156results about How to "The pretreatment method is simple" patented technology

The invention provide a ultra-performance liquid chromatogram-mass spectrum detection method for 23 types of drugs and mental disease resistant drugs in blood. The method comprises the following steps: 1) sample processing: employing an organic solvent for processing a sample through protein sediment; 2) primary screening detection: employing a ultra-performance liquid chromatogram-tandem mass spectrum (UPLC-MS/MS) multi-reaction monitoring (MRM) mode for primary screening detection; and 3) employing the ultra-performance liquid chromatogram-tandem mass spectrum (UPLC-MS/MS) multi-reaction monitoring (MRM) mode for reinspection of the positive sample through the primary screening in the step 2). According to physical and chemical properties of 9 types of drugs and 14 types of mental disease resistant drugs, during reinspection, the UPLC-MS/MS detection condition which is different with the primary screening detection is employed, different sample pretreatment methods are employed, so that the detection method can satisfy the rapid, sensitive and accurate requirements of primary screening detection, and misjudgement of false positive results can be reduced.

The invention discloses a callicarpa nudiflora medicine, an intermediate and a fingerprint detection method of a preparation. The method comprises the following steps: (a) preparation of a reference solution; (b) preparation of a test solution; (c) chromatographic condition; (d) formulation of a standard fingerprint of isoacteoside as a reference peak; and (e) quality control of the fingerprint. According to the above method, a pretreatment method of each tested object is simple, characteristic constituents are retained completely, stability is good, precision is high, and there is certain specificity. The separation effect of each characteristic peak in the fingerprint is good. The callicarpa nudiflora medicine, the intermediate and the fingerprint of the preparation have good correlation. The method can be used for identifying quality of the callicarpa nudiflora medicine and increasing production process controllability of the callicarpa nudiflora preparation, and is helpful for guaranteeing quality stability and clinical efficacy of the callicarpa nudiflora preparation. The invention also discloses the callicarpa nudiflora medicine obtained according to the above fingerprint detection method, the intermediate and the standard fingerprint of the preparation.

The invention discloses a kit and method for quantitatively detecting five fat-soluble vitamins in blood plasma. The kit comprises a fat-soluble vitamin calibrator, an isotope mixed standard substance, a fat-soluble vitamin quality control substance, an instrument quality control substance and a mobile phase additive. According to the invention, a solid-phase support liquid-liquid extraction method is adopted and is matched with an automatic pipetting station, so a sample pretreatment method is greatly simplified, and the aim of simultaneously and accurately detecting the five fat-soluble vitamins at high flux and high speed is fulfilled by combining a liquid chromatography-tandem mass spectrometry method. According to the invention, during the detection of a peripheral blood plasma sample, five fat-soluble vitamins can be quantified at a time only by about 250 microliters of plasma sample; moreover, due to a fact that the pretreatment method is simple and quick, the operation time issaved, the content of the fat-soluble vitamins in a human body can be effectively diagnosed and detected according to the indexes, and diseases caused by lack or excess of the fat-soluble vitamins canbe prevented and diagnosed in time. Therefore, the kit and method have extremely high application values in clinical, health examination and scientific research.

The invention provides a method for detecting fish parvalbumin through liquid chromatography tandem mass spectrometry. The method comprises the following steps: step 1: choosing a characteristic peptide fragment; step 2: making a standard curve: taking the concentration value of a quantitative peptide fragment standard product as the x-coordinate and a quantitative daughter ion peak area as the y-coordinate to draw the standard curve, and obtaining an equation; step 3: processing and implementing enzymolysis on a to-be-detected fish meat sample to obtain a liquid supernatant, implementing HPLC-MRM-MS/MS detection on the liquid supernatant, obtaining the daughter ion peak area of the quantitative peptide fragment in the fish meat sample, resolving the concentration of the quantitative peptide fragment in the sample, and further obtaining the concentration of the parvalbumin in the sample. The invention aims at establishing a liquid chromatography tandem mass spectrometry method, and themethod has the advantages of accuracy, precision, sensitivity and the like.

