33 results about "Fast protein liquid chromatography" patented technology

The invention discloses a method for detecting estrogen, nonyl phenol, octyl phenol and bisphenol A in water body sediment based on an accelerated solvent extraction (ASE), liquid-liquid extraction (LLE) and liquid chromatography / tandem mass spectrum (LC / MS / MS) technology. The method comprises the following steps of: performing accelerated solvent extraction by using acetone as an extracting agent to extract the estrogen, the nonyl phenol, the octyl phenol and the bisphenol A in the water body sediment; dissolving residues generated after extract is blown by nitrogen by using 1mol / L sodium hydroxide solution, performing centrifugal collection on the supernate, and performing liquid-liquid extraction by using ethyl acetate under the condition that the pH is equal to 2; and performing concentration detection by using a 3200QTRAP type liquid chromatography / tandem mass spectrometer and an Agilent 1100 high performance liquid chromatography system of American Applied Biosystem Company and an automatic sample injector of American Agilent Company. The recovery rate is 59 to 94 percent, and the detection limit is 0.04ng / g.

An ultrahigh-pressure dual on-line solid phase extraction / capillary reverse-phase liquid chromatography (DO-SPE / cRPLC) system is provided. The system comprises: a sample loading valve into which a first solvent and a sample to be analyzed are loaded; a first column valve in flow communication with a first solid-phase extraction column and a first reverse-phase liquid chromatography column; a second column valve in flow communication with a second solid-phase extraction column and a second reverse-phase liquid chromatography column; a column-switching valve for determining whether the sample is transferred to either the first column valve or the second column valve; a solvent selection valve in flow communication with the first and second column valves to supply the first solvent or a mixed solvent of the first solvent and a second solvent to the first and second column valves; a second solvent loading valve, in flow communication with a solvent mixer, into which the first and second solvents are loaded; a supply pump for loading the second solvent into the second solvent loading valve; and a supply pump for loading the first solvent into the sample loading valve, the second solvent loading valve and the solvent selection valve. The system requires minimal time (i.e. dead time) for column equilibration between successive experiments to shorten the total time required for the experiments by a factor of about two. In addition, the system enables rapid sample injection, on-line sample desalting and sample enrichment. Furthermore, the system is highly reproducible in terms of liquid chromatography (LC) retention time and can be operated at a pressure as high as 10,000 psi.

The invention provides a detection method of a carbostyril drug residue in a veterinary drug. The method comprises the following steps of: determining the carbostyril drug residue in the veterinary drug by means of liquid chromatography-tandem mass spectrometry; firstly, sampling a standard working liquid and a sample solution in a set liquid chromatography-tandem mass spectrometry condition; judging whether the sample contains corresponding detected objects or not, wherein the following conditions need to be met: a mass chromatographic peak retaining time in the sample solution is consistent to a mixed matrix standard working liquid with the allowable deviation of being smaller than + / -2.5%; and if the relative abundance of the set mass spectrum qualitative ions of the drug corresponding to the chromatographic peak is consistent to the relative ion abundance of the matrix standard working liquid equivalent in concentration, and the relative abundance deviation does not exceed the set specification, determining that the drug is contained. During pre-treatment of the sample by the method, the purifying process is cancelled, and the method has the characteristics of being simple in processing program, quick and high in determining accuracy rate and the like. Analyzed from a veterinary drug source, the medicinal safety of breeding industry is effectively ensured, and the animal food safety is improved.

The invention discloses a preparation method for quickly separating plant proanthocyanidin dimer and trimer. The method comprises the following steps: performing liquid-liquid extraction on an alcohol solution rich in plant proanthocyanidin raw material, and then flowing by a gel column, performing FPLC (Fast Protein Liquid Chromatography) or HSCCC (High Speed Counter Current Chromatography) separation, thereby separating and acquiring the proanthocyanidin dimer and trimer components. The technology disclosed by the invention is suitable for the separation and purification of the proanthocyanidin dimer and trimer from different resources and has universality. The proanthocyanidin dimer and trimer acquired according to the preparation method disclosed by the invention are higher in purity. The method has the advantages of high safety, simple operation, less time consumption, low production cost, environmental protection, reaching green chemical standard, suitability for industrial production and ultrahigh commercial value.

The invention discloses a separation and analysis method based on non-aqueous reverse-phase gradient liquid chromatography. Methanol, dichloromethane and triethylamine are taken as mobile phases, a gradient elution mode is adopted, circular and linear oligomers and homologs thereof of a Chimassorb 944 product are separated for the first time, and the molecular weight of the Chimassorb 944 product is identified through MALDI-TOF; by combining with the synthetic route of the Chimassorb 944 product, it is determined that chromatographic peaks of a liquid chromatogram stand for different types of the oligomers with the molecular weights with one constitutional unit deviation and the homologs thereof, attribution is conducted on the peaks, and an effective detection method for the mass control of the Chimassorb 944 product is provided. According to the hindered amine light stabilizer mass control and / or identification detection method, instruments used in the method adopt an ordinary reverse-phase chromatographic system, the operability is strong, and important economic value is achieved by applying the method to the measurement and the product mass control of the Chimassorb 944 product.

