50 results about "Dinitrofluorobenzene" patented technology

The invention discloses an isophorone fluorescence probe, and a preparation method and an application thereof. The structure of the fluorescence probe is represented by formula I. The preparation method comprises the following steps: adding isophorone, malononitrile and pyridine to a reaction bottle, carrying out heating refluxing under the protection of an inert gas for 18-24h, purifying, adding the above obtained pure product, p-hydroxybenzaldehyde and pyridine to the reaction bottle, carrying out heating refluxing under the protection of the inert gas for 4-18h, purifying, adding the obtained pure product, 2,4-dinitrofluorobenzene and triethylamine to the reaction bottle, stirring above materials for 8-36h, and purifying the obtained mixture to obtain the fluorescence probe. The fluorescence probe has large Stokes shift (182nm), long fluorescence emission wavelength (592nm), high sensitivity and good selectivity, can specifically detect hydrogen sulfide in organisms, environment and foods, has good biomembrane permeability and low cytotoxicity, and also has the advantages of simple synthesis route, high yield and very large practical values.

The invention relates to a fluorescence enhancement type hydrogen sulfide fluorescent probe and particularly relates to a fluorescence enhancement type hydrogen sulfide fluorescent probe based on flavone derivatives. Flavone derivatives are directly reacted with 2,4-dinitrofluorobenzene, and a reaction product is subjected to column chromatography to generate a pure probe product. According to the fluorescence enhancement type hydrogen sulfide fluorescent probe, probe molecules have the maximum absorption wavelengths of 460nm, relatively good solubility in a 1.5mM CTAB water solution and stable optical performance; by adding the probe molecules together with hydrogen sulfide, the absorption wavelengths are blueshifted from 460nm to 450nm, and the intensity of a fluorescence spectrum is continuously enhanced at 612nm and is maximally enhanced by 96 times. According to the fluorescence enhancement type hydrogen sulfide fluorescent probe, the deficiencies that an existing fluorescent probe is slow in response to hydrogen sulfide and high in detection line, and detection wavelengths are in a visible light region are overcome; the probe molecules are high in sensitivity, stable in optical performance, relatively high in synthetic yield, strong in capability of identifying hydrogen sulfide, high in response speed, wide in detection range and low in detection lower limit, the response range is 0-50 mu M, and the detection limit is 0.09 mu M; therefore, the fluorescent probe has practical application values in the fields of biological chemistry, environmental science and the like.

The invention provides a fluorescent probe for detecting hydrogen sulfide in cells, a method for preparing the fluorescent probe and application thereof. A chemical structural formula of the fluorescent probe is shown. Reaction can be carried out on 2,4-dinitrofluorobenzene and reaction products of 4-ethynylbenzonitrile and 4-bromine-2-hydroxybenzaldehyde to obtain the fluorescent probe. The hydrogen sulfide in solution or the cells or organisms can be detected by the fluorescent probe by the aid of fluorescence. The fluorescent probe, the method and the application have the advantages that the fluorescent probe can be obtained by means of chemical synthesis, synthesis processes are simple and feasible, raw materials are inexpensive and are easily available, and accordingly the fluorescentprobe is low in preparation cost; the fluorescent probe is high in specificity, and interference due to other components can be prevented in detection procedures; the fluorescent probe is short in response time, high in sensitivity and excellent in fluorescence emission spectral characteristic, and the hydrogen sulfide in the cells can be quickly and accurately detected by the fluorescent probe;the fluorescent probe has a broad application prospect in research on the influence of the hydrogen sulfide in the biological cells on physiological and pathological procedures.

Pharmacological test shows that the externally-used preparation of Cetirizine has ideal allergy resistant and anti-inflammatory action to the rat passive cutaneous anaphylaxis (Rat PCA) model and dimethylbenzene caused mouse otitis model, and also prevents the adverse effect to the central system caused by whole body administration. It is also found in the test, that the externally used preparation of Cetirizine also has very fine inhibitory action to dinitrofluorobenzene caused mouse porphyria hypersensitivity (PTH), the novel pharmacological action of the Cetirizine shows that the Cetirizine external preparation has good therapeutic action to skin inflammations which mainly include porphyria hypersensitivity.

