitrile-0. 1% formic acid aqueous solution is taken as a mobile phase, gradient elution is carried out, and the content of chlorogenic acid in the sample is detected. The qualitative and quantitative detection of the effective components of the spleen-tonifying, appetite-promoting and digestion-promoting pill is realized.

The invention discloses a method for detecting phosphate impurities, namely diethyl phosphoacetic acid and diethyl phosphate, in afatinib, and establishes a simple and sensitive ion chromatography detection method based on the hydrolysis property of a phosphate compound under an alkaline condition. Sodium hydroxide or potassium hydroxide solution-water is used as a mobile phase for isocratic or gradient elution, and a conductivity detector is used for detection. According to the present invention, the accurate quantification of the impurities in the afatinib is achieved, the detection speed is fast, the cost is low, the operation is simple, and the good specificity, the sensitivity, the precision and the accuracy are provided, such that the product quality of the afatinib maleate bulk drug synthesized by using the diethyl phosphoacetic acid as the starting material and the related preparation can be further ensured.

The application provides a detection method of hydroxypropyl cellulose in a povidone-containing preparation, and specifically comprises the following steps: (1) preparing a sample solution by pretreating a sample to be detected; (2) detecting the sample solution by using HPLC, wherein an evaporative light scattering detector or an electrospray detector is used as a detector, a C18 chromatographic column is used as a chromatographic column, the column temperature is 20-40 DEG C, water is used as a mobile phase A, methanol is used as a mobile phase B, the flow rate is 0.5 ml / min-1.5 ml / min, and gradient elution is adopted. The detection method has good specificity and peak type, can not only separate hydroxypropyl cellulose from povidone and other high-molecular auxiliary materials in a pharmaceutical preparation, accurately quantify the content of hydroxypropyl cellulose, but also effectively identify the model, and provides a good method for reverse analysis, component analysis, auxiliary material release detection of the pharmaceutical preparation.

The application relates to the technical field of natural medicinal chemistry, and specifically discloses a triterpenoid compound and application, and a preparation method of the compound. The preparation method comprises the following steps: drying and crushing schisandra chinensis roots to obtain dried and crushed schisandra chinensis roots, extracting the dried and crushed schisandra chinensis roots by using 70% ethanol water solution under negative pressure cavitation, combining and concentrating the extract to obtain a crude extract, separating the crude extract by using a D101 macroporous adsorption resin, eluting the crude extract by using water, 30% ethanol, 70% ethanol and 90% ethanol in sequence, collecting a 70% ethanol elution part, performing MCI column chromatography on the 70% ethanol elution part, performing gradient elution on the 70% ethanol elution part by using methanol-water, collecting a depigmentation sample, performing ODS column chromatography on the depigmentation sample, performing gradient elution on the depigmentation sample by using water-methanol, collecting a target component, and purifying the target component by using a preparative high performance liquid chromatograph to obtain the target compound. The application separates a novel triterpenoid compound from schisandra chinensis roots for the first time, expands the development range of medicinal resources of schisandra chinensis plants, simultaneously provides a novel structure mother nucleus and a candidate active molecule for anticancer drug research and development, and enriches the research and development reserves of antitumor natural medicines.

The invention relates to the technical field of vegetable and fruit pesticide residue detection, in particular to a method and a system for separating and determining ethiprole enantiomer residue in grapes by ultra performance convergence chromatography. The method comprises the following steps: extracting a sample twice by 1% acetic acid acetonitrile, performing rotary evaporation concentration, redissolving by dichloromethane / methanol, purifying by adopting an amino solid-phase extraction column, concentrating, fixing the volume by isopropanol / n-heptane (1: 9), and filtering. The method comprises the following steps: separating by using a Trefoil CEL2 chiral chromatographic column, carrying out gradient elution at 35 DEG C and 10.3 MPa by using supercritical CO2 as a main mobile phase and 0.5% ammonia water methanol as a modifier, detecting PDA at 280 nm, and carrying out external standard quantification. The method is rapid in separation and good in peak shape, the linear range is 0.5-20.0 mg / L, the LOQ is 0.1 mg / kg, the adding standard recovery rate is 80.0%-108%, the RSD is 3.1%-8.4%, and the method is suitable for monitoring ethiprole enantiomer residues in grapes.

