103 results about "Thiamphenicol" patented technology

The invention discloses a synthesis method of synthesizing florfenicol. The synthesis method comprises the following steps: L-threo-(p-(methylsylfonyl) phenyl) serine ethyl ester which is used as raw material is processed by the protection by a protecting group, configurational transition, hydrolyzation, acetylation, re-protection, deoxidation, fluorination, and pre-hydrolyzation, so that the florfenicol is obtained, wherein, the protecting group R is one of benzoyl chloride, phthalic anhydride, cyanophenyl, and allyl compounds; the configurational transition is performed when sodium alcoholate or sodium methoxide exists. The raw material which is used in the method is a byproduct which is generated during the process of preparing thiamphenicol, is easy to get in the market, and is inexpensive; the technological operation is simple, the cost is low, the yield rate is high, and the synthesis method has industrialized value.

This invention relates to a synthetic method for thiamphenicol and florfenicol and their key intermediate. Through a series of chemical reaction-first, MCPBA oxidation or deshydroxyl fluorination in advance then MCPBA oxidation, then hydrolization for ring-opening, benzyl removal and finally acetylation, the raw material No. 7 compound is ultimately converted into thiamphenicol or florfenicol. In this method, the targeted compound's chiral center is efficiently configurated and the complicated and wasted resolution process is avoied.

Novel formulations containing a fluorinated chloramphenicol or thiamphenicol derivative antibiotic such as florfenicol, and methods for using such formulations in the treatment and prevention of infectious diseases of bovines and swine, including bovine respiratory disease.

The invention relates to a preparation method of 2-nitryl-4-thiamphenicol benzoic acid, which comprises the following steps: (1) reacting 2-nitryl-4-thiamphenicol benzoic acid with cyanide under the condition of carbonitriding reaction and in the existence of catalyst, and obtaining 2-nitryl-4-thiamphenicol cyanophenyl; and (2) hydrolyzing the 2-nitryl-4-thiamphenicol cyanophenyl obtained in the step 1. The product prepared by adopting the method has high productivity and high purity, and the invention has simple process, moderate reaction conditions and shorter reaction time; in addition, the invention also avoids the problems of serious equipment corrosion and environmental pollution caused by the use of strong acid and strong oxidizer, such as HNO3, H2SO4, H2O2, and the like.

The invention discloses a test card for rapidly diagnosing pancreatic trauma and acute pancreatitis and a preparation method of the test card. The test card comprises a plastic shell, a bottom lining and detection modules, wherein the plastic shell is provided with a sampling hole and an observation window, and the sampling hole and the observation window are fixed with transparent waterproof films. The bottom lining is provided with multiple longitudinally parallel arranged slots; and the number of the detection modules is consistent to that of the bottom lining, and the detection modules are glued into the slots of the bottom lining. Each detection module comprises chromatographical membranes, combination pads, sample pads, filtration pads and water sucking pads. The chromatographical membranes are provided with test lines and quality control lines, the test lines are TAP (thiamphenicol) polyclonal antibodies, and the quality control lines are covered rabbit anti-mice immune globulin antibodies. The test card for rapidly diagnosing pancreatic trauma provided by the invention is capable of quickly and accurately diagnosing the diseases such as pancreatic trauma and acute pancreatitis, and adding multiple samples simultaneously for positive control and negative control, and has the advantages of being convenient and rapid to detect, high in flexibility and accuracy, stable in property and cheap in cost.

The invention discloses a thiamphenicol molecularly imprinted electrochemical sensor and a preparation method and application thereof. A porous graphene-molybdenum disulfide nano flower-shaped compound is prepared through a hydrothermal one-step method, and the compound is dropped on the surface of an L-type glassy carbon electrode; aminated multi-walled carbon nanotubes and porous Pt-Pd nanoparticles are dispersed so that the imprinting surface area of the electrode can be increased and stability of a modification interface can be enhanced, and accordingly a three-dimensional porous imprinting substrate is obtained; thiamphenicol serves as template molecules, 1,2-diaminobenzene serves as functional monomers, and an imprinted membrane is prepared through cyclic voltammetry; ascorbic acid serves as a photoelectric chemical probe, and the electrochemical sensor for detecting thiamphenicol is built. The sensor has good thiamphenicol responsiveness, the linear range of the sensor is 1.0*10<-9>-3.5*<-6> mol L<-1>, and the detection lower limit is 5.0*10<-9> mol L<-1>. The sensor can be used for detecting thiamphenicol in meat samples and feed samples.