The invention discloses a near-infrared fluorescent probe for high-selectivity detecting of thiophenol and a synthesis method and application thereof, and belongs to the technical field of chemical analysis and detection. The near-infrared fluorescent probe is obtained by reaction between a dicyanoisophorone-julolidine large pi system and 2,4-dinitrofluorobenzene, and has the following structure (please see the specifications for the structure). Fluorophore of the probe is the dicyanoisophorone-julolidine large pi system, and a response group to thiophenol is 2,4-dinitrophenoxy. Molecules of the probe have high selectivity and sensitivity to thiophenol, the detection range is 1-60 [mu]mol.L<-1>, and the limit of detection is 0.13 [mu]mol.L<-1>. The probe can be used for detecting thiophenol in water bodies, soil and cells.

The invention discloses a near-infrared fluorescent probe for detecting thiophenol and a synthesis method and application thereof, and belongs to the technical field of chemical analysis and detection. The near-infrared fluorescent probe is obtained by reaction between a dicyano-substituted isophorone large pi system and 2,4-dinitrofluorobenzene, and has the following structure (being defined as in the specification). Fluorophore of the probe is the dicyano-substituted isophorone large pi system, and a response group to thiophenol is 2,4-dinitrophenoxy. Molecules of the probe have high selectivity and sensitivity to thiophenol, the detection range is 0.5-10 [mu]mol.L<-1>, and the limit of detection is 23 nmol.L<-1>. The probe can be used for detecting thiophenol in water bodies, soil and cells.

The invention relates to a glutathione fluorescence probe as well as a preparation method and an application thereof. A probe structure is shown in a formula (I). The preparation method comprises the following steps of: dissolving 2,4-dinitrofluorobenzene, fluorescein and potassium carbonate into anhydrous dimethyl formamide (DMF); after reaction, preparing the glutathione fluorescence probe; the application of the glutathione fluorescence probe refers to detection on contents of glutathione having non-diagnostic property. According to the glutathione fluorescence probe as well as the preparation method and the application of the glutathione fluorescence probe, the fluorescence reaction only on the fluorescence probe and glutathione is carried out while the fluorescence reaction on the fluorescence probe and other amino acids is avoided, so that the glutathione fluorescence probe has high selectivity and specificity; the preparation process of the probe is easy and feasible, and the probe is easy for scale production.

The invention provides an enhanced type fluorescent probe for detecting hydrogen sulfide. The fluorescent probe is an NRS fluorescent probe, the structural general formula of the NRS fluorescent probe is shown as (I), the preparation method comprises the following steps: adding nile red, 2,4-dinitrofluorobenzene and potassium carbonate into dimethylformamide, heating to 70-80DEG C, performing reflux reaction for 3 hours, extracting the reaction liquor by dichloromethane and collecting an organic phase, drying the organic phase with anhydrous magnesium sulfate, and purifying through silica column chromatography to obtain a target product. The probe has a mitochondrial location function, can perform real-time and on-site online detection to mitochondria, and can help us to further master the physiological function of the hydrogen sulfide and promote the understanding of physiological action of H2S, and provide a visible detection tool for research and development of novel cardiovascular drugs.

The invention relates to a high-performance liquid chromatography analytical method for N1,N1-diisopropyl ethylenediamine. The analytical method is characterized by including the following steps that 1, N1,N1-diisopropyl ethylenediamine standard solutions of different concentrations are prepared, excess 2,4-dinitrofluorobenzene is added into the standard solutions for a derivatization reaction, after the reaction is completed, high-performance liquid chromatography analysis is carried out on reaction solutions, and the DNB-N1,N1-diisopropyl ethylenediamine peak area corresponds to a N1,N1-diisopropyl ethylenediamine concentration drawing standard curve; 2, a test sample is prepared into a solution, excess 2,4-dinitrofluorobenzene is added into the solution to react, after the reaction is completed, high-performance liquid chromatography analysis is carried out on the reaction solution, and the content of N1,N1-diisopropyl ethylenediamine in the test sample is calculated. The analytical method is accurate, high in repeatability and sensitivity, and capable of being used for detecting N1,N1-diisopropyl ethylenediamine in the producing and placing processes of acotiamide hydrochloride and tablets thereof and detecting N1,N1-diisopropyl ethylenediamine in other samples.