The invention provides a method which takes HepG2 cells as testing cells and carries out an exposure treatment experiment of pollutants. The method comprises the following steps: (a) establishing a pre-treatment method for rapidly extracting intracellular and extracellular metabolic products; (b) carrying out panoramic analysis and target analysis on the metabolic products of the cells by using a UPLC-QTOF and HPLC-MS/MS; (c) classifying and screening high-flux metabolites by statistical analysis; and (d) analyzing a high-attention metabolism path of organic pollutant influenced cells by combining a metabolism flow analysis system and a path analysis technology. The pre-treatment method is simple; the UPLC-QTOF is combined with the HPLC-MS/MS so that the intracellular and extracellular metabolic products of the cells can be effectively analyzed; and the high-attention metabolism path of the organic pollutant influenced cells can be directly analyzed by combining statistical treatment, metabolism flow analysis and metabolism path analysis; and the method has the advantages of simplicity in operation, short analysis time, good repeatability, capability of acquiring comprehensive information quantity and the like.

The invention discloses a chemiluminescent enzyme-linked immunosorbent assay kit of a tenuazonic acid and an application method thereof, and belongs to the technical field of chemiluminescent enzyme-linked immunosorbent assay. An indirect competition method is adopted by the assay kit; the kit comprises a chemiluminescent ELISA (Enzyme-Linked Immuno-Sorbent Assay) plate coated with tenuazonic acid antigens, a tenuazonic acid standard substance, tenuazonic acid antibodies, enzyme-labeled antibodies, a chemiluminescent liquid and a washing liquid. The application method of the kit comprises the following steps: (1) pretreating a sample to be detected; (2) orderly adding the solution or sample of the tenuazonic acid standard substance and the tenuazonic acid antibodies, and adding the enzyme-labeled antibodies after a competing reaction, and finally adding the chemiluminescent liquid to carry out the quantitative determination of the tenuazonic acid through a chemiluminescent immunoassay analyzer; (3) processing and analyzing the results. The chemiluminescent enzyme-linked immunosorbent assay kit of the tenuazonic acid provided by the invention is high in sensitivity, good in stability and suitable for screening of lots of samples, and thus has enormous practical application and popularization significance.

The method comprises: synthesizing the hapten 2-methyl-3-phenyl benzyl succinic acid ester (for short: LBC) and the 2-methyl-3-phenylbenzene benzoic acid (for short: LBY); coupling the LBc with protein to prepare the artificial immunity antigen and immunity rabbit to the specificity polyclonal antibody of Bifenthrin; coupling the LBy with the protein to prepare the envelope antigen; using the synthesized envelope antigen and specificity antibody to establish the enzyme immunoassay EIA analysis method; the detection range of the Bifenthrin can reach 0.016mg/L, and the linear range of it is 0.01-50mg/kg.

The invention discloses a detecting method for hexavalent chromium in gelatin and products thereof, particularly relates to the detecting method for the hexavalent chromium in colored gelatin products. The method includes the following steps: using phosphate buffered solution to extract; adjusting PH value of the extraction solution to >=12.5; directly adding graphitized carbon black powder in the extraction solution with colorant for purification and decoloration; in acid medium, hexavalent chromium oxidation diphenyl carbonyl two hydrazine forms soluble amaranthine compounds. The ultraviolet spectrophotometry method is adopted to detect the content of the hexavalent chromium. The detecting method has the advantages that under the condition of highly alkalinity, the recovery rate of the hexavalent chromium can be guaranteed. Moreover, the graphitized carbon black powder can carry out sufficient decoloration for pigment in samples and avoid color interference. The detecting method is high in recovery rate, simple in pretreatment, low in cost, quick and accurate in result.

