805results about How to "Good peak shape" patented technology

The invention relates to a construction method of ganoderma spore powder polysaccharide fingerprint and a standard fingerprint of the ganoderma spore powder polysaccharide, belonging to the fingerprint technical field of the traditional Chinese medicine and products thereof and the functional food raw material and products thereof. The construction method in the invention comprises the following steps: extracting ganoderma spore powder polysaccharide; hydrolyzing a part of ganoderma polysaccharide; performing PMP derivatizing reaction on a part of the hydrolyzate of ganoderma polysaccharide; performing reversed phase HPLC fingerprint analysis and determining the standard fingerprint; performing the HPLC analysis on the polysaccharide fractions of ganoderma spore powder samples from fifteen different producing areas and comparing the fingerprints of the ganoderma spore powder samples to determine the common fingerprint characteristics so as to obtain a standard fingerprint. The fingerprint has nineteen common peaks in all, the sum of the peak areas of the common peaks accounts for 98% of the total peak area, and the peak area of each of four fingerprint peaks is more than 5% of the total peak area. The method in the invention is stable, has high degree of precision and good repeatability and is easy to grasp; and the quality situation and producing area of the ganoderma spore powder polysaccharide can be grasped from the overall characteristic of the chromatography, and a new scientific method for the quality control and identification of ganoderma spore powder can be provided.

The invention relates to a detection method for simultaneous determination of nine water soluble vitamins, during determination of water soluble vitamins by use of high performance liquid chromatograph (HPLC), a phosphate buffer-acetonitrile system with the concentration of 10-50mmol / L and pH of 2.0-3.0 is used as a mobile phase, dissociation of water soluble vitamin components can be effectively inhibited in order to increase the retention time of the water soluble vitamin components in a C18 chromatographic column stationary phase, and because of the concentration of the phosphate buffer system is 10-50mmol / L, the mobile phase has great buffer capacity, and when an acidic or alkaline sample is introduced into the chromatographic system, the pH value of the mobile phase can be maintained in no change so as to ensure the separation effect of the water soluble vitamins. The method can realize simultaneous determination of the nine water soluble vitamins, has the characteristics of fast speed, high sensitivity, accurate nature determination and quantification, and is suitable for multicomponent determination of the water soluble vitamins in vitamin nutrition fortified foods.

The invention provides a detection method for a fingerprint chromatogram of flavonoid and organic acid components in a ginkgo biloba extract. The detection method comprises the following steps: (1) preparing a test solution; (2) preparing a reference solution; (3) respectively determining the test solution and the reference solution by adopting high-performance liquid chromatography, and comparing the acquired fingerprint chromatogram with a standard fingerprint chromatogram to obtain the fingerprint chromatogram of the flavonoid and organic acid components in the test solution. The invention further provides the application of the detection method in the quality detection and the component test determination of the flavonoid and organic acid components in the ginkgo biloba extract. According to the detection method for the fingerprint chromatogram of flavonoid and organic acid components in the ginkgo biloba extract and the application of the detection method provided by the invention, the fingerprint chromatogram of flavonoid and organic acid medicinal components in the ginkgo biloba extract is established; the quality control level of the flavonoid and organic acid medicinal components in the ginkgo biloba extract is improved; effective quantitative analysis can be performed.

The invention discloses a method for simultaneously determining sweetening agents and preservatives in tobacco essence, and belongs to the technical field of chemical component detection of auxiliary materials for tobaccos. The method comprises the following steps that 1, a sample to be determined is diluted, the pH value of a solution is regulated to be 9-10, extraction is performed, extraction liquid is purified through an Oasis HLB column, and the purified extraction liquid is filtered for standby application; 2, filtrate is taken to be subjected to ion chromatographic analysis, and the content of the sweetening agents and the preservatives in the sample to be determined is calculated by contrasting a standard curve. According to the method, impurities disturbing determination in the essence are purified and removed in a classifying mode according to the physical and chemical properties of different types of the tobacco essence, one-time sample feeding is performed on the three sweetening agents (sodium cyclamate, acesulfame and saccharin sodium) and the two preservatives (sorbic acid and benzoic acid) through an AS17C analytical column and an electrical conductivity detector, and separation and determination are simultaneously performed. Compared with an industrially recommended determination method, the method has the advantages of being wide in linear range, low in quantitation limit, little in sampling quantity, high in determination efficiency and the like.

