Preparation of APIs
Technique 1. Alcohol-alkali saponification technique
Prep work of saponification remedy Take pig heart deposit, press completely dry and also consider, add 300g/L industrial pyrogallic acid according to the weight of the dry deposit, stir well, add alcohol-alkali solution (3-3.5 times the quantity of ethanol, 320g/L of the completely dry deposit) Salt hydroxide), warmed as well as mixed to reflux for 25-30min, rapidly cooled to area temperature to acquire a saponified remedy. Pig heart deposit [NaOH] → [Pyrogallic acid, ethanol] Preparation of saponification liquid concentrate Take the saponification fluid, promptly add 1/10 of its volume of petroleum ether or 120 # fuel to extract 3-4 times, mix, layer, get the essence. Clean with water until virtually neutral, concentrate to 1/10 of the initial volume at listed below 40 ° C, amazing, allow stand overnight below -5 ° C, as well as filter to get a focused remedy. Saponification option [oil ether] → extraction remedy [< 40 ℃] → concentrate Ubidecarenone Preparation of refined items The concentrate went through silica gel column chromatography, eluted with oil ether and 10% ether-petroleum ether together, and the eluate was collected, The solvent was recovered to obtain a yellow oil. Dissolve in outright ethanol by heating, filter, stand the filtrate, crystallize by cooling, and dry in vacuum to acquire Ubidecarenone refined product Concentrate [silica gel column, ether-petroleum ether] → eluent [absolute ethanol] → Ubidecarenone refined item.
Approach 2, alcohol-ether mixed solvent extraction method
Preparation of Ubidecarenone Crude item Take the pig heart residue,add 1.5 times the amount of V ethanol: V ether = 3:1 mixed solvent, add Chemicalbook to heat for 3-4 times, each 15-20min, cool to room temperature, filter, and extract together liquid. Concentrate, add appropriate amount of water, add petroleum ether for extraction, concentrate the extract, and the concentrate is a yellow oily product, namely Ubidecarenone crude product. Preparation of Ubidecarenone Finished Ubidecarenone Take the crude Ubidecarenone product, dissolve it in acetone, set it to below -10°C to separate out impurities, filter, evaporate the filtrate to remove acetone, add a small amount of petroleum ether to dissolve, separate it by silica gel column chromatography, add anhydrous ethanol to crystallize, and obtain coenzyme Q10 finished product. Ubidecarenone crude product [silica column] → [acetone, anhydrous ethanol] Coenzyme Q10 finished product
Method 3. Use beef heart slag as raw material
Beef heart dregs [10%NaOH-80% ethanol]→brown black solution [extraction]→gasoline extract [washing]→orange butter layer [concentration]→Ubidecarenone crude product [fat separation]→clear oil layer [column chromatography]→ Ubidecarenone eluent [frozen, concentrated] → orange-yellow oil [crystal dry] → coenzyme Q10 finished product injection Properties This product is a yellow and clear liquid, with the prolongation of storage time, there will be orange-yellow precipitation, which can be heated in hot water A few minutes, shake to dissolve, does not affect the curative effect. The stability of this crystal is poor. When placed for 3-6 months, the content decreases by about 3%-5%, and the highest is more than 8%. However, the rate of decrease of the content becomes slower with the passage of time. Preparation This product is a sterile aqueous solution made of Ubidecarenone and Tween-80 or other cosolvents.