The invention discloses an application of globeflower flavonoids in preparation of a medicine for treating itch dermatoses. The application range of globeflower flavonoids is expanded; a novel medicine is provided for treatment of itch dermatoses; from a pharmacology experiment, the globeflower flavonoids have good prevention and treatment effects on a mice chronic eczema model, have an obvious inhibiting effect on mice delayed-type allergic reaction caused by 2,4-dinitrofluorobenzene, have obvious anti-inflammatory effect in ear swelling in mice caused by xylene, and have a significant inhibiting effect on capillary permeability increase in mice caused by glacial acetic acid; and the globeflower flavonoids can have relatively good counteraction on guinea pig pruritus caused by histamine phosphate, are low in toxicity and safe to use, and have a relatively good application prospect.

The invention discloses a method for detecting amino acid content in calcium zinc gluconate oral solution. According to the detection method, pre-column derivatization-reversed-phase high-performanceliquid chromatography is adopted, and 2,4-dinitrofluorobenzene is taken as a derivatization reagent. The detection method comprises the following steps: (1) preparing a separation degree stock solution containing lysine hydrochloride and other impurity amino acids; (2) determining a corresponding relation between the dose of the derivatization reagent and the amino acid content in the separation degree stock solution; (3) preparing a test stock solution by utilizing calcium zinc gluconate oral solution, and carrying out derivation reaction, wherein the addition amount of the derivatization reagent is determined according to the corresponding relation determined in the step (2) and the amino acid content in the test stock solution; and (4) detecting by utilizing a reversed-phase high-performance liquid chromatograph. According to the method for detecting amino acid content in calcium zinc gluconate oral solution disclosed by the invention, the addition amount of the derivatization reagent is optimized, the pH value of a mobile phase is optimized, the detection process is excellent in repeatability, and the method is high in sensitivity and stable and reliable in appearance time.

The invention relates to a method for detecting aminobutyric acid in a sample by high efficiency liquid chromatography. The method comprises the following steps of: performing derivatization reaction between a to-be-tested sample and NaH2CO3 in the presence of a derivatization reagent 2,4-dinitrofluorobenzene; and performing high efficiency liquid chromatography on the derivatization product under the conditions that the C18 column is adopted, the mobile phase A is a mixture of acetonitrile and water at a volume ratio of 1:1, the mobile phase B is 0.05 M KH2PO4 solution with pH of 3.3-3.7, the flow Velocity is 0.8-1.2 mL / min, the column temperature is 30-40 DEG C, the sample size is 20-40 MuL; and the UV detection wavelength is 350 nm, to obtain the content of aminobutyric acid in the sample. The high efficiency liquid chromatography method is advantageous in short operating time, high baseline stability, high recovery rate and good precision and reproducibility, can effectively detect the content of aminobutyric acid in brain tissues, and can be widely applied to clinical examination and scientific research.

The invention discloses a manufacturing method of a cast-in-place LOFT floor slab; secondary design and construction are carried out after the civil engineering of a main project is completed; the manufacturing method has the following process steps that steel sheet meshes are welded on I-shaped steel and channel steel; galvanized steel wire meshes are bound with the steel sheet meshes; then dinitrofluorobenzene (DFB) light aggregate is cast; polystyrene boards are buried in the DFB light aggregate in parallel; glass fiber grid cloth is respectively paved in the middle of the DFB light aggregate above and below the polystyrene boards; after being cast, the DFB light aggregate is leveled, compacted and cured; and then the cover surface of an anti-crack layer is plastered with mortar aggregate. According to the manufacturing method, no formwork is needed, the construction efficiency is improved, the weight is light, the strength is high, and the strength requirements can be fully met. The manufacturing processes of the method are easy to operate, so that energy is saved and environment is protected. The manufactured LOFT is light, has high strength and good integral fire-proofing performance, and the manufacturing method is a complete process technology which is easy to promote.