The invention discloses a method for establishing a lonicerae and forsythiae powder UPLC fingerprint spectrum.The method can quickly and accurately identify authenticity and merits of a product and has the advantages of simplicity, convenience, stability, high precision, good repeatability and the like.By means of the method, kinds and quantity of chemical components contained in lonicerae and forsythiae powder can be comprehensively reflected, global description and evaluation are conducted on the quality of the lonicerae and forsythiae powder, the quality and the medicine effects of the lonicerae and forsythiae powder are truly combined, which is conductive to illuminating the function mechanism of the lonicerae and forsythiae powder, and a basis is provided for technical promotion and deep development of the lonicerae and forsythiae powder.By means of the method, the number of the chemical components detected in the lonicerae and forsythiae powder fingerprint spectrum is relatively large, characteristic peak height proportions are moderate, a base line is stable, and the separation degree, peak shapes and column efficiency are good.

The invention provides a method for detecting trace phosphine gas in a water sample by a gas chromatograph (GC)-cooperating pre-column twice cold trap enrichment method, and aims to overcome the shortcomings of the existing various measurement methods. The method mainly comprises the following steps of: (1) cooling and enriching the phosphine gas and establishing a GC/NPD (nitrogen phosphorous detector) detection device; (2) extracting and dissolving the phosphine gas in lake water by a gas-liquid two-phase phase equilibrium method, and preparing a gas sample to be detected; (3) preprocessingthe gas sample; (4) extracting a certain volume of the gas sample into a gas absorption tube; (5) performing primary enrichment of the processed gas sample in a cold trap I, and removing the impuritygas with a relatively low boiling point; (6) heating the cold trap I so that the gas enters a cold trap II for secondary enrichment; (7) detecting the final enrichment product by a nitrogen phosphorous detector in a gas chromatograph through a chromatographic column; and (8) converting the measured area of a characteristic peak of the phosphine according to a certain formula to obtain the concentration of the phosphine in the water sample to be detected.

The invention belongs to the pharmaceutical field, and specifically relates to a preparation method and a detection method for edaravone dimers and tautomers thereof. The preparation method is characterized in that edaravone is dissolved in a solvent; a catalyst is added; the mixture is heated and filtered to obtain an insoluble substance; the substance is washed and dried to obtain a product. The detection method adopts a high performance liquid chromatography method. The preparation method of the invention has convenient operation and easily available initial raw materials, and the detection method is applicable to the detection of edaravone dimers in edaravone raw materials and preparation samples.

The invention discloses a high performance liquid chromatographic analysis method for pyromellitic dianhydride. The method comprises the following steps: (1) adopting chromatographic conditions, (2) preparing a mobile phase, (3) preparing a PMDA standard solution, (4) building a standard curve, (5) preparing a PMDA sample solution, and (6) carrying out quantitative analysis by using an external standard percentage method. The invention provides the method for quantitatively analyzing pyromellitic dianhydride, which fills the technological gaps of corresponding fields. The method has the advantages of simple sample treatment and analytical procedure process, good peak shape, high analysis result accuracy, good reproducibility and the like and has an important practical significance in the fields of quality analysis and quality control of PMDA.

The invention discloses a method for measuring formaldehyde and acetaldehyde content in paper for a cigarette at the same time, which comprises the following steps of: preparing a mixed standard stock solution; preparing a standard working solution; creating a standard working curve; preparing a derivatization reagent; preparing a sample solution; analyzing by ultra high performance liquid chromatography; and calculating a result. According to this method, a sample processing method and the chromatographic condition are improved and optimized, so that two compounds to be measured have good separation effect and good peak shape. A scanning operation is carried out by employing two wavelength channels at the same time, so that this method has obvious advantage in sensitivity in comparison with single wavelength measurement at the same time. The ultra high performance liquid chromatography is employed, so that analysis time is greatly shortened. The two compounds to be measured both have better chromatographic peak separation and better linear correlation, the detection limit of the formaldehyde is 0.57mg/kg and the detection limit of the acetaldehyde is 0.34mg/kg. In the method, the recovery rate of the formaldehyde is 98.14%, the recovery rate of the acetaldehyde is 97.55% and the average relative standard deviations of the formaldehyde and the acetaldehyde are both less than 2.5%.