The invention provides a biological preparation method of a key intermediate of thiamphenicol and florfenicol. Specifically, the method of the present invention comprises the following steps: (a) in aliquid reaction system, a reaction represented by formula A is carried out in the presence of a coenzyme and catalyzed by a carbonyl reductase, using compound X as a substrate, thereby forming compound Y; and (b) optionally separating the compound Y from the reaction system after the reaction of the previous step. The invention also provides a reaction system comprising: (i) an aqueous solvent; (ii) a substrate, said substrate being the compound X; (iii) coenzyme; (iv) carbonyl reductase; (v) a co-substrates; and (vi) enzymes for coenzyme regeneration.

The present invention discloses certain novel prodrugs of chloramphenicol or thiamphenicol, or of an analog of either, including prodrugs of pharmaceutically acceptable salts of chloramphenicol or thiamphenicol or of their analogs, including nitrogen-containing esters of both alcohol groups of such compounds. In certain embodiments these novel prodrugs are sufficiently water-soluble to serve the functions needed of a prodrug of chloramphenicol or thiamphenicol or of an analog of either. In one embodiment, a certain subclass of the compounds also possesses the hydrolytic stability needed to maintain the prodrug in solution in the subject's system until appropriate conditions exist when the prodrug can hydrolyze, releasing the active compound in question.

The invention discloses test paper and a method for detecting florfenicol and thiamphenicol. The test paper comprises a micropore reagent and a test strip, the micropore reagent comprises freeze-dried colloidal-gold-labelled thiamphenicol medicament specific antibody, wherein the thiamphenicol medicament specific antibody is thiamphenicol medicament monoclonal antibody or thiamphenicol medicament polyclonal antibody; the test strip is formed by successively connecting a sample absorption pad, a reaction membrane, a water absorption pad, a protective membrane and a base plate, the reaction membrane comprises a detection zone and a quality control zone, the detection zone is coated with thiamphenicol hapten-carrier protein conjugate, and the quality control zone is coated with antiantibody. The method for detecting florfenicol and thiamphenicol by using the test paper provided by the invention is simple, rapid, visualized, accurate, wide in application scope, low in cost and easy to popularize and use.

The invention provides a three-in-one colloidal gold chromatographic test strip for detecting thiamphenicol, chloramphenicol and florfenicol and a preparation method thereof, and belongs to the technical field of immunological detection. The preparation method comprises two parts, namely, the preparation of a monoclonal antibody and the preparation of a colloidal gold chromatographic test strip, wherein the monoclonal antibody can be used for recognizing thiamphenicol, chloramphenicol and florfenicol at the same time and is high in sensitivity; the colloidal gold chromatographic test strip comprises a polyvinyl chloride backing; a sample pad is arranged at the front end of the polyvinyl chloride backing and is connected with the front end of a nitrocellulose membrane; the rear end of the nitrocellulose membrane is connected with a water absorbing pad; the monoclonal antibody marked by colloidal gold is used as a combining pad; the nitrocellulose membrane is sequentially wrapped with a chloramphenicol sodium succinate-BSA (Bovine Serum Albumin) antigen test ray T and a goat-anti-mouse IgG control ray C. The three-in-one colloidal gold chromatographic test strip for detecting thiamphenicol, chloramphenicol and florfenicol is fast to detect, and the detection needs only 3 to 5 minutes; the test strip is convenient to carry, and suitable for detection on site; the operation is simple and convenient and does not need a professional technical person.