The invention discloses a fingerprint map detecting method of radix astragali drug, intermediate compound and a preparation thereof, the method is as follows: taking onocol as reference substance, obtaining each sample solution through the processes of extracting/ dissolving, determining constant volume and the like, performing HPLC detection under the condition of the same chromatogram, performing gradient elution, recording a chromatogram map, and obtaining the product. In the method, the preliminary treatment method for each sample is simple, the reservation of the characteristic components is complete, the sample solution is stable; the precession is high, reproduction quality is good, and the solution has a certain specificity; the separation effect of each characteristic peak in the obtained fingerprint map is good, the fingerprint map of the radix astragali drug, intermediate compound and the preparation has better correlation; the method can be used for identifying the fake of the radix astragali drug, increases the controllability of the production process of the radix astragali preparation, and is in favour of ensuring the quality stability and the clinical healing efficacy of the radix astragali preparation. The invention also discloses a standard fingerprint map of radix astragali drug, intermediate compound and preparation thereof obtained by the fingerprint map detecting method.

The invention relates to a method for monitoring environmental element pollution by transplanting fresh water bivalves, which adopts the following steps: using pond culturing mussels as a comparison population, and taking mussels with same-batch and consistent specification transplanted to a water area to be monitored as an experimental population; temporarily culturing living mussels in aerated water to remove impurities in shells and alimentary tracts, removing the shells to obtain mussel parenchyma, storing the mussel parenchyma in a refrigerator; taking the mussel parenchyma out, washing the mussel parenchyma by using ultra-pure water after unfreezing, and drying, grinding the mussel parenchyma into powder for being placed in a dryer for standby application; taking the dried mussel parenchyma, placing the dried mussel parenchyma into a container, adding high-pure nitric acid, and acid-splitting the dried mussel parenchyma under room temperature; digesting by a microwave oven, and performing the constant volume to solution to be monitored by using ultra-pure water; and measuring and indicating the element accumulation discrepancy of shellfishes-mussels parenchyma and the content of heavy metal pollutant and the like as well as the experiment monitoring effect by utilizing an inductively-coupled plasma spectrometer. The invention can more accurately reflect the difference of multiple heavy metals and trace elements in shellfishes in changeable water environment on pollution degree and accumulation level.

The invention discloses a UPLC fingerprint spectrum detection method of lamiophlomis rotata (Benth.)Kudo and preparations thereof. The method includes the following steps of: (a) the preparation of areference substance solution; (b) the preparation of a test solution; (c) the provision of UPLC detection conditions; (d) the formation of a standard fingerprint spectrum with sesamoside, caffeic acid, chlorogenic acid, shanzhiside methyl ester, loganin, 8-O-acetyl shanzhiside methyl ester, forsythiaside B, galuteolin, verbascoside, Isoacteoside and the like adopted as reference peaks; and (e) thequality control of the fingerprint spectrum. According to the method, during test solution preparation, an extraction solvent is environment-friendly. The method is simple. Compared with a traditional HPLC method, the method is more convenient and rapider, and save energy and reduce energy consumption. The separation effect of the characteristic peaks of the fingerprint spectrum of the lamiophlomis rotata (Benth.)Kudo and the preparation thereof is good; and characteristic compositions and medicinal compositions can be reserved completely. The method has the advantages of good repeatability,high stability, high precision and strong specificity. The method can accurately and quickly control the lamiophlomis rotata (Benth.)Kudo and the preparations thereof.

The invention discloses a method for measuring D-sorbitol in plasma or urine with the liquid chromatography-mass spectrometry, which comprises the following steps: taking a to-be-tested sample, adding a certain amount of an organic solvent protein precipitation for protein precipitation, separating via a chromatographic column after pretreatment, and detecting with a mass spectrometric detector. The method disclosed by the invention is rapid, accurate, high in sensitivity and convenient in operation, and is suitable for measuring concentration of D-sorbitol in plasma and urine.