The invention relates to an environmental analysis detection method, and specifically, relates to a high performance liquid chromatography determination method of tetracycline antibiotic in soil. The high performance liquid chromatography determination method of tetracycline antibiotic in soil comprises the following steps of 1, a sample collecting and preparation process comprising collecting soil in a plough layer having thickness of 0 to 20 centimeters, wherein soil in a composting place and field edges is not adopted, uniformly mixing multiple single-point samples, carrying out quarteringreduction to obtain a mixed soil sample having weight of about 1kg, putting the mixed soil sample into a sealing bag, bringing the sealing bag with the mixed soil sample back with low-temperature preservation in the dark, putting the mixed soil sample into a room, drying in air, crushing, screening by a nylon sieve of 60 meshes, and weighing 2g of the mixed soil sample for next use, 2, an extractpreparation process, 3, an extraction, purification and enrichment process, and 4, an elution, volume metering and detection process. The high performance liquid chromatography determination method of tetracycline antibiotic in soil has normalized processes, reduces a vacuum drying process, produces low jamming, shortens operation time and improves operation accuracy. Through connection between astrong anion solid phase extraction column and a C18 inverted solid phase extraction column in series, purification and enrichment effects are greatly improved.

The invention relates to the technical field of analytical chemistry and discloses a method for detecting afatinib dimaleate isomer and main degradation impurities through a high performance liquid chromatography.According to the method, afatinib dimaleate raw materials or preparations are compounded into a detection solution with diluent, bonding amylose-trichlorobenzene carbamic acid ester serves as a stationary phase, a normal hexane-ethanol-organic base solution serves as a mobile phase for isocratic elution, and an HPLC spectrogram is recorded under afatinib absorption wavelength.According to the method, a chromatographic column with trichlorobenzene carbamic acid ester serving as a filling material, the normal hexane-ethanol-organic base solution serves as the mobile phase, the content of isomers existing in afatinib dimaleate and preparations thereof can be measured quantitatively, afatinib, the isomers and the main impurities can be separated completely, the peak pattern is good, the method meets the specifications in Chinese Pharmacopoeia, quality of afatinib dimaleate and afatinib dimaleate preparation products is effectively controlled, and the method is great in specificity, high in sensitivity and good in accuracy.

The invention discloses a method for analyzing a night cold flu cough allergy capsule by utilizing HPLC (High Performance Liquid Chromatography). The night cold flu cough allergy capsule contains acetaminophen, phenylephrine hydrochloride, succinic acid doxylamine and dextromethorphan hydrobromide. In the HPLC analysis, an octadecyl silane bonded silica gel column is adopted as a chromatographic column; a sodium 1-octanesulfonate-phosphate buffer solution with the pH of 2.0-3.0 acts as a mobile phase A; acetonitrile and a mixed solution of acetonitrile and methyl alcohol act as a mobile phase B. The method can be simultaneously and effectively used for detecting four effective ingredients in the night cold flu cough allergy capsule, is simple to operate, analyzes rapidly, is good in repeatability, has favorable specificity, and can effectively and comprehensively control the product quality of the night cold flu cough allergy capsule.

The invention discloses a method for performing qualitation and quantification on triterpenoid saponin in traditional Chinese medicine by utilizing an electrospray protonation pyrolysis-mass spectrummulti-reaction detection mode. The triterpenoid saponin can form a stable [M+H]<+> and/or [M+NH4)<+> molecular ion peak in a flow phase containing formic acid or ammonium formate. According to the method disclosed by the invention, a liquid chromatogram-tandem quadrupole mass spectrometry combined instrument is utilized, an electrospray positive ion tandem mass spectrum detection mode is utilized,and mass spectrum parameters of declustering potential, impact energy, impact chamber injection voltage and the like can be quickly optimized in an online mode by a single factor and response surfacemethod; thus, high-strength triterpenoid saponin protonation pyrolysis MRM target ion pairs can be formed; a Q1 calculation formula is [M+H]<+> or [M+NH4]<+>, and a Q3 calculation formula is [aglycone +H-nH2O]<+>. By means of the series of characteristic MRM target ion pairs, the purpose of quick qualitative and quantitative detection on the triterpenoid saponin in the traditional Chinese medicine is realized. The method disclosed by the invention provides an effective technology method for the qualitative and quantitative detection on the triterpenoid saponin in the traditional Chinese medicine and has been successfully applied to content measurement on the triterpenoid saponin of caulophyllum robustum and aralia elata.