The invention relates to the technical field of medicine detection, in particular to a separation method of N-fluorenylmethoxycarbonyl-N '-trityl-L-histidine and related substances. The invention provides a method for analyzing the purity of N-fluorenylmethoxycarbonyl-N '-trityl-L-histidine and related substances, which comprises the following steps: high performance liquid chromatography is adopted, and the chromatographic conditions are as follows: a filler of a chromatographic column is pentafluorophenyl silica gel; the mobile phase A is an aqueous solution containing 0.1 wt% of phosphoric acid (the pH is adjusted to 3.7 by using ammonia water); the mobile phase B is acetonitrile: methanol (1: 1, V / V); a gradient elution procedure; according to the method, the Fmoc-His (Trt)-OH and the related substances as well as the related substances can be effectively separated, the separation degree is greater than or equal to 1.5, the peak shape symmetry is better, the detection sensitivity of each related substance is high, the content (purity) detection result of each component is accurate and effective, and the quality of the Fmoc-His (Trt)-OH can be correctly reflected.

The invention discloses a high-purity column chromatography purification method of a burning rate catalyst Cartosin, and aims to solve the problems of low purity and high HPLC (High Performance Liquid Chromatography) cost in the traditional method. According to the method, 200-300-mesh silica gel is used as a stationary phase for wet column packing, a Cartosin crude product is dissolved in a low-polarity solvent for sample loading, and a silica gel column is obtained; a mixed solvent composed of a non-polar solvent and a polar solvent is adopted as an eluent for gradient elution, a target fraction is monitored and collected through TLC, and then a product is obtained through rotary evaporation and vacuum drying; according to the method, the purity of cartosin can be increased from about 60% to 93.0% or above, equipment is simple, the cost is low, the process is stable, large-scale amplification from a laboratory to industrial production is easy, and the method is suitable for the requirement of a high-performance propellant.

The invention discloses a preparation method of an eruptoria paniculata polysaccharide for improving ulcerative colitis, and relates to the field of biological medicines. Comprising the following steps: S1, extracting crude polysaccharide, namely extracting the crude polysaccharide from a Rhododendron simsii raw material by adopting a water extraction and alcohol precipitation method; s2, impurity removal of the crude polysaccharide: removing impurities through enzymolysis, solvent treatment and adsorption; s3, ion purification: carrying out gradient elution purification by using an ion exchange column; s4, gel purification: further purification is performed through a gel chromatographic column, and the polysaccharide component HBP-1 of the hedyotis diffusa is obtained; the step S1 specifically comprises the following steps: S11, crushing and sieving the raw materials of the seedlings, and extracting fat-soluble impurities by using absolute ethyl alcohol; and S12, after water extraction, centrifugally collecting supernate, concentrating and carrying out alcohol precipitation to obtain crude polysaccharide. The method is simple, efficient and suitable for industrial production, and a new potential drug source is provided for treatment of ulcerative colitis.

A method for determining multi-characteristic components of ASDZW is provided. By optimizing the gradient elution program of high performance liquid chromatography (HPLC), strictly controlling the initial mobile phase ratio of the gradient elution program, cooperating with the selections of the chromatographic column and the mobile phase, the invention finally realizes the simultaneous, rapid and comprehensive determination of six characteristic components in ASDZW under the condition of a single wavelength; specifically, the six characteristic components are polygalaxanthone III, 3,6′-disinapoyl sucrose, ginseng saponin Rb1, β-asarone, dehydrotumulosic acid, and pachymic acid. The whole detection process is a single wavelength detection with high detection efficiency and short analysis time, and the detection limits of the six components are lower than 0.008 μg / mL, meaning this method has high sensitivity, good specificity, accurate results, and good reproducibility.

The invention discloses a method for detecting related substances in testosterone enanthate by high performance liquid chromatography. A mobile phase A and a mobile phase B are used as mixed mobile phases for gradient elution; the mobile phase A is water; the mobile phase B is acetonitrile; the volume ratio of the mobile phase A to the mobile phase B is (5%-70%): (30%-95%); a chromatographic column adopted by the high performance liquid chromatography method is Agilent ZORBAX Eclipse XDB-C8, and the detection method is characterized in that the detection method is simple and easy to implement. According to the method, the testosterone enanthate and the related substances thereof are separated and detected by screening a stationary phase chromatographic column and optimizing a mobile phase elution mode and an elution component ratio, and compared with a method in European Pharmacopoeia, after the chromatographic column is subjected to gradient elution, not only is the retention time of an impurity D prolonged, but also the quality of the impurity D is improved. And the separation degree of the impurity F and the impurity G is increased, so that the elution capacity and the separation degree among the impurities are enhanced.

