GB508469A - - Google Patents

Abstract

508,469. High - vacuum distillation vitamins. KODAK, Ltd. Nov. 27, 1937, No. 32773. Convention date, Nov. 27, 1936. Drawings to Specification. [Class 32] [Also in Group IV] Oils containing fat-soluble vitamins are subjected to a high-vacuum distillation process in which the oil is first distilled at a pressure below 0À01 mm. of mercury, at least one fraction containing most of the fatty acids at a temperature below 170‹ C. segregated, and fractions of high vitamin ester potency at temperatures between 180 and 240‹ C. collected. The process may be carried out under conditions of molecular distillation and a fraction substan.- tially of vitamin A ester collected at 180‹ C. In practice, components up to 170‹C. (e.g. free fatty acids) are segregated, the fraction distilling between 170 and 195‹ C. collected and returned to fresh incoming oil, fraction of high vitamin potency over the range 195-230‹ C. being collected. In an example, the free fatty acids are removed from cod liver oil by distilling up to 120‹ C. These fatty acids contain a small amount of free vitamins A and D. The fraction at 170‹ contains 50 per cent of fatty acids, 49 per cent of glycerides, cholesterol and 600 U.S.P.X free vitamin D. The fraction at 185‹ C. contains 5-12 per cent of fatty acids, 2,000-3,000 U.S.P.X free vitamin D, and 20,000 U.S.P.X. vitamin A esters per gram. The fraction at 215‹ C. contains 1,500-2,500 U.S.P.X. high-boiling vitamin D, 50,000- 70,000 U.S.P.X. vitamin A ester and 3 per cent of cholesterol. The fraction at 235‹ contains 500-1,500 U.S.P.X. high boiling vitamin D, 20,000 U.S.P.X. units of vitamin A ester and 1 per cent of cholesterol. The fraction at 240‹ C. consists of bland oil. The first fraction may be used as a source of free fatty acids. The second fraction may be filtered, distilled or saponified and extracted to recover the vitamin and cholresterol content. The third fraction is rich in vitamin D and poor in vitamin A and may be neutralized and redistilled to separate the vitamins. The fourth fraction is rich in both vitamin A and D. The two vitamins may be separated by saponifying and distilling off the vitamin D in the non-saponifyable portion. The high boiling vitamin D from the fifth fraction may be obtained by saponification and if necessary, distillation. British Specifications 479,802, 482,880, 482,883, and 487,697, and U.S.A. Specifications 1,942,858 and 1,955,321 are referred to.