The invention discloses fluorescent probes for specific recognition of thiophenol and a preparation method of the fluorescent probes. The probes are obtained through base catalysis of 2,3,6,7-tetrahydro-10-hydroxyl-1H,5H-quinolizino(9,1-GH)coumarin and 2,4-dinitrofluorobenzene in an organic solvent. In an acetonitrile / PBS buffer system, the probes react with thiophenol selectively to release a fluorescent substance 2,3,6,7-tetrahydro-10-hydroxyl-1H,5H-quinolizino(9,1-GH)coumarin, so that the reaction system has a strong fluorescence signal at the wavelength of 519 nm. Experiment results indicate that the probes can specifically recognize thiophenol, have the characteristics of low limit of detection (only 36 nmol / L) and large Stokes displacement (128 nm) and the like and can realize qualitative and quantitative detection of thiophenol by use of the fluorescence enhancement response to thiophenol. The probes can be obtained through chemical synthesis, the synthesis process is simple andeasy to implement, and the detection method is simple to operate, high in sensitivity and good in selectivity, so that the probes have actual application value in the biological field.

The invention provides a highly-sensitive method for determining the residual quantity of piperidine in a bulk drug. The method comprises the following steps: 1, taking a bulk drug sample, diluting the sample, adding 2,4-dinitrofluorobenzene, adding an acid binding agent, and carrying out a derivation reaction; and 2, determining the residual quantity of piperidine in the sample through liquid chromatography by using an ultraviolet detector. The derivation reaction adopted by the method has mild conditions, can be carried out at room temperature, and is fast and complete; a generated derivation product has ultraviolet absorption, the detection sensitivity is obviously improved, and the detection limit can reach 0.30 ng; and a derivation reaction solution has a good state stability, and thedetermination method is stable and reliable.

The invention discloses application of azalomycin F to the preparation of medicines for treating atopic dermatitis. Proved by experiments, the azalomycin F can obviously decrease the concentrations of IL-4 (Interleukin-4) and Ig E (Immunoglobulin E) in the serum of a model mouse suffering from the atopic dermatitis caused by DNFB (Dinitrofluorobenzene), inhibit the ear swelling of the mouse suffering from the atopic dermatitis and decrease the thymus index and the spleen index of the mouse, obviously improves the skin-lesion symptom of the mouse, and further presents the effect of being capable of radically treating the atopic dermatitis, thereby showing that the azalomycin F has an obvious anti-atopic-dermatitis function; the azalomycin F can be used for preparing the medicines for treating the atopic dermatitis; the favorable application and development prospect of the azalomycin F are shown.

The invention discloses a method for detecting amino acid content in calcium zinc gluconate oral solution. According to the detection method, pre-column derivatization-reversed-phase high-performanceliquid chromatography is adopted, and 2,4-dinitrofluorobenzene is taken as a derivatization reagent. The detection method comprises the following steps: (1) preparing a separation degree stock solution containing lysine hydrochloride and other impurity amino acids; (2) determining a corresponding relation between the dose of the derivatization reagent and the amino acid content in the separation degree stock solution; (3) preparing a test stock solution by utilizing calcium zinc gluconate oral solution, and carrying out derivation reaction, wherein the addition amount of the derivatization reagent is determined according to the corresponding relation determined in the step (2) and the amino acid content in the test stock solution; and (4) detecting by utilizing a reversed-phase high-performance liquid chromatograph. According to the method for detecting amino acid content in calcium zinc gluconate oral solution disclosed by the invention, the addition amount of the derivatization reagent is optimized, the pH value of a mobile phase is optimized, the detection process is excellent in repeatability, and the method is high in sensitivity and stable and reliable in appearance time.

The invention discloses an application of an imiquimod / dinitrofluorobenzene double drug-carrying nano carrier. The invention provides an application of the imiquimod / dinitrofluorobenzene double drug-carrying nano carrier in preparing a drug for treating cutaneous malignant melanoma. The administration route of the imiquimod / dinitrofluorobenzene double drug-carrying nano carrier is delivered by means of an ultrasonic conductometer in a targeted mode. The imiquimod / dinitrofluorobenzene double drug-carrying nano carrier disclosed by the invention improves the curative effect on malignant melanoma, improves the living quality of patients and prolongs the lifetime.

