68 results about "Dansyl chloride" patented technology

The invention belongs to the field of food inspection, relates to an assay determination method for endocrine disruptors in food, and particularly relates to a method for analyzing and determining a plurality of endocrine disruptors in milk powder and liquid milk. The method comprises the steps of dissolving a sample with water, adding an organic solvent mixable with water, extracting a to-be-detected material by ultrasonic, adding a sodium salt to make the organic solvent separated from a water phase to realize liquid-liquid extraction, taking an organic solvent containing quantitative to-be-detected material, purifying by extraction with a solid phase filled with C 18 materials, deriving by dansyl chloride, and analyzing and detecting four types of 26 endocrine disruptors in the food by using ultra-high performance liquid chromatography-quadrupole-time of flight-mass spectrometry at the same time. The method can overcome the disadvantages that a conventional technology cannot realize simultaneous analysis of the plurality of the endocrine disruptors in the food by once chromatographic sample injection, can increase sensitivity of the quadrupole-time of the flight-mass spectrometry, and realize accurate analysis of the endocrine disruptors in the food by using the quadrupole-time of the flight-mass spectrometry.

The invention discloses a separation and liquid chromatography column pre-column derivatization method of biogenic amine in a soybean paste, comprising the following steps of: (1) adding a trichloroacetic acid solution to the soybean paste, homogenizing, centrifuging and collecting a supernate; (2) adding normal hexane to the supernate, vibrating and taking out a lower layer trichloroacetic acid phase for later use after static layering; (3) adding an NaOH solution to the trichloroacetic acid phase, then adding an NaHCO3 solution for buffering, and mixing in a dansyl chloride acetone solution to carry out derivatization; and (4) removing dansyl chloride to terminate the reaction to obtain a derivative solution and filtering. The separation method has simple treatment process and low reagent consumption and avoids analyte loss caused by transfer. The soybean paste can reach detection demands after being separated and purified; undesired peak disturbance of a spectrogram is less and the determinand loss is low, and the recovery rate of the biogenic amine can reach more than 80 percent. The method determines the optimum condition for deriving the biogenic amine; dansyl chloride derivative products are stable and the detection sensitivity is high.

The invention discloses a method for analyzing amine substances in dansyl chloride derived-plasma based on liquid chromatography mass spectrometry. The method is characterized in that dansyl chloride is used as a derivatization reagent to perform derivatization on a metabolite containing primary amine and secondary amine, therefore the retention capability of the amine substances in reversion phase chromatography is increased, the ionization efficiency in mass spectrometric detection is increased, and the purpose of increasing the quantitative accuracy and detection sensitivity of the amine substances is achieved. The method has wide coverage for amine metabolites (comprising amino acid, methylation products, acetylation products, dipeptide and the like), can utilize 100 [mu]L of plasma samples to detect 113 amine substances, supplies the outline information of metabolome of the amine substances, and has the characteristics of good specificity, high accuracy and repeatability, less reagent consumption and the like.

The invention discloses a method for detecting catecholamine in blood plasma by liquid chromatography tandem mass spectrometry. The method comprises the following steps of preparing a standard product, separating by liquid chromatography, detecting by a mass spectrum, drawing a standard curve, and detecting the catecholamine in the blood plasma. The method has the beneficial effects that the catecholamine is detected by innovatively applying a high-flux liquid chromatography tandem triple quadrupole mass spectrograph; protein is precipitated by acetonitrile, dansyl chloride is used for performing derivative reaction, and the liquid chromatography tandem triple quadrupole mass spectrograph is used for detecting after extraction, so that the pretreatment steps are simple, the interference of a matrix in the blood plasma is effectively removed, and the specificity is good; after the derivatization of dansyl chloride, the detection sensitivity is effectively improved; the high-flux liquid chromatography tandem rod mass spectrograph is used for detecting, three types of catecholamine, including dopamine, epinephrine and norepinephrine, in the blood plasma can be quantitatively and accurately detected; the detection time is short, the flux is high, the detection sensitivity is high, the specificity is good, and the cost is low.