The present invention discloses a method for separating a liquid chromatogram of the amino acid contented in tobacco and the product thereof. The method comprises the procedures of preparing an extraction liquid of the sample to be measured; and taking an A phase 99%water-1%ethane nitrile-0.1%nonafluoro valeric acid and a B phase 10%water-90%ethane nitrile-0.1%nonafluro valeric acid as a flowing phase gradient for elution and separation on the HyPURITY C18 reverse-phase chromatographic column. Aiming at the disadvantage of the method for analyzing the content of amino acid contended in tobacco and the product thereof, the invention accurately limits the condition of the liquid chromatogram analysis and provides an integral and whole experiment plan for obtaining an excellent chromatographic peak shape and an appropriate color spectrum runtime. Furthermore, the isomeride of the amino acid can be facilitated to obtain a base line separation. The chromatogram separation method provided by the invention can obtain an accurate analyzing result to the content of the amino acid in tobacco and the product thereof when combined with a mass spectrometric detection.

The invention discloses a method for simultaneous determination of organic acids and flavone components in polygonum viviparum, wherein the method comprises the following steps: (1) preparing a test sample solution; (2) detecting with LC-MS/MS; and (3) carrying out component qualitative analysis. On the basis of qualitative analysis of the components of the polygonum viviparum, a reference substance solution is prepared, and the contents of chlorogenic acid and gallic acid in the polygonum viviparum are also determined. 10 kinds of substances in the two active components of the organic acids and the flavones in the polygonum viviparum are determined at the same time for the first time, and a quality control method of the polygonum viviparum medicinal material is improved. The LC-MS/MS analysis detection method is adopted to be combined with a multi-wavelength switching procedure, and the method has the advantages of being simple, stable, fast, high in efficiency, high in sensitivity, good in repeatability and low in interference, can complete the detection of 10 kinds of substances within 1 h, and obtains a chromatogram which can contain multiple pieces of wavelength information at the same time.

The invention provides a method for detecting phosphatidylcholine, which is used for determining the chemical composition and quantifying the phosphatidylcholine in yolk lecithin by using a method of using both high performance liquid chromatography and an ultraviolet detector. The method is characterized in that a silicagel column ZORBAX RX-SIL (4.6 mm X 250 mm, 5 microns) manufactured by Agilent is adopted as an analytical column and methanol/acetic acid is used as a mobile phase to carry out isocratic elution, and other elution conditions are an ultraviolet detection wavelength of 200 nm, a column temperature of 30 DEG C, a sample feeding quantity of 15 microliters and a flowing speed of 0.5 ml/min. The mobile phase of the method has the characteristics of binary system, simpler composition, lower flowing speed of 0.5 ml/min, faster peak time within 14 minutes and linear range of a phosphatidylcholine standard curve of 10-160 microgram/ml; the added 3.75% acetic acid solution improves a peak shape of the phosphatidylcholine and effectively inhibits serious tailing phenomenon; and the use cost of a solvent is saved. It is proved by a methodological replication experiment that the method has the advantages of high precision, good stability and higher accuracy.