The application discloses a kind of 10 kinds of antioxidants in medical device leachable determination method.The present application, by ultra-high performance liquid chromatography time-of-flight mass spectrometry technology realizes the simultaneous determination of ten kinds of antioxidants in medical device leachable, covers different types of antioxidants such as phenolic and phosphite.The pretreatment process only needs to extract the measured product, and the extracted liquid is blown dry by nitrogen, methanol is added, vortexed and filtered through microporous filter to complete the preparation of test solution, and the operation steps are simple, without complex derivatization or purification process, greatly reducing the difficulty and time cost of sample processing.In the analysis process, the ultra-high performance liquid chromatography system is used in conjunction with specific chromatographic column and mobile phase gradient elution program, which can quickly realize the baseline separation of ten kinds of antioxidants, combined with the high sensitivity detection of time-of-flight mass spectrometry, significantly improves the analysis efficiency, and is suitable for rapid screening and quantitative analysis of large quantities of samples.

The invention discloses a method for determining the content of 27-hydroxycholesterol in a biological sample, and relates to the field of biochemical analysis. Comprising steps as follows: sample pretreatment: 27-hydroxycholesterol in a biological sample is extracted with an organic solvent, and a deuterated internal standard 27-hydroxycholesterole-d6 is added for correction; liquid chromatography-mass spectrometry detection is carried out, and a gradient elution procedure and a multi-reaction monitoring mode are adopted in the liquid chromatography-mass spectrometry detection, so that the 27-hydroxycholesterol is specifically separated and detected; the content of the 27-hydroxycholesterol is calculated through an internal standard method in a quantitative analysis manner, the biological sample is a serum or tissue sample, and liquid chromatography conditions comprise that an ACQUITYUPLCHSST3 chromatographic column is used, a mobile phase A is an aqueous solution containing 0.1% of formic acid, and a mobile phase B is an acetonitrile solution containing 0.1% of formic acid. The method has the advantages of high specificity, high accuracy, high sensitivity, high flux and high economical efficiency.

The invention discloses a QuEChERS-high performance liquid chromatography determination method for diarrheogenic illegal additives in food, and the method comprises the following steps: step 1, taking 2.0 g of a food sample, adding 10 mL of an extraction solvent, carrying out vortex oscillation-ultrasonic treatment, then adding anhydrous magnesium sulfate and sodium chloride, carrying out vortex mixing, carrying out centrifugal treatment, and extracting a supernatant; 2, taking 5mL of the supernate, adding the supernate into a purification tube containing purification salt, carrying out vortex oscillation-centrifugal treatment, taking the supernate, and enabling the supernate to pass through a 0.45 mu m polytetrafluoroethylene microfiltration membrane, so as to obtain a solution to be detected; and 3, injecting the solution to be detected into a high performance liquid chromatograph, carrying out gradient elution by adopting a C18 chromatographic column and taking acetonitrile-water as a mobile phase at a flow rate of 1.0 mL / min, a column temperature of 30 DEG C, a detection wavelength of 210 nm and a sample size of 10 [mu] L, and quantitatively analyzing a target compound through an external standard method. The invention aims to obtain a method for detecting illegal additives in food, which is low in cost and high in detection efficiency.

The application discloses a fingerprint spectrum construction method of a Huahong composition, and comprises gradient elution and determination by a high performance liquid chromatograph; the high performance liquid chromatograph conditions are as follows: a chromatographic column is a reversed-phase C18 chromatographic column; a detection wavelength is 326 nm; and a mobile phase is that a mobile phase A is 0.1% formic acid aqueous solution, and a mobile phase B is methanol, and gradient elution is adopted. The UPLC fingerprint spectrum of the Huahong composition is established by optimizing chromatographic conditions and establishing a test product preparation methodology. The method is simple, accurate, and good in repeatability, and can better control the quality consistency of the Huahong composition.