The invention belongs to the field of biochemistry detection, in particular to the measurement of bioactive molecules of neuroendocrine immunological network, particularly to a measurement method of amino bioactivators in organism (such as blood or brain tissue), in particular discloses a method for the single-time measuring of ten amino bioactivators in organism, which comprises: taking dansyl chloride as derivative reagent to perform single-time measuring on ten amino bioactivators such as epinephrine (E), noradrenalin (NE), dopamine (DA), 5-hydroxytryptamine (5-HT), histamine (HA), gluetamic acid (Glu), aspartic acid (Asp), Gamma-aminobutyric acid (GABA), glycin (Gly) and trilute (T3) within 75min. The method is simple and rapid, can sensitively measure the concentrations of the ten amino bioactivators in organism fluid, and is suitable to the research requiring to completely analyze the ten amino bioactivators in the organism.

The invention belongs to the fields of micro-nano materials and photochemical analysis, and relates to a universal and efficient multi-band-gap photonic crystal microchip for detecting multiple substrates. The photonic crystal microchip arranged in array is prepared through fast self-assembly of multi-sprayer fine ink-jet printing technology and polyacrylic acid-polymethyl acrylate (shell)-polystyrene (core) polymer nano spheres. The microchip is provided with a design of full-band-gap photonic crystal array, and can perform fluorescence enhancement and amplification to fluorescent chemosensors such as oligomerization ethylenediamine and the like marked by 8-quinolineol or dansyl chloride at different wavelengths, and identifiable detection and analysis of the multi-substrate which cannot be finished by a single and a simple chemosensor can be achieved. By building a multi-band-gap photonic crystal micro-array, detection and analysis of the multiple substrates using the single chemosensor is achieved. The microchip has broad-spectrum universality and high operability in identification and detection of the multi-substrate in various complicated environments.

The invention discloses a manufacturing method of 9, 11-deestering material, which comprises the following steps: adopting intermediate dehydrogenation as raw material; proceeding sulfur-esterifying reaction through dansyl chloride; diluting; filtering; obtaining the wet product; heating to reflux completely; complementing temperature-control water; adjusting reflux reaction at 109+-2 deg.c; diluting; filtering; drying to obtain methylprednisolone 9, 11- deestering material.

A method for detecting amino acid decarboxylase activity of spoilage bacteria in food belongs to the technical field of agricultural products. First, spoilage bacteria are isolated from food, fermented to obtain strain fermentation liquid, and then inoculated into a liquid medium containing amino acids to obtain biogenic amine detection. Use the spoilage bacteria fermentation liquid, and then obtain the supernatant of the sterile body by centrifugation, add Na2HPO4, NaOH and dansyl chloride to the supernatant and the mixed standard solution of biogenic amines, and obtain the derivatives of spoilage bacteria biogenic amines in a water bath under dark conditions. Derivative samples of samples and standard biogenic amines; after pointing and drying, put them into the development tank, wait for the developer to expand to 17cm from the sample point, take them out and dry them, then use automatic gel imaging analysis under ultraviolet light to take pictures respectively, and compare them Yes, determine the type of biogenic amine in the sample according to the Rf value, and judge the amino acid decarboxylase activity of the strain. The invention is convenient and quick, has low cost and can accurately realize the qualitative detection of biogenic amine.

The invention discloses a qualitative and quantitative method for various biogenic amines in white wine and belongs to the technical field of white wine analysis and detection. According to the qualitative and quantitative method, the liquid-liquid extraction is utilized to enrich the biogenic amines in the white wine; derivation is required by both gas phase qualitative treatment and liquid phase quantitative treatment; a derivation agent adopted by the gas phase is TFAA (Trifluoroacetic Anhydride); and dansyl chloride precolumn derivatization is taken as the derivation agent for the liquid phase. According to the method provided by the invention, 9 biogenic amines are firstly determined in the white wine; the limit of detection of the quantitative method can be reduced to about 10ug/L; the linearly dependent coefficient is more than 0.99; the recovery rate is 80.19%-104.05%; the relative standard deviation is within 4%; the biogenic amines in the white wine can be detected by using the qualitative and quantitative method; the feasibility is excellent; and the precision is high.