The invention discloses a research for realizing quick classification and identification of chemical components in an ixeris sonchifolia hance injection based on a UPLC-Q-TOF-MS technology, and aims to take flavonoids, organic acids, amino acids and nucleosides in the ixeris sonchifolia hance injection as research objects to realize quick classification and identification of the chemical components in the ixeris sonchifolia hance injection based on a UPLC-Q-TOF-MS technical platform. The research comprises the following steps: firstly, performing information integration on components of flavonoids, organic acids, amino acids and nucleosides in the ixeris sonchifolia hance injection to discover and summarize a rule for diagnosing fragments and neutral losses of the four types of substances; meanwhile, performing mass spectrographic analysis on reference substances of different types of compounds by adopting the UPLC-Q-TOF-MS technology, and performing verification; and constructing a method for realizing quick classification and identification of chemical components in the ixeris sonchifolia hance injection by using a method for diagnosing fragments and neutral losses as a screening and identifying tool.

The invention relates to a quality control method of rhizoma gastrodiae, a decoction piece thereof and rhizoma gastrodiae extract. Based on high-performance liquid chromatography, by the aid of a one-standard multi-measurement analysis method, the contents of gastrodin components of gastrodin, p-hydroxybenzyl alcohol, parishin A, parishin B, parishin C and parishin E in the rhizoma gastrodiae arecalculated by relative correction factors, the low-cost gastrodin with stable property serves as an internal standard substance, and six effective components in the rhizoma gastrodiae are simultaneously measured. The multi-index quality control method is high in detection sensitivity, rapid in analysis and good in stability, can objectively, comprehensively and accurately evaluate the quality of the rhizoma gastrodiae, the decoction piece thereof and the rhizoma gastrodiae extract, is of great significance for ensuring the curative effect of the rhizoma gastrodiae and can solve the problems that parishin component reference substances are unstable, high in price and the like, and the quality of the rhizoma gastrodiae, the decoction piece thereof and the rhizoma gastrodiae extract cannot becomprehensively controlled.

The invention provides a method for determining trace low-valent phosphate in natural water. The determination detection limit of the method on low-valent phosphate reaches 10<-3> micrometers, which is sufficient to meet the detection requirement for low-valent phosphate in natural water, while the detection limit of existing domestic determination methods for low-valent phosphate is about 0.5 micrometers. Compared with other detection methods, the method of the invention has the advantages of high sensitivity, low detection limit, rapid pretreatment, and simplicity. The specific determining steps of the method include: A. off-line pretreatment; and B. gradient elution. After various negative ions in a water sample to be determined are separated by a separation column, the elution solution and the sample enter an ASRS suppressor and are inhibited to lower background noise, and finally enter a conductance cell for detecting the conductivity of ions in the sample. The Chromeloen 6.5PS2 workstation can draw a spectrum according to the conductance signals received by a data collection system, and a chromatographic workstation is employed to automatically record the area of a characteristic peak, then the actual concentration of low-valent phosphate in the sample can be calculated according to a formula.

The invention discloses a method for determining glucose, fructose and saccharose in tobacco essence perfume through a high performance liquid chromatography/differential refraction detector. The method comprises the following steps: dissolving a sample through 0.01 mol/L of caustic soda solution to be constant volume; adopting a cation exchange chromatography column, which takes highly cross-linked lead type sulfonated styrene-divinylbenzene (SDVB) resin as a filler, as a separation column; using pure water as a moving phase to carry out isogradient elution; detecting through the differential refraction detector; using an external standard method for quantification; and computing contents of the glucose, the fructose and the saccharose. The method has favorable linearity with correlation coefficient being greater than 0.999, recovery of 97.1 percent-102.4 percent, within-day precision being less than 1.2 percent, day to day precision being less than 3.0 percent, detection limit being lower than 1.8mug, and good sensitivity, and is suitable for analyzing and determining the glucose, the fructose and the saccharose for various tobacco essence perfume samples.

The present invention provides a bisamide-containing novel liquid chromatographic media and method of synthesizing the same. A novel polar bisamide functional group, which can form hydrogen bonds or ion pairs with residual silanols on the surface of silica gel, is used as the bonded phase on the surface of silica gel to better shield the activity of silanols and to eliminate the influence of residual silanol groups. Compared with conventional C18 columns, these novel bonded phases have different selectivity; they can work not only in 0 to 100% water but also in 0 to 100% organic mobile phase. In particular, they exhibit good peak shapes and resolutions for polar and basic compounds and have good stability within a very wide pH range. These properties make the new stationary phases a useful complement to conventional C18 columns for a variety of HPLC applications.