The invention discloses a method for establishing a fingerprint spectrum of a diaphoresis and antipyretic preparation, which comprises the following steps: preparing a test solution, and carrying out high performance liquid chromatography detection on the test solution, the test solution is prepared by the following steps: adding 65-75% of methanol or ethanol into a diaphoresis and anti-pestilence preparation, and carrying out ultrasonic treatment; the high performance liquid chromatography detection adopts gradient elution, and the gradient elution procedure is as follows: 0-15 min, 6-12% A; 12% A is changed into 20% A, and 20%-22% A is changed into 20% A after 15 min to 45 min and 45 min to 65 min; when the time is 65-85 minutes, 22% A is changed into 70% A; the fingerprint spectrum of the diuresis and antipyretic granules established by the invention can be used for objectively, comprehensively and accurately evaluating the quality of the diuresis and antipyretic granules, and has important significance for controlling the quality of diuresis and antipyretic granules and ensuring the clinical curative effect.

The invention belongs to the technical field of vitamin content detection, and particularly relates to a method for measuring the content of various water-soluble vitamins B. The water-soluble vitamins B comprise vitamin B1, vitamin B2, vitamin B3, vitamin B6, vitamin B7, vitamin B12 and nicotinamide. A high performance liquid chromatograph and an electrospray detector are used as detection instruments, and chromatographic conditions are as follows: a mobile phase A is ammonium formate or ammonium acetate, a mobile phase B is methanol, and gradient elution is performed; the gradient elution procedure is as follows: a solvent of a test sample is a mixed solution of acetonitrile, water and glacial acetic acid, and the volume ratio of the acetonitrile to the water to the glacial acetic acid is 5: 95: 0.5; the atomization temperature of the electrospray detector is 35 DEG C; the method is better in separation degree and higher in specificity and sensitivity.

The application discloses a separation and detection method of methoxy PEG derivatives and methylsulfonyl PEG derivatives, which comprises the following steps: mixing a sample to be detected, ammonia and an ammonium salt catalyst, carrying out a derivatization reaction to obtain a derivative product, and detecting the derivative product by using a liquid chromatography method. The sample to be detected is a methoxy PEG derivative or a methylsulfonyl PEG derivative sample. In the method, the stationary phase of the chromatographic column is octadecylsilane bonded silica gel, the mobile phase A is a 0.01-5% formic acid aqueous solution in terms of volume percentage concentration, the mobile phase B is acetonitrile and methanol in a volume ratio of (1-5):1, a gradient elution program is adopted, and an electrospray detector is used. The method can effectively separate and quantitatively analyze the methoxy PEG derivatives and the methylsulfonyl PEG derivatives, and the method is completely in line with the standards and performs well in the quantitative limit, the linear range, the accuracy and the like, thereby providing an effective guarantee for subsequent product quality control or evaluation.

The invention discloses a method for detecting the content of formaldehyde in polyethylene glycol 400, and relates to the technical field of detection. The invention relates to a method for detecting the content of formaldehyde in polyethylene glycol 400, which comprises the following steps: S1, precisely weighing 4-(3-methylphenyl)-2H-pyridine [4, 3, e]-1, 2, 4-thiodiazine-1, 1-dioxo, and adding methanol to dissolve the 4-(3-methylphenyl)-2H-pyridine [4, 3, e]-1, 2, 4-thiodiazine-1, 1-dioxo to prepare a reference solution; s2, precisely weighing polyethylene glycol 400 and reactants to prepare a test solution; and S3, respectively detecting the test solution and the reference solution by adopting a high performance liquid chromatography, and calculating the content of formaldehyde in polyethylene glycol 400, wherein the chromatographic conditions of the high performance liquid chromatography are as follows: gradient elution is adopted; a chromatographic column is characterized in that octadecylsilane chemically bonded silica is used as a stationary phase; the mobile phase comprises a first mobile phase and a second mobile phase, the first mobile phase is a buffer solution, and the second mobile phase is an organic solvent. The method provided by the invention can accurately measure the content of formaldehyde in polyethylene glycol 400.

The invention relates to the technical field of biotechnology, enzyme engineering and biological pharmacy, in particular to a ribonuclease purification production method. According to the method, a deep sea antifreeze polypeptide and rare earth nanocrystal composite bionic system is constructed, quorum sensing signal molecules and a pulsed electric field are introduced in a fermentation stage for two-factor regulation, and a light-operated micro-fluidic chip selective extraction technology is combined, so that efficient separation of target enzyme is realized. A double-ligand magnetic microsphere chromatographic column is innovatively adopted for gradient elution, and the enzyme activity retention rate and the long-term storage stability are remarkably improved through thermotropic liquid crystal capsule stabilization and radio frequency assisted freeze drying processes. According to the invention, the destructiveness of the traditional chromatography technology to enzyme conformation is broken through, the problem of batch fluctuation caused by multi-step purification is solved, a ribonuclease product with high purity, high activity and environmental response characteristic is provided for the field of biological medicine, and the ribonuclease is especially suitable for industrial preparation of gene therapy products and virus vectors.

