4 results about "Saxagliptin" patented technology

The invention discloses a saxagliptin crude product and finished product recovery method, which comprises the following steps: (1) concentration process: merging the crude product and the finished product mother liquor, carrying out vacuum concentration at 30-50 DEG C under the vacuum condition of less than or equal to-0.085 MPa to a certain volume, cooling, crystallizing, carrying out suction filtration and drying to obtain a saxagliptin crude product solid with lower purity; and (2) a purification process: carrying out (1) salifying back extraction and impurity removal on the obtained saxagliptin crude product solid, (2) controlling the solution moisture, (3) dripping water for three times to hydrate and precipitate the crude product for impurity removal, and (4) carrying out evaporation solvent impurity removal on a first desolventizing solvent and a second desolventizing solvent, so that the purity of the obtained saxagliptin crude product is greater than or equal to 99.95%. The solid quality of the obtained crude product is better than that of a directly prepared crude product, the cost is saved, and the utilization efficiency of raw materials is improved.

This invention provides a method for detecting related substances in saxagliptin. The method employs high-performance liquid chromatography (HPLC) and includes the following steps: (1) preparation of the test solution and the reference solution; (2) separately measuring the test solution and the reference solution, injecting them into the HPLC instrument, recording the chromatograms, and calculating the percentage content of each related substance in the test solution using the principal component self-comparison method with correction factors. The detection method provided by this invention enables accurate qualitative and quantitative detection of related substances in saxagliptin, with a resolution of 3.75 between impurity A and impurity C, which is beneficial for effective quality control of saxagliptin and thus ensures its clinical safety. The detection method provided by this invention has the advantages of simple operation, high specificity, high sensitivity, and high accuracy.

The invention relates to the technical field of gene engineering and enzyme engineering, in particular to a phenylalanine dehydrogenase mutant and application thereof. The phenylalanine dehydrogenase mutant comprises a PDH-ST mutant or a PDH-SC (Phenylalanine Dehydrogenase) mutant; the amino acid sequence is shown as SEQ ID No. 1 or 2. Compared with a wild type enzyme, the PDH mutant provided by the invention has the advantage that the catalytic performance is obviously improved. In practical application, the conversion rates of the mutant to 2-(3-hydroxy-1-adamantane)-2-oxoacetic acid are 97.4% and 95.9% respectively, the generation rates of a saxagliptin intermediate product are 96.5% and 95.8% respectively and are 1.53 times and 1.52 times of those of a wild type respectively, and the technical bottlenecks of low catalytic efficiency and long conversion period of a natural enzyme are effectively solved.

The application provides a slow-release preparation of saxagliptin and metformin and a preparation method thereof. The slow-release preparation of saxagliptin and metformin has the characteristics of slow release, can maintain sustained release within 24 hours, thereby maintaining a relatively stable blood drug concentration and a longer action time, reducing the frequency of taking medicine, improving the compliance of patients, and having good stability, simple process, high production efficiency and suitability for industrial mass production.