The invention firstly establishes an ultrahigh-efficiency liquid chromatography method which is used for quickly extracting and determining nine medicinal biogenic amines in the kudzu vine root whichis a medicine-and-food homologous product. The nine biogenic amines comprise tryptamine, phenylethylamine, putrescine, cadaverine, histamine, octopamine, tyramine, spermidine and spermine. After breaking a kudzu vine root sample, extraction by 0.4mol/L hydrochloric acid is utilized. Derivatization is performed in front of a dansyl chloride column. Ammoniacal liquor is added for terminating reaction, and acetonitrile is added for realizing a constant volume. A UPLC chromatographic column is utilized. Ammonium acetate and acetonitrile are used as mobile phase for performing gradient elution. A diode array detector is utilized for detecting in a wavelength of 254nm. The detecting method has an excellent linear relation. The sample recovery rate is 75.6-97.2%, and the relative standard deviation is 0.12-5.32%. The method limit of quantitation of the nine biogenic amines are respectively 10mg/kg. The method has advantages of simple operation, high speed and high sensitivity. The method canbe used for simultaneously measuring the residual amount of nine biogenic amines in the animal and botanical food such as kudzu vine root.

The invention provides a fluorescent material, and also provides a fluorescent molecularly imprinted polymer prepared by the fluorescent material. The fluorescent material is dansyl methacrylic acid, and the preparation method comprises the following steps: performing a sulfonylation reaction of dansyl chloride and aminoethyl methacrylamide hydrochloric acid under the action of a catalyst to obtain a dansyl methacrylic acid solution, performing extraction and purification of the obtained solution to obtain the dansyl chloride fluorescent material of dansyl methacrylic acid. A molecularly imprinted polymer synthesized by using the dansyl methacrylic acid fluorescent material of the invention as a functional monomer not only can be used as a traditional molecular recognition material for specific separation and combination of target template molecules, but also can be used as a sensing material for direct rapid qualitative and quantitative analysis of endocrine disruptors in environment and food.

The invention relates to a silicon-nanowire-based fluorescence chemical sensor with selective fluorescence response to free copper ions and complexing copper ions as well as a preparation method and application of the silicon-nanowire-based fluorescence chemical sensor. A silicon nanowire or a silicon nanowire ordered array is reacted with 3-2-(2-amino ethyl amino) ethyl amino propyl trimethoxy silane and dansyl chloride after being subjected to surface activation, so that surface functionalized modification of the silicon nanowire or the silicon nanowire ordered array is realized, and the fluorescence chemical sensor is obtained. The fluorescence chemical sensor disclosed by the invention can be used for detecting the free copper ions and the complexing copper ions in a common solution system and a biological system which contain the free copper ions and the complexing copper ions and can be used as a substrate for cell growth to construct an active detection chip with cells; furthermore, the silicon-nanowire-based fluorescence chemical sensor can be used for observing the release of the free and complexing copper ions in a cell withering process in real and time and in situ.

The invention relates to the field of veterinary drug residue detection, in particular to an analysis method for efficiently detecting piperazine residues in chicken tissue, eggs and pork. The methodcomprises the steps of extracting and purifying the chicken tissue, eggs or pork samples through an accelerated solvent extraction method and a solid phase extraction method, performing derivatizationwith dansyl chloride and then performing detection by using an ultra-high performance liquid chromatography fluorescence detection method. Compared with other detection methods, the method has the advantages of higher analysis efficiency, less mobile phase consumption, a high recovery rate, high accuracy, high sensitivity and good reproducibility.

The invention belongs to the technical field of isotope derivatization reagents, and particularly relates to 3-deuterated dansyl chloride and a preparation method and application thereof. According tothe preparation method, 3-deuterated dansyl chloride can be prepared from reaction raw materials including 5-amino-1-naphthalene sulfonic acid, paraformaldehyde, sodium borohydride, sodium hydride, deuterated methyl iodide, phosphorus oxychloride and phosphorus pentachloride. According to the preparation method, the raw materials are easy to obtain, few intermediate products are produced, and the3-deuterated dansyl chloride derivative reagent can be obtained and can be used for fluorescence detection or metabonomics analysis and research.