An exemplary multimodal chromatographic medium of the invention includes one or more strong anion exchange, weak anion exchange, strong cation exchange and / or weak cation exchange binding sites in combination with one or more reverse phase and / or hydrophilic interaction chromatography binding site. In an exemplary embodiment, the sites interact with one or more glycans in a mixture of glycans in a manner that allows separation of glycans in the mixture and analysis of the glycan mixture. The media are incorporated into devices and systems for chromatographic analysis. Also provided are methods of using the multimodal media of the invention to analyze glycans.

The invention discloses a bactrocerin, and a preparation method and an application thereof. The bactrocerin is a polypeptide separated from pupas of Bactrocera dorsalis, the molecular weight is 2.3 Dalton, the isoelectric point is 11.43, and the amino acid sequence of the bactrocerin is represented by SEQ ID NO:1. The invention also discloses the preparation method of the antimicrobial peptides of the bactrocerin. The method comprises the following steps: inducing the pupas of Bactrocera dorsalis with a mixed bacterial liquid, carrying out tissue homogenization to obtain a crude extract, and carrying out ion exchange chromatography, reversed phase fast protein liquid chromatography and reversed phase high pressure liquid chromatography purification on the crude extract to prepare the bactrocerin. The bactrocerin has an inhibition effect on Gram-positive bacteria, Gram-negative bacteria and fungi, has no hemolytic activity, can be used as a raw material for developing biotechnological products for preventing pathogenic organism infection of humans and animals, and also can be used in transgenic plants and transgenic animal breeding as an anti-disease gene through transgene and other biotechnologies.

The invention discloses a preparation method for quickly separating plant proanthocyanidin dimer and trimer. The method comprises the following steps: performing liquid-liquid extraction on an alcohol solution rich in plant proanthocyanidin raw material, and then flowing by a gel column, performing FPLC (Fast Protein Liquid Chromatography) or HSCCC (High Speed Counter Current Chromatography) separation, thereby separating and acquiring the proanthocyanidin dimer and trimer components. The technology disclosed by the invention is suitable for the separation and purification of the proanthocyanidin dimer and trimer from different resources and has universality. The proanthocyanidin dimer and trimer acquired according to the preparation method disclosed by the invention are higher in purity. The method has the advantages of high safety, simple operation, less time consumption, low production cost, environmental protection, reaching green chemical standard, suitability for industrial production and ultrahigh commercial value.

According to the method disclosed by the invention, under the same liquid chromatography condition, an aspartame and alitame mixed standard solution and the aspartame and alitame mixed standard solution added with a to-be-tested solution are injected to a liquid chromatograph respectively, qualification is carried out based on whether component signals are increased or not under the same retentiontime condition, and whether alitame or aspartame is contained in a to-be-tested food is judged; and comparison between the peak appearance signal of the mixed standard solution with the peak appearance signal difference of the mixed standard solution added with the to-be-tested solution is carried out for quantification, and the contents of the alitame and the aspartame are measured. The method is high in working efficiency, low in cost, less in interference and high in accuracy.

The invention relates to a liquid chromatography-tandem mass spectrometry test method of wilforlide, triptonide, triptolide and tripterine. The test method includes the following steps: taking liquid samples or tissue samples, cutting into pieces and placing into a tube with a stopper; adding a certain amount of a sodium hydroxide solution into the samples to adjust the pH to be 9-10, adding ethyl acetate, oscillating for 10 minutes, and performing high speed centrifugation for 10 minutes; after separation of an organic phase, adding an organic solvent for secondary extraction, mixing the two obtained organic phases, and placing on a concentrator with the temperature of 50 DEG C for evaporation until the organic phases are dried; using an initial mobile phase to dilute the residue, enabling the obtained solution to pass through a 0.22-[um]m microporous organic membrane, and taking the filtrate for analysis by a liquid chromatography-tandem mass spectrometer. The test method provided by the invention is simple, efficient, quick, sensitive, high in accuracy and extensive in practicability, can be applied to qualitative and quantitative testing for wilforlide, triptonide, triptolide and tripterine in biological samples, and is suitable for tests on in-vitro samples and suspicious physical evidences.

The invention relates to a matrine liquid chromatographic determination method in the chemical detection technical field. The method comprises the following steps: respectively diluting a matrime sample and a matrime reference substance with methanol to volume, taking aqueous solution containing the methanol, phosphoric acid and triethylamine as a mobile phase and injecting into a liquid chromatograph, and then sequentially determining precision, 24h stability, reproducibility and recovery rate of the matrine sample. The determination method has the advantages of simple operational steps, strong adaptability and good reproducibility of analysis results.