The invention relates to a method for preparing a molecular imprinted polymer capable of recognizing chloromycetin, thiamphenicol and florfenicol simultaneously, which belongs to the technical field of bioengineering. The method comprises the following concrete steps: adding a functional monomer and a cross-linking agent into a pore-forming agent, uniformly mixing and heating; then adding template molecule thiamphenicol and an initiating agent, further ultrasonically degassing the mixed solution, sealing in a nitrogen or vacuum pumping state and carrying out polymerization reaction; after the polymerization reaction is finished, taking the compounded polymer out to grind and screen; eluting by organic solvent to remove template molecules by a combined method of Soxhlet extraction and solid phase-extraction cartridges till the template molecules are not detected by a high performance liquid chromatography-mass spectrometry; finally removing the polymer of the template molecules and drying in vacuum to obtain the molecular imprinted polymer. The polymer can be simultaneously applied to the pre-processing of the antibiotic detection of chloromycetin, thiamphenicol and florfenicol in foods and realizes the specific and selective separation and the efficient enrichment of the chloromycetin, the thiamphenicol and the florfenicol.

The invention discloses a method for detecting residues of chloramphenicols in milk products. Chloramphenicols include chloramphenicol, thiamphenicol and florfenicol. The method comprises the following steps: carrying out pretreatment on a to-be-detected sample: weighing m1g of the to-be-detected sample, adding v1ml of ethyl acetate for extraction to obtain a first extract, dissolving the first extract by virtue of v2ml of methanol, adding v3ml of normal hexane, mixing uniformly, carrying out centrifuging, abandoning superstratum to obtain a second extract, and purifying the second extract by virtue of a solid phase extraction column, so as to obtain purified substances; analyzing the purified substances by virtue of a liquid phase-tandem mass spectrometer, and detecting the residues of the chloramphenicols in the to-be-detected sample, wherein m1 is less than or equal to 5, v1 is less than 20, v2 is less than 1, and v3 is less than 8. According to the method, an interior label is not required, so that an emulsification phenomenon in the detection process can be avoided, and the interference caused by a matrix to the detection can be reduced; chloramphenicol drugs can be simultaneously detected, the sensitivity and the recovery rate are high, the cost is saved, and the operation is easy.

The embodiment of the invention provides a synthetic method of a florfenicol intermediate cyclic product and belongs to the technical field of chemical synthesis. The method comprises the following steps of: (1) carrying out reduction reaction on D-4-Methylsulfonylphenyl serine ethyl ester and potassium borohydride in an organic solvent at a temperature of -5 to 100 DEG C in the presence of anhydrous calcium chloride serving as a catalyst to obtain a thiamphenicol amine organic solution; adding hydrochloric acid or sulfuric acid to the thiamphenicol amine organic solution and acidifying; controlling the pH to 2-3; steaming out a part of the organic solvent at a reduced pressure; cooling and crystallizing; and separating to obtain thiamphenicol amine hydrochloride or thiamphenicol amine sulfate; (2) dissolving thiamphenicol amine hydrochloride or thiamphenicol amine sulfate into the organic solvent; adjusting the pH to be 7 to 7.5 through alkali; performing cyclization reaction with dichloroacetonitrile under 30 to 70 DEG C; cooling and crystallizing after the reaction is done; and separating to obtain the florfenicol intermediate cyclic product. The synthetic method provided by the invention enables the production cycle to be reduced greatly; and the synthetic yield of the florfenicol intermediate cyclic product reaches more than 90.5%.

The invention relates to a hydrochloric acid thiamphenicol aminoacetic acid ester asepsis lyophilized formulation for injection, which is characterized by being prepared through the following steps: adding right amount of water with 0.6-1.3kg of hydrochloric acid thiamphenicol aminoacetic acid esterc, 0-0.2kg of mannite, 0-1000ml of solubilizer, after evenly mixing, replenishing water for injection to 2000-10000ml, and then respectively filling 1000 bottles; according to the thiamphenico, the content of the thiamphenico in each bottle is 0.5-1.0g; the solubilizer is at least one of propanediol, polyethylene glycol and Polysorbate-80. The hydrochloric acid thiamphenicol aminoacetic acid ester asepsis lyophilized formulation for injection adopts packages of tube schering bottle for antibiotic, seal of butyl rubber stopper and aluminum cap, thus being capable of overcoming the shortages existing in solution-typed injection. The lyophilized formulation is white block-shaped objects with loosen texture, can be quickly dissolved by being added with little water (3-10ml), and then the solution after dissolution is added into physiological saline for being clinically applied. The lyophilized formulation has good drug stability, long valid useful-life, convenient clinical use, portability and transportation, thus being a new formulation for the clinical use of the hydrochloric acid thiamphenicol aminoacetic acid ester.