The invention relates to a fluorescent probe of recognizing H2S based on 4-styrene pyridinium long wave emission and a synthetic method and application thereof. The fluorescent probe has a structuralformula as follows: a formula is as shown in the description. The preparation method comprises the following steps: inputting 4-(diethylamino) salicylaldehyde, 4-methyl pyridinium and piperidine by taking ethanol as a solvent; heating the mixture for a reflux reaction; spinning out a solvent; purifying a coarse product by means of silica gel column chromatography; carrying out separation by methane and dichloromethane as an eluent to obtain a compound 1; inputting compounds 1,2,4-dinitrofluorobenzene and potassium carbonate by taking DMF as a solvent; stirring the mixture at room temperature;filtering the mixture to obtain a coarse product; purifying the coarse product by means of silica gel column chromatography; and carrying out separation through an eluent to obtain the fluorescent probe L. The fluorescent probe has the advantages that the fluorescent probe is simple in synthetic step and easy to separate and purify; the fluorescent probe can recognize H2S in a water medium in an enhanced manner by long wave emission of fluorescence, has good selectivity, relatively high sensitivity and relatively good interference resistance and can be applied to an actual water sample to detect H2S.

The pharmacological experiment shows that, the externally used preparation of Loratadine has very good allergy resisting and anti-inflammatory action to the rat passive cutaneous anaphylaxis (Rat PCA) model and dimethylbenzene caused mouse otitis model, in the experiment, it is found by chance that, the externally used preparation of Loratadine also has very fine inhibitory action to dinitrofluorobenzene caused mouse porphyria hypersensitivity (PTH), the novel pharmacological action mechanism of the Loratadine shows that the Loratadine external preparation has good therapeutic action to skin inflammations which mainly include porphyria hypersensitivity.

The invention discloses a preparation method of an alkali-resistant yellow disperse dye, which comprises the following steps: reacting 2, 4-diaminotoluene with 2, 4-dinitrofluorobenzene to obtain a compound of formula (II-1); performing diazotization and coupling reaction to obtain a compound shown as a formula (III-1); and reacting with methyl bromide to obtain the compound shown in the formula (I-1). The dye prepared by the preparation method can realize short-process dyeing on polyester fiber fabrics, not only can improve the alkali resistance of alkali-resistant disperse dyes under the condition that the pH value is 10-12, but also can significantly improve the dyeing defect or non-uniform dyeing phenomenon of the polyester fabrics.

The invention relates to the technical field of fluorescence detection, and provides a fluorescent probe for detecting H2S, and a preparation method and uses thereof. The preparation method comprisesthe steps: step 1, weighing phenanthrenequinone and p-hydroxybenzaldehyde and dissolving in absolute ethanol, and then adding ammonium acetate to obtain a mixed solution A, heating the mixed solutionand stirring to react; after the reaction is finished, cooling to room temperature, subjecting a precipitate to suction filtration under reduced pressure to obtain a filter cake, then recrystallizingwith a solvent to obtain an intermediate product; step 2, adding the intermediate product obtained in step 1 and 2,4-dinitrofluorobenzene to acetonitrile, and then adding anhydrous potassium carbonateto obtain a mixed solution B, stirring at room temperature to react, after the reaction is finished, removing the solvent, and obtaining the fluorescent probe for detecting H2S by column chromatography purification. The invention develops a novel high-performance hydrogen sulfide fluorescent probe, which is successfully applied to detecting hydrogen sulfide in food.

The invention relates to preparation and application of a hydrogen sulfide (H2S) near-infrared fluorescent probe, wherein the structural formula of the probe is shown in the specification. The invention provides the preparation method for synthesizing the fluorescent probe by taking isophorone-xanthene dye, 2,4-dinitrofluorobenzene and the like as raw materials. The fluorescent probe is a hydrogen sulfide fluorescent probe with large Stokes shift and near infrared emission. Firstly, the fluorescent probe shows good sensitivity to H2S, the linear range is 1 [mu]M-10 [mu]M, and the detection limit is 0.3 [mu]M; secondly, the fluorescent probe shows high selectivity on H2S, and is not influenced by various other ions, active oxygen and biological mercaptan; moreover, the fluorescent probe can quickly act with H2S, and the response time is within 10 minutes; and in addition, the fluorescent probe can also be applied to detection of H2S content in living cells.

