Indaconitone sand fried product, preparation method and application thereof
A technology for processing indoculine and cuconitine, which is applied in the field of medicinal chemistry, can solve the problems of different toxicity and efficacy, lack of quantitative quality control indicators, and reduced toxicity, and achieve excellent treatment of arrhythmias, good application prospects, and reduced toxicity. toxic effect
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Embodiment 1
[0056] Example 1. Screening of process parameters for the processing of indomethacin
[0057] 1. Chromatographic conditions
[0058] Chromatographic column: COSMOSIL PAK 5C18-MS-II (4.6mm×250mm, 5μm); mobile phase: acetonitrile-0.03mol / L ammonium bicarbonate solution (concentrated ammonia adjusted to pH 9.5) (43:57) isocratic elution; column Temperature: 35°C; Flow rate: 1.0 mL / min; Detection wavelength: 230 nm.
[0059] 2. Preparation of reference solution
[0060] Take 46 mg of the reference substance of Indomethacin, accurately weigh it, place it in a 100 mL measuring flask, and add dichloromethane to make a reaction stock solution with a concentration of 0.4626 mg / mL. Take 4mL of the reaction stock solution, place it in a 10mL volumetric flask, evaporate the solvent, add 0.1% hydrochloric acid-methanol to make a constant volume to make a 0.185mg / mL reference solution, shake well, and pass through a microporous membrane (0.45μm), Take the continuous filtrate to obtain the referen...
Embodiment 2
[0077] Example 2. Separation and structural identification of the processed and transformed components of incoconutine
[0078] 1. Column chromatography separation sample preparation
[0079] Take 520mg of indomethamine, put it in a 250ml round-bottom flask, add 100ml of dichloromethane to dissolve it, and use a rotary film evaporator to evaporate the solvent at 40℃ to make the indomethine evenly adhere to the inner wall of the round bottom flask, In an oil bath at ℃ for 30 minutes, take it out and let it cool to obtain the processed product (450mg) of indomethacin, which is used for the column.
[0080] 2. Separation and purification
[0081] Carry out silica gel column chromatography (200-300 mesh, 120g) on the processed product of invoxine, and elution gradient of petroleum ether-acetone-triethylamine (8:1:0.01, 6:1:0.01, 3:1:0.01) , Each gradient is 1.5L, the thin-layer plate is inspected, and the fractions containing compound 1 are combined to obtain component B. Component B ...
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