The invention belongs to the field of biological cell diagnosis and specifically relates to an irreversible rhodamine-based ClO<-> fluorescent probe and a synthetic method thereof. A structural formula of the irreversible rhodamine-based ClO<-> fluorescent probe is as shown in a figure in the specification. The irreversible rhodamine-based ClO<-> fluorescent probe contains a rhodamine fluorophorewith high sensitivity, good light stability, high fluorescent quantum yield and long wavelength. A certain amount of rhodamine lactam and dansyl chloride are subjected to a condensation reaction undercertain conditions to obtain the irreversible rhodamine-based ClO<-> fluorescent probe with a special structure. A synthetic process has simple and easily-available raw materials, mild reaction conditions and simple operation, the obtained rhodamine fluorescent probe can quickly detect ClO<-> in biological cells in an aquatic environment, is free from interference of other ions, belongs to response type identification in combination with the ClO<-> and has irreversibility.

The invention discloses a method for detecting selenomethionine (SeMet) in selenium-enriched yeast and belongs to the technical field of food analysis. The method comprises the following main steps of: (1) performing enzymolysis on combined SeMet in the selenium-enriched yeast; (2) derivating the SeMet through dansyl chloride serving as a derivating agent; and (3) separating and measuring components of derivating liquid by a high performance liquid chromatography-fluorescence detection (HPLC-FLD) method, and calculating content of the SeMet in a sample by an external standard method. Enzymolysis conditions and parameters in the derivatization process are optimized, the technical problem of extracting and derivating the SeMet in the selenium-enriched yeast is solved, the HPLC-FLD method for detecting the SeMet in the selenium-enriched yeast is established, and an accurate, easy and economic effective method is provided for quality evaluation of the selenium-enriched yeast.

The invention provides a ferrous ion fluorescent probe molecule based on dansyl acid structure, a preparation method and application. The molecular formula of the ferrous ion fluorescent probe molecule is C12H14NO4S, and is called FeP1 for short. The probe is prepared by one-step reaction of a commercial reagent dansyl chloride, the synthesis yield is high, and the preparation cost is low. Recognition characteristics of the probe FeP1 in a Tris-DMSO (4:1, pH=7.4, v/v) solution with metal ions, common anions, active sulfur, active oxygen and other small molecular substances are studied througha fluorescence spectrometer. The result shows that: the probe FeP1 has efficient and specific selectivity on ferrous ions (Fe<2+>), has strong anti-interference capability, fast recognition speed andwide pH value application range, has a lowest detection limit of 18 nM, and can be widely applied to detection of ferrous ions in biological systems and environmental samples.

The invention provides a method for detecting catecholamines in blood plasma by using liquid chromatography-tandem mass spectrometry, which belongs to the technical field of blood detection and analysis. The method comprises the steps of (1) preparing a test blood sample; (2) preparing an internal standard working solution; (3) taking the standard mother liquor of the to-be-detected substance, anddiluting the standard mother liquor with a standard diluent; (4) taking out the internal standard working solution, and preparing the following solutions: a standard curve sample, a substrate samplesolution, a test sample and a quality control sample; (5) transferring the supernatant of the standard curve sample, the substrate sample solution, the test sample and the quality control sample intoan EP tube by using a pipette, and carrying out freeze drying; (6) adding a NaOH solution and a dansyl chloride acetonitrile solution, and carrying out a derivative reaction; and (7) adding a reactionterminator, and carrying out liquid chromatography-mass spectrometry in a pore plate. According to the invention, potential anions are eliminated, the ionization efficiency in a positive ion mode isimproved, potential solvents or other interfering substances can be reduced, meanwhile, the polarity of an analyte is reduced, and the detection sensitivity is improved.

