36 results about "Milbemycin oxime" patented technology

The present invention provides a method for synthesizing Milbemycin oxime. The method comprises the following steps. (1) Oxidizing reaction: oxidizing Milbemycin, using hypochlorite or chlorite as oxidizers and piperidine nitrogen oxygen free radicals as the catalyst and halide as the catalyst promoter. The oxidation reaction is conducted in a dichloromethane solvent for 0.5-4 hours at −5-15° C. to produce the intermediate product Milbemycin ketone. (2) Oximation reaction: reacting the Milbemycin ketone with a hydroxylamine hydrochloride oximation agent in a 1,4-dioxane reaction solvent for 10-16 hours at 25-35° C. to obtain Milbemycin oxime. The method provided by the present invention realized the industrial production of Milbemycin oxime for the first time domestically. Moreover, the yield of the prepared product is higher than competing products both at home and abroad.

The invention discloses a method for preparing high-purity milbemycin. After extracting milbemycin A3 and milbemycin A4 from fermentation broth and preliminarily purifying them, they are oxidized with an oxidizing agent with low oxidation activity and subjected to silica gel chromatography. Increase the content of milbemycin A3 ketone and milbemycin A4 ketone from less than 25% to more than 75%, and naturally precipitate crystals during the concentration process, making milbemycin A3 ketone and milbemycin A4 ketone The content of milbemycin A3 oxime and milbemycin A4 oxime is adjusted to be 1:4 by resin chromatography, and the content of the product can be improved to More than 98%. The whole process is relatively simple, requires less equipment, has good versatility, and is suitable for large-scale industrial production.

The invention relates to a phage antibody library which assembles an ScFv gene fragment between Restriction Enzyme cutting sites of SfiI and NotI of a pCANTAB5E carrier. The phage antibody library is characterized in that the ScFv gene fragment can be affinitive and enriched with antigens of 16-membered macrolide agricultural chemicals to form a soluble single-chain antibody and the phage antibody library is applied to immunoassay of pesticide residue. The phage antibody library has the advantages that the antibody with high affinity can be obtained without animal immunization, the test period is short, the antibody library is the phage antibody library which takes small molecular milbemycin oxime of a 16-membered macrolide generic structure as immunogen to construct, the antibody librarytheoretically can directly obtain a specific antibody library of 16-membered macrolide compound through screening, the screening flux is high, the efficiency is high, the specificity is strong, and the affinity selecting range is wide, so that the phage antibody library has wide application prospect in the aspects such as agricultural chemical antibody preparation, testing technique development and the like.

The invention provides a preparation method of milbemycin oxime. The preparation method of milbemycin oxime comprises the following steps: extracting milbemycins, namely taking milbe mycelia obtained through fermentation as a raw material, extracting, concentrating, extracting, concentrating, extracting again and concentrating again, so as to obtain milbemycin; preparing milbemycin ketone, namely taking the milbemycin as a raw material, establishing an oxidation reaction system, after reaction is finished, filtering, concentrating, extracting and concentrating the reaction system, so as to obtain an intermediate product milbemycin ketone; synthesizing milbemycin oxime, namely dissolving milbemycin ketone with methanol and dioxane, dropwise adding hydroxylamine hydrochloride solution and reacting, concentrating the reaction system, extracting, drying and concentrating, so as to obtain a milbemycin oxime crude product; and purifying milbemycin oxime, namely crystallizing the milbemycin oxime crude product with a mixed solvent of trichloromethane and normal heptane, dissolving a crystalline product with ethanol, dropwise adding into water while stirring for carrying out crystallization, filtering, and drying, so that the milbemycin oxime finished product is obtained. The preparation method of the milbemycin oxime has the advantages that productivity is greatly improved, and cost is obviously reduced, so that the preparation method provided by the invention is obviously better than an existing preparation method.

The invention discloses a panda epidermis insect repellent spray and a preparation method thereof. The spray is prepared from the following components in parts by weight: 18 to 25 parts of minoxidil,10 to 20 parts of stearic acid, 8 to 13 parts of polyethylene glycol, 22 to 34 parts of milbemycin oxime, 8 to 15 parts of tea leaves, 7 to 18 parts of ivory crumbs, 11 to 21 parts of bead tree bark,10 to 16 parts of cotex dictamni, 3 to 6 parts of seaweed, 3 to 5 parts of fructus xanthii, 2 to 6 parts of folium artemisiae argyi, 4 to 7 parts of honeycomb, 8 to 16 parts of galla chinensis, 2 to 3parts of dioctyl sulfosuccinate sodium salt, and 1 to 2 parts of fatty alcohol-polyoxyethylene ether. The spray can be used for quickly expelling insects and relieving itching, is durable in effect and not easy to recur, and has no toxic and side effects on pandas at the same time.

The invention provides a milbemycin oxime separation and purification method. The milbemycin oxime separation and purification method comprises the following steps: carrying out crude separation on a sample to be separated through silicagel column chromatography, wherein the silicagel column chromatography adopts wet-process column packing and dry-method sample loading; purifying the product after crude separation by high performance liquid chromatography; concentrating the purified sample by a nanofiltration membrane to obtain concentrated solution; performing reduced-pressure vaporization to the concentrated solution, filtering and drying to obtain a refined product; dissolving the refined product, heating up, dropwise adding isooctyl alcohol, normal heptane or petroleum ether, cooling to be crystallized, and filtering to obtain a crystallized product; dissolving the crystallized product, filtering, dropwise adding filtrate into purified water stirred constantly, after dropwise adding, carrying out suction filtration to obtain a crystal transformation product; drying the crystal transformation product, crushing, and drying again to obtain milbemycin oxime finished product. The method can realize industrial production of milbemycin oxime in China firstly, and the product has high purity and high yield which are higher than those of the similar products at home and abroad.

The invention relates to a purification method of a milbemycin oxime crude product. The method includes the process steps that firstly, the milbemycin oxime crude product is washed at the pH of 8-9; then, a milbemycin oxime wet product obtained after filtering is dissolved in butyl acetate or isobutyl acetate and then decolored with macroporous resin, water is added for mixing, standing layering and filtering are carried out, obtained filter liquor is dried with anhydrous calcium chloride, filter liquor is collected after filtering, water is added again for mixing, filtering and drying are carried out after heating crystallization, and a milbemycin oxime pure product can be obtained. By means of the method, impurities in the milbemycin oxime crude product are effectively separated, the quality of the finished product is improved, and the home and abroad market competiveness of the product is easily enhanced.