The invention provides an anti-salt liquid chromatogram and electro-mist mass spectrometry combined interface device. The device mainly comprises a liquid phase mist generation module, a rotary barrier piece module, a probe high-voltage make-and-break module and a power module, the rotary barrier piece module comprises an insulating part and a barrier piece, one end of the insulating part is fixedly connected with the barrier piece, and the barrier piece is composed of barrier blades and barrier piece notches; one end of the probe high-voltage make-and-break module is connected with high voltage, and the other end of the probe high-voltage make-and-break module is connected with a conducting probe. According to the anti-salt liquid chromatogram electro-spray mass spectrometry combined interface device, by selecting the barrier piece notches of different sector angles or adjusting the rotation speed of the power module, the sampling capacity (the sampling quantity is generally several nano-liters) of the PESI conducting probe is satisfied, and combination of the liquid phase and the mass spectrum (PESI) is achieved. Meanwhile, the sharp end of the conducting probe generates electro-mist, so that unionized salt is deposited on the surface of the conducting probe, the problem that a high-salt sample access is blocked due to salt deposition is avoided, the detection sensitivity of the mass spectrum for a target compound in a high-salt base material is enhanced, and the liquid chromatogram and mass spectrometry coupling technology of a high-salt sample is achieved.

The invention relates to a method for determining synthesized intermediate and product in wastewater in TATB production by liquid chromatogram, belonging to the technical field of chemical analysis. The method comprises the following steps: firstly, preparing standard solutions of phloroglucinol, TETNB and TATB standard substances by using liquid phase chromatogram mobile phase; secondly, treating the TATB wastewater, regulating pH to be neutral, extracting to-be-detected substance, drying the to-be-detected substance, adding the liquid phase chromatogram mobile phase for dissolving, filtering through a microfiltration membrane to remove impurity to obtain a liquid phase chromatogram detection sample; thirdly, performing liquid phase chromatographic analysis on the standard solutions, and drawing a standard curve; and fourthly, respectively analyzing the samples by using the liquid phase chromatogram, comparing the analysis result with the standard curve to determine the intermediate and the product in the TATB wastewater. Trace amount of intermediate related substances, such as phloroglucinol, TETNB and the product, namely TATB in the TATB wastewater can be accurately detected by using the method disclosed by the invention, and the defects in the prior art are filled.

The invention discloses a separation and purification method of c-di-GMP (cyclic diguanylate), comprising the following steps of: directly sampling a c-di-GMP crude product solution on a fast protein liquid chromatography equipped with an ion exchange chromatographic column; carrying out gradient elution by using a buffer solution with pH of 8.0; carrying out detection under 254 nm by an ultraviolet detector; collecting an eluent in the peak position; confirming a structure by using a mass spectrum; and freeze-drying the eluent with target compounds, thereby obtaining the solid c-di-GMP. The c-di-GMP prepared according to the method provided by the invention has the purity of over 95% through reversed-phase high performance liquid chromatography detection, and realizes c-di-GMP separation and purification from the c-di-GMP crude product solution in one step; moreover, the method provided by the invention has simple technology, short period and nonuse of toxic organic solvents, and is a novel method with high efficiency, environment friendliness and suitability for industrialized production.

Methods of making functionalized support material are disclosed. Functionalized support material suitable for use in chromatography columns or cartridges, such as in a high pressure liquid chromatography (HPLC) column or a fast protein liquid chromatography (FPLC) column, is also disclosed. Chromatography columns or cartridges containing the functionalized support material, and methods of using functionalized support material, such as a media (e.g., chromatographic material) in a chromatography column or cartridge, are also disclosed.

The present invention relates to a high performance liquid chromatography method for polypeptide mixtures. Specifically, the method including the following steps: step (1): preparing a solution of the glatiramer acetate to be tested; step (2): performing gradient elution on a sample to be tested with an anion exchange liquid chromatography, a cation exchange liquid chromatography, or a reversed-phase liquid chromatography; step (3): determining a peak area corresponding to each component of the glatiramer acetate, comparing the peak area with to a peak area of a reference substance to determine whether the content of each component of the sample to be tested is in a qualified range.

The embodiment of the invention provides a method for detecting 25(hydroxyl)vitamin D by using a high-pass liquid chromatography-tandem mass spectrometry. The method comprises the following steps of: adding an acetonitrile solution containing an internal standard substance of the 25(hydroxyl)vitamin D into a human serum sample to carry out protein precipitation; sufficiently and uniformly mixing the solution, and then, adding an n-hexane extracting solvent; sufficiently and uniformly mixing the solution, then centrifuging the solution, movably taking a supernatant and drying the supernatant, and adding a complex solution to obtain a sample to be detected; detecting the sample to be detected by using a high-pass liquid chromatography-tandem quadrupole mass spectrometer; and quantifying according to the relative retention time of 25(hydroxyl)vitamin D2 and / or 25(hydroxyl)vitamin D3 and the detected abundance ratio of quantitative ion pairs by using an internal standard curve method. According to the embodiment of the invention, the method has the advantages of simplicity in pretreatment, strong specificity and matrix interference resistance, short detection time, high pass, high detection precision and low cost.