METHOD OF OBTAINING FAT-SOLUBLE VITAMINS A AND D FROM FISH RAW MATERIALS Russian patent published in 2023 - IPC C11B1/16 

FIELD: pharmaceutical and food industries.

SUBSTANCE: method of producing fat-soluble vitamins A and D from fish raw materials is performed as follows: the raw materials used are cultivated fish species and non-processable fish production waste, while the original chilled raw materials are crushed in an inert gas environment by continuous supply of nitrogen to a container, grinding is carried out with a disperser with rotational speed of the dispersing element 8,000–8,200 rpm for 15 min at a temperature of 20–24°C to obtain a homogenized minced fish, a sample of 10.0 g is taken into a fluoroplastic glass, then 3.4 ml of a 12.5% solution of potassium hydroxide, 3.4 g of ascorbic acid and 134 ml of ethyl alcohol 96% are added to the sample, protein degradation is carried out stepwise continuously for 30 minutes, then mineralization is carried out at a microwave power of 400 W, which is gradually increased to a maximum value of 1,000 W, in three stages at a temperature of 20–90°C with steps of 30°C and a pressure of at least 3 atmospheres in an inert gas environment, while the temperature is raised every 10 minutes, after heating is completed, after 30 minutes, the microwave radiation supply is stopped and the pressure inside the glass is relieved, cooling is carried out in the closed state, without removing from installation for mineralization, to room temperature for 30–40 minutes, after cooling, the glass is removed from the holding device and placed on a shaker for 15 minutes, the resulting hydrolyzed solution is diluted with 67 ml of ethyl alcohol 96% and deionized water in an amount of 300 ml, obtained the solution is transferred to a separating funnel, fat-soluble vitamins are extracted with petroleum ether or n-hexane for 2 minutes, then the mixture is left in a separating funnel at rest for 30 minutes until a clear phase boundary appears, then the phases are separated into different containers, the organic phase contains the final product — vitamins A and D, and the hydrolyzate is subjected to repeated extraction, which is repeated three times with portions of the extractant, 100 ml each, then the combined extract is washed from alkali with portions of ionized water, 150 ml each, until the alkaline reaction of the washings disappears, and then the resulting extract in an organic solvent is filtered through a filter with 5.0 g of anhydrous sodium sulfate, then the solvent is removed using a rotary evaporator at a temperature not exceeding 50°C, the resulting extract is dissolved in isopropyl alcohol.

EFFECT: invention allows to isolate vitamins A and D from fish raw materials as completely as possible.

2 cl, 4 tbl, 3 ex