The invention discloses a method for determining the concentration of tadalafil in blood plasma by liquid chromatography-mass spectrometry, which adopts a liquid chromatography-mass spectrometry system for determination and comprises the following steps: taking a sample to be detected, adding a certain amount of mixed organic solvent for extraction and pretreatment, performing separating by usinga chromatographic column, and performing detecting by using a mass spectrometry detector. The method disclosed by the invention is rapid, accurate, high in sensitivity and simple and convenient to operate, and provides a basis for measuring the blood concentration of tadalafil; according to the method, the linear range of a plasma standard curve is 1-600ng/mL, the intra-batch precision RSD and theinter-batch precision RSD are both less than +/-15%, and the method is suitable for measuring the concentration of tadalafil in plasma.

The invention relates to a pretreatment method for base rubber of single-component dealcoholized type room temperature vulcanized silicone rubber, and belongs to the field of dealcoholized type room temperature vulcanized silicone rubber. The pretreatment method comprises the following steps that a catalytic reaction is carried out, wherein the base rubber with the viscosity ranging from 10,000 mPa.s to 60,000 mPa.s is fed into a reaction still with a stirring device, and a catalyst and a cross-linking agent are sequentially added; a neutral reaction is carried out, wherein after the reaction is finished, neutralizer accounting for 0.2-10 parts by mass is added for the neutral reaction; a devolatiligation process is carried out, wherein after neutralization, low components generated in the reaction are all removed in the water removal process of the base rubber. 107 rubber treated through the steps is subjected to 1HNMR, 29Si-NMR and IR analysis and contains no silicon hydroxyl. No obvious rising phenomenon occurs when the treated 107 rubber is used as raw materials for preparing the single-component dealcoholized type room temperature vulcanized silicone rubber. Under the condition of accelerated aging, surface drying after placing, curing time, extrusion and the like have no obvious changes.

The invention discloses a method for determining concentration of carbamazepine in plasma by liquid chromatography mass spectrometry. A liquid chromatography mass spectrometry system is used for determining. A sample to be determined is added with a certain amount of mixed organic solvent to extract twice, is separated through a chromatographic column after pretreatment, and is detected by a massspectrometer. The method is rapid, accurate, high in sensitivity, and simple and convenient to operate. The method provides a basis for the blood drug concentration determination of carbamazepine. Thelinear range of a plasma standard curve in the method is 5 to 1000 ng/mL. The intra-batch and inter-batch precision RSD are less than +/-15%. The method is suitable for determining the concentrationof carbamazepine in the plasma.

The invention relates to a method for detecting the pesticide residue quantity in radix ophiopogonis. The method comprises the following steps of (1) weighing radix ophiopogonis to be tested; performing treatment by using a QuEChERS pretreatment technology; preparing a first test product solution; (2) weighing a proper amount of ribonolactone and sorbitol; adding acetonitrile and water for dissolution; using the materials as an analysis protection agent; (3) measuring the first test product solution; blowing the solution to the near dry state by nitrogen; adding acetone for dissolution; addingthe analysis protection agent; performing uniform mixing; using the materials as a second test product solution; (4) weighing a pesticide reference product solution; respectively adding acetonitrileto prepare a first reference product solution; measuring and taking the first reference product solution; respectively adding acetone to prepare a second reference product solution; (5) using a testing method; (6) calculating the content of pesticide in the first test product solution and the second test product solution according to an outer standard method. The method has the characteristics ofhigh repeatability, high accuracy, low utilization cost and the like. The pesticide residue quantity in the radix ophiopogonis can be fast, effectively, simply and conveniently detected.

The invention discloses a met/hod for determining the concentration of 5'-methoxyl-3',4'-methylenedioxyphenyl cinnamic acid isobutyl amide in plasma. A liquid chromatography-mass system is adopted to determine. The method comprises the following steps: taking a to-be-determined sample first, adding a certain quantity of organic solvent for extraction, separating through a chromatographic column after pretreatment, and determining by using a mass spectrometry detector. The method disclosed by the invention has the advantages of rapidity, accuracy, high sensitivity, simplicity and convenience in operation and is suitable for determining the concentration of 5'-methoxyl-3',4'-methylenedioxyphenyl cinnamic acid isobutyl amide in plasma.