The invention relates to a chiral catalytic synthesis method of thiamphenicol which is a chloramphenicol broad-spectrum antibiotic. Thioanisole serves as an initating raw material, acylation and bromo are achieved, nitrogen iridine containing substituent groups is synthetized, and a qualified product which meets the requirement of drug administration is synthetized through chiral catalytic reduction, oxidizing reaction, acidification loop opening, deprotection and acylation reaction. The chiral catalytic reduction includes that under the action of a catalyst trans-RuC12[(R)-xylbinap][(S)-DPEN], [1-substituent group nitrogen iridine-2-group] [4-(methylthio group) phenyl group] ketone is subjected to hydrogenation reduction to obtain [1-substituent group nitrogen iridine-2-group] [4-(methylthio group) phenyl group] ketone with a high ee value and a high de value. D-methylsulfonylphenyl serine ethyl ester used in industrial production serves as a raw material to synthetize the thiamphenicol, the D-methylsulfonylphenyl serine ethyl ester is obtained through chemical chiral resolution by using a racemic compound, and the other half of the raw material is wasted. According to the unsymmetrical chiral catalytic dynamic reduction method, waste of the other half of the raw material is avoided, the utilization rate of a material is improved, and the production cost is reduced.

The invention provides a method for synthesizing a florfenicol midbody RT0131, which comprises the following steps of: dissolving RT0130 into an aprotic polar solvent and leading RT0130 to generate fluorination reaction under XtalFluor-E and base catalysis so as to generate the florfenicol midbody RT0131. On the other hand, the invention provides a method for generating thiamphenicol into the florfenicol midbody RT0131 through hydrolysis, condensation and fluorination reaction. The method has the advantages of convenience in operation, less by-products, easiness for purification of products and good environmentally-friendly effect.

The invention relates to a compound doxycycline hydrochloride injection for veterinary use and a preparation method thereof. The raw materials comprise doxycycline hydrochloride, thiamphenicol, dexamethasone sodium phosphate, trimethoprim, diclofenac sodium, organic solvent and water for injection. As a special compound preparation for veterinary use, the injection has obvious curative effects on infectious diseases caused by gram-positive bacteria, gram-negative bacteria and mycoplasma, quickly takes effects after the injection is injected into livestock with the diseases, and has special efficacy on mixed infection and severe diseases caused by various pathogenic bacteria and viruses. After intramascular for animals, the injection is easily absorbed, takes effect for a long time and causes little local stimulation. The injection has the advantages of convenient use, short treatment course, low drug resistance, and the like.

The invention discloses a monoclonal antibody for detecting thiamphenicol and florfenicol. The monoclonal antibody is secreted by a hybridoma cell strain TAP / 5F4, the hybridoma cell strain TAP / 5F4 is preserved in the CCTCC (China Center for Type Culture Collection), and the collection number is CCTCC NO: C201549. The invention further discloses an ELISA (enzyme-linked immunosorbent assay) method for detecting thiamphenicol and florfenicol and a kit. Compared with the prior art, the prepared monoclonal antibody has higher sensitivity, high detection accuracy and good precision and has the advantages of simplicity, convenience, quickness, easiness in operation and the like.