The invention provides a method for detecting the content of taurine in formula milk powder for special medical purposes. The method comprises the following steps: (1) preparing a taurine standard substance working solution; (2) extracting taurine: accurately weighing a to-be-detected milk powder sample, dissolving the to-be-detected milk powder sample in water, performing ultrasonic treatment, adding a precipitator, uniformly mixing, centrifugally extracting supernate, and fixing the volume to obtain a to-be-detected sample solution; (3) derivatization treatment: respectively adding a derivatization reagent dansyl chloride into the standard substance working solution and the to-be-detected sample solution prepared in the steps (1) and (2), and carrying out a derivatization reaction in an alkaline environment to obtain a standard substance derivative product and a sample derivative product; and (4) detection and analysis: detecting the content of the taurine derivative product in the sample derivative liquid prepared in the step (3) by adopting a two-dimensional liquid phase system. According to the method, a sample pretreatment method is designed to be combined with a two-dimensional liquid phase system, so that the problem that the content of taurine in the special medical milk powder cannot be accurately analyzed in the national standard is solved, and the detection accuracy is high.

The invention relates to a hydroxyl metabolite derivatization method and a non-targeted metabonomics efficient analysis method. The hydroxyl metabolite derivatization method comprises the steps that 1, hydroxyl metabolite extraction is conducted on a sample to be detected through a first solvent, then drying is conducted to remove the first solvent, and a dried sample is obtained; and 2, the dried sample is mixed with a second solvent to dissolve the dried sample, then 4-dimethylaminopyridine and dansyl chloride are added, the solution and the added substances are well mixed, and heating is performed for incubation; and after incubation is completed, sodium hydroxide is added, then heating is conducted for incubation, finally formic acid is added, and a derivatizated sample is obtained. According to the non-targeted metabonomics efficient analysis method, 12C labeling and 13C labeling are synchronously carried out by adopting the derivatization method, so that the metabolite detection sensitivity is improved, more metabolite can be detected at the same time, and the metabolite coverage rate is higher; and the detected metabolite is a peak pair, so that the influence caused by instrument drift and matrix is reduced, and the quantification is more accurate.

The invention discloses a method for detecting taurine in formula food for special medical purposes, and relates to the technical field of food detection, and the method comprises the following steps:firstly, preparing a standard solution; preparing a sample; and finally analyzing a result. According to the method, a sample is dissolved with water, protein is precipitated by potassium ferrocyanide and zinc acetate, supernatant is taken to subjected to a derivative reaction by using dansyl chloride, a derivative is separated by using a C18 reversed-phase chromatographic column, and finally thetaurine content in the formula food for special medical purposes is detected by using a detector.

The invention discloses a method for determining residual allyl amine in Sevelamer carbonate. The method includes the steps of extraction, derivatization reagent preparation and determination. The method is as below: extracting the residual allyl amine in Sevelamer carbonate by using solvents, then adding a derivatization reagent dansyl chloride in the extracting solution, adjusting the pH value with Na2CO3 solution, so that the allyl amine forms derivatization products, and determining under a fluorescence detector by a liquid chromatography method. The Na2CO3 solution has pH value of 9.5 and concentration of 0.002mg / mL; and the dansyl chloride stock solution has concentration of 0.27mg / mL. The determining method of the invention can make the allylic amine exist in a non-volatile state, stabilize the derivatization product, increase fluorescence absorption sensitivity of sample and improve the detection limit, has the advantages of accuracy, sensitivity and reliability, and provides strong scientific basis for effective control of the residual allyl amine in Sevelamer carbonate.

The invention belongs to the technical field of organic synthesis and biological mercaptan detection, and particularly relates to a dansyl derivative fluorescent probe as well as a synthesis method and application thereof. The synthesis method of the fluorescent probe comprises the steps: dropwise adding a trichloromethane solution of dansyl chloride into a trichloromethane solution containing bromo-substituted alcohol and triethylamine in an inert atmosphere at room temperature, stirring and reacting at room temperature after the dropwise addition is finished, washing and drying a reaction solution after the reaction is finished, evaporating to remove a solvent, separating and purifying a reactant through column chromatography, and thus obtaining the dansyl derivative fluorescent probe. The fluorescence probe and methyl green-pyronin Y are used as a double-fluorescence probe, and a supermolecular proportional fluorescence sensing platform is constructed by utilizing the solubilizationeffect of a surfactant CTAB and is used for selectively detecting H2S.