The invention provides a preparation method of an N-aryl pyridine thiazolothiazole-cucurbituril compound, which comprises the following steps: dissolving 2, 5-bis (4-pyridyl) thiazolothiazole in 2, 4-dinitrofluorobenzene, heating, cooling, washing with n-hexane, and carrying out vacuum drying to obtain a Zincke salt; the preparation method comprises the following steps: adding ethanol and water into Zincke salt and parachloroaniline, uniformly mixing, heating and refluxing, cleaning with diethyl ether, and recrystallizing an obtained crude product in a methanol solution to obtain N-aryl pyridine thiazolothiazole molecules; the molecule and cucurbituril 8 are respectively dissolved by dimethyl sulfoxide and then are mixed to prepare a storage solution. The oxidoid enzyme activity of the thiazolothiazole derivative is found for the first time, and the compound and macrocyclic molecule cucurbituril are self-assembled, so that the photoinduced oxidase activity of N-aryl pyridine thiazolothiazole is greatly improved, and the nano compound with excellent photoinduced oxidase activity is constructed. And the method has a better application prospect in nano-enzyme biological treatment and sensing.

The invention discloses a pulsatilla saponin composition. The pulsatilla saponin composition comprises pulsatilla saponin B4 and pulsatilla saponin B5 in a weight ratio of (3-9): 1. The invention further discloses a medicine containing the pulsatilla saponin composition and application of the medicine. According to the application disclosed by the invention, oxazolone and 2, 4-dinitrofluorobenzene (DNFB) are respectively utilized to prepare two specific dermatitis mouse models (Atopics, AD), imiquimod is utilized to prepare a mouse psoriasis model, the protective effects and possible mechanisms of pulsatilla saponin B4 and pulsatilla saponin B5 on skin diseases are discussed, and a theoretical basis is provided for treating the skin diseases.

The invention discloses a method for measuring the sulfur-containing amino acid content of Astragali mushroom, and relates to the field of measurement of amino acid content of the Astragali mushroom.The method comprises the following steps: performing performic acid oxidation protection on the Astragali mushroom serving as a raw material, performing acid hydrolysis, performing ultrafiltration centrifugation, performing derivatization by taking 2,4-dinitrofluorobenzene as a derivatization reagent, performing gradient elution on the obtained derivative sample liquid through high performance liquid chromatography and by taking acetonitrile-water and sodium acetate as flowing phases, detecting under the wavelength of 360 nm, separating derivatives of cysteic acid and methionine sulfone, measuring the peak area of a cystine standard product and a methionine standard product under different concentration gradient, drawing a standard curve, and measuring the cystin content and the methioninecontent separately to obtain the sulfur-containing amino acid content. According to the method, the requirement on instruments is low, the reaction condition does not need to be strictly limited, thequantity of the needed samples is small, the samples are not damaged, single component can be analyzed, and the method is a measuring method which is efficient, accurate, simple, convenient and easyto operate and low in price.

The invention relates to an HPLC (high performance liquid chromatography) measuring method for amino acid of hydrolyzed vegetable protein (HVP) liquid. According to the method, a salt solution serves as a flowing phase on the basis of HPLC, and certain N,N-dimethyl formamide and acetic acid are added to improve chromatographic peak shape and separation degree. The amino acid of the HVP liquid is measured by a 2,4-dinitrofluorobenzene pre-column derivation-HPLC-ultraviolet detection method. The peak shape is improved by preparing and taking the specific salt solution as the flowing phase, so that the separation degree of each amino acid derivative is good, the matrix interference is small and quantification is more accurate. The method is high in analysis precision, is particularly suitable for various amino acid mixtures and is good in separation and accurate in quantification.

The present disclosure provides a method for photocleavage of an amide bond, the method has mild reaction conditions and can realize the cleavage of amide bonds by using light. The method comprises the following steps: subjecting 2,4-dinitrofluorobenzene to a reaction with an amino group of a substance represented by structural formula I with an α-amino acid at the end to produce a compound 1 represented by structural formula II; then under light irradiation, subjecting the compound 1 to a cleavage reaction of amide bond;Wherein, R1 is the side chain group of α-amino acid; R2 is: aryl, aliphatic hydrocarbon, —CH(R)—COOH or polypeptide.