The invention provides a carbon quantum dot fluorescent probe and a method for detecting the content of thiamphenicol in food and living cells. The preparation method of the carbon quantum dot fluorescent probe comprises the following steps of (1) crushing the crayfish shells, (2) dispersing the crayfish shell powder in ultrapure water, adding L-cysteine, transferring the mixture into a reaction kettle, and carrying out carbonization treatment at 200 DEG C for 8 hours by adopting a hydrothermal method, and (3) after cooling to room temperature, centrifuging the obtained substance, filtering, collecting supernate, filtering with a 0.22 mum filter membrane, dialyzing and purifying, freeze-drying the obtained solution to obtain carbon quantum dots, and dissolving the carbon quantum dots in water to obtain the carbon quantum dot fluorescent probe. The carbon quantum dot fluorescent probe provided by the invention can be effectively quenched in a static quenching manner, is wide in linear detection range, reasonable in detection limit, high in sensitivity and good in selectivity, can be well applied to rapid detection of trace thiamphenicol residues in food and living cells, and is not interfered by a complex environment.

The invention belongs to the technical field of chemical medicaments, in particular to a synthesis method of florfenicol (1). The method comprises the following steps of: 1, performing fluorination on a compound (II) so as to obtain a compound (III); 2, performing ring opening on the compound (III) under the action of p-toluenesulfonic acid so as to obtain a compound (IV); 3, performing palladium-carbon hydrogenation and deprotection on the compound (IV) in an organic solvent under an acid condition so as to obtain a compound (V); and 4, performing dichloro acetylization on the compound (V) in an organic solvent under the action of alkali so as to obtain the florfenicol (1). The method has the advantages that: the design is novel, the condition is mild, the operation is easy and convenient, and industrial production prospect is obtained.

The invention relates to a synthesis method for stable isotope labeled thiamphenicol and belongs to the field of organic synthesis. The synthesis method for stable isotope labeled thiamphenicol is characterized in that p-bromobenzaldehyde and stable isotope labeled dimethylsulfoxide are taken as raw materials, the raw materials are synthesized to obtain stable isotope labeled p-methylthiobenzaldehyde, oxidization is performed to obtain stable isotope labeled 4-methylsulfonyl benzaldehyde, next, condensation is performed on stable isotope labeled 4-methylsulfonyl benzaldehyde and benzhydrylamine to obtain imine, then imine further reacts with ethyl diazoacetate under the action of (R)-VAPOL and triphenyl borate to build an ethylene imine structure fragment, at last, ring opening is performed on ethylene imine under a dichloroacetic acid condition, an ester group is reduced to synthesize stable isotope labeled thiamphenicol. The raw materials required for synthesis and an intermediate are simple and easily accessible, and the target product (stable isotope labeled thiamphenicol) is high in purity and stable isotope abundance, can be used for internal standard substances for veterinary drug residue test in the food safety field and study of the thiamphenicol metabolic mechanism, and has an important practical application value.

The invention discloses a synthesis method of florfenicol, wherein the method comprises the steps: by using thiamphenicol as a raw material, carrying out cyclization, rearrangement, dehydroxyfluorination and hydrolysis under the action of sulfuryl fluoride to obtain florfenicol. According to the method, sulfuryl fluoride is used as a dehydroxylation fluorination reagent to replace an ishikawa's reagent adopted in an original process, a large number of ishikawa's reagent frameworks which are difficult to recycle and reuse are avoided, a byproduct obtained after sulfuryl fluoride reaction is sulfuric acid, and compared with an ishikawa's reagent byproduct, the treatment difficulty is low, and the treatment process is mature; the process route provided by the invention is simple, thiamphenicol is used as a raw material, and florfenicol can be directly prepared at a medium yield through a one-pot synthesis method.

The invention relates to a preparation method of thiamphenicol by one step synthesis from hydrolysis of D-thero-2-(dichloromethyl)-4,5-dihydro-[p-methylsulfonyl phenyl]-4-oxazole methyl alcohol.