The invention provides a quality detection method of heart-nourishing pulse-activating granules, a fingerprint spectrum and a construction method of the fingerprint spectrum, and relates to the technical field of medicine detection. The quality detection method comprises the following steps: preparing a test solution: weighing heart-nourishing and pulse-activating granules, adding a methanol aqueous solution with the volume fraction of 25%-100%, dissolving, carrying out ultrasonic treatment, and filtering; a reference substance solution: weighing a salvianolic acid B reference substance, adding a methanol aqueous solution with the volume fraction of 25%-100%, dissolving into a solution with the concentration of 1 mg / mL, and filtering; respectively injecting the test solution and the reference solution into a liquid chromatograph, and measuring to obtain chromatograms; in the chromatographic column, octadecylsilane chemically bonded silica is used as a filling agent; an acetonitrile solution is used as a mobile phase A, and a phosphoric acid aqueous solution with a volume fraction of 0.05-0.15% is used as a mobile phase B; and gradient elution. According to the quality detection method provided by the invention, the effective components are extracted to the greatest extent, and relatively comprehensive effective component information is obtained.

The application discloses a method for simultaneously detecting 18 kinds of amino acids in Daqu based on high-resolution liquid chromatography-mass spectrometry, and belongs to the technical field of liquor detection. Chromatographic conditions of the method include that an ethylene bridge hybrid particle with surface-bonded amide groups is used as a filler, ammonium acetate-formic acid aqueous solution is used as mobile phase A, and acetonitrile is used as mobile phase B for gradient elution; mass spectrometry conditions include that an H-ESI ion source is used, the spray voltage in the positive ion mode is 3000-4000 V, and the spray voltage in the negative ion mode is 2000-3000 V; qualitative analysis is performed according to mass-to-charge ratios of the 18 kinds of amino acids, and quantitative analysis is performed by using a standard curve method. The method has the characteristics of simple pretreatment operation, easy-to-obtain reagents, high extraction efficiency and good stability, can realize synchronous and accurate qualitative and quantitative analysis of the 18 kinds of amino acids, and provides reliable data support for flavor substance research of Daqu.

The invention discloses a method for improving the detection recovery rate of ascorbyl palmitate in a compound product, which comprises the following steps: taking a sample, adding BHT (butylated hydroxytoluene), then adding an isopropanol-n-hexane mixed solution containing 0.8-1.2% by volume of glacial acetic acid as an extraction solvent, then fully mixing, extracting, freezing, centrifuging, taking supernate, and collecting the supernate to obtain the ascorbyl palmitate. The chromatographic conditions are as follows: a C18 reversed-phase chromatographic column is adopted, a mobile phase A and a mobile phase B are used for gradient elution, the flow velocity of the mobile phase is 0.8-1.2 mL / min, the column temperature is 28-32 DEG C, and the maximum absorption wavelength of ascorbyl palmitate is taken as the detection wavelength. According to the method, the extraction efficiency is improved by optimizing a sample pretreatment process, and the problem that the liquid phase detection error of the substance in the compound product is generally higher than 10% is effectively solved in combination with improved high performance liquid chromatography separation conditions.

The application belongs to the technical field of agricultural chemistry, and particularly relates to a naphthoquinone compound with anti-tobacco black shank disease activity and a preparation method and application thereof. The naphthoquinone compound is extracted from honeysuckle branches with high-concentration methanol, high-concentration acetone / water or high-concentration ethanol / water, the extract is combined, filtered, and concentrated into an extract under reduced pressure; the extract is subjected to silica gel column chromatography by dry column packing with silica gel; gradient elution is performed with chloroform-acetone solution; and the 7:3 part of the eluate is further separated and purified by high-performance liquid chromatography to obtain the required naphthoquinone compound. The application also discloses the application of the compound. The active test shows that the compound has a good inhibitory effect on tobacco black shank disease. The compound has a novel structure, good anti-black shank disease activity, and can be used as a lead compound for anti-tobacco black shank disease and for the research and development of anti-tobacco black shank disease biological pesticides.