The invention relates to a preparation method of antibiotic, in particular to a preparation method of thiamphenicol. The preparation method comprises the following steps: by weight, dissolving 100 parts of D-4-Methylsulfonylphenyl serine ethyl ester in 500-700 parts of methanol solvent, adding 24-27 parts of KBH4 to react at 30-60 DEG C for 4-8 hours, recycling 300-400 parts of methanol, neutralizing reaction solution with acid to adjust the pH value of the solution to 6-10, adding 42-45 parts of dichloroacetonitrile, performing a cyclization reaction for 4-6 hours, reducing pressure to recycle all of the solution, adding water to perform solid-liquid separation and obtain a solid mixture, adding 600-800 parts of water in the solid mixture, heating to 85-90 DEG C, keeping temperature at 85-90 DEG C for 30 minutes, and discoloring to obtain thiamphenicol. The invention is characterized by fewer steps, simple operation, short reaction time, low cost and the like.

The invention relates to a method for simultaneously screening multiples categories of drug residues in fish by using ultra performance liquid chromatography-quadrupole rod time-of-flight mass spectrometry. The multiples categories of drugs screened simultaneously comprise enrofloxacin, danofloxacin, tetracycline, oxytetracycline , chlortetracycline, doxycycline, chloramphenicol, thiamphenicol, florfenicol, sulfamethoxazole, sulfamethoxazole, sulfathiazole, sulfadiazine, sulfadoxine, sulfisoxazole, sulfaphenirazole, sulfacetamide, sulfamethazine, azithromycin, tilmicosin, medimycin, roxithromycin, acetylspiramycin, doramectin, sudan I, sudan II, sudan III, sudan IV and rhodamine B. By optimizing the parameters of a d-SPE pretreatment method, all target drugs can obtain good recovery rates.29 kinds of target drugs are simultaneously screened by an optimized chromatographic mass spectrometry condition, thereby achieving simultaneous screening of common multiples categories of drug residues in fish. The method has a good application prospect in the field of fish food.

The invention discloses a synthesis process for DL-p-methyl sulfone benzene ethyl serinate water-carrying esterification. The synthesis process comprises the following steps: (1) putting a copper saltand absolute ethyl alcohol into a reactor, dropping sulfuric acid to carry out an esterification reaction, and after the reaction is completed, filtering so as to obtain esterification filtrate; (2)heating the esterification filtrate obtained in the step (1), concentrating, performing water-carrying esterification with the absolute ethyl alcohol, and after the water-carrying esterification is completed, performing aftertreatment, thereby obtaining DL-p-methyl sulfone benzene ethyl serinate. The synthesis process is simple in reaction route, high in product yield, good in synthesis product stability and high in purity, and can be adopted to synthesize a key intermediate of a veterinary drug florfenicol and an antibacterial raw material medicine thiamphenicol.

The invention discloses a thiamphenicol high-sensitivity detection method based on an up-conversion nanomaterial NaYF4: Yb, Er-gold nanoparticle fluorescent probe switch system, and relates to a thiamphenicol detection method. The invention aims to solve the problems that the existing thiamphenicol detection method is low in sensitivity and selectivity, some fluorescent materials excited by ultraviolet and visible wavelengths are relatively strong in background fluorescence in biological analysis and are not beneficial to analysis and detection of biological samples, and the like. The preparation method comprises the following steps: 1, preparing an oleate precursor; 2, preparing NaYF4: Yb, Er; 3, performing surface modification of NaYF4: Yb, Er; 4, preparing gold nanoparticles; 5, preparing the NaYF4: Yb, Er-gold nanoparticle fluorescent probe. The application method comprises the following steps: adding a thiamphenicol standard solution into an incubated NaYF4: Yb, Er-gold nanoparticle fluorescent probe solution, and carrying out fluorescence detection; adding the labeled and treated egg sample into an incubated NaYF4: Yb, Er-gold nanoparticle fluorescent probe solution, and carrying out fluorescence detection. According to the invention, the prepared NaYF4: Yb, Er-gold nanoparticle fluorescent probe is good in fluorescence performance. The established method is good in selectivity, low in detection limit and high in accuracy.

This method discloses a zymochemistry method to synthesize optically active cyanohydrin compounds. By using hydroxyl-cyano lyase HNL---contained in almond, loquat seed, apple seed and Badawood seed to conduct catalytic reaction to obtain a new hydroxyl-cyano compound which can be used to synthesize various compounds such as thiamphenicol, florfenicol, etc..