SU857096A1 - Method of separating lipids and polythyleneoxides - Google Patents

Description

The invention relates to organic chemistry, in particular to the separation and purification of fats and fatty substances (LIPIDS) from mixtures with other organic substances, and may find application in chemical, light industry, pharmacology and health care. Mixtures of LIPIDS and polypeioxides are used in various fields of industry — in the manufacture of lubricants, emollients, antistatic agents, paints in pharmacology — in the manufacture of ointments, solubilizers, suspensions, emulsions; in perfumery - in the manufacture of creams, cosmetics, lipsticks, lotions, in health care - in low-temperature preservation of tissues, as well as in scientific research. However, there is a need to separate 1B1 mixtures of lipids and polyethylene oxides, for example for cleaning and repeating qualitative and quantitative composition. Lime is a method of extracting and isolating lipids from various objects with organic solvents and solvent systems. According to the most widely applied method of Folch in the Bly and Dyer modification, lipids are extracted in a single phase solvent system. n water Cl: 1: 0.9). The chloroform lipid solution is then separated and purified by evaporation of the solvent and redistributing lipids in chloroform. However, such methods do not provide for the separation of lipids and polyethylene oxides when they are present in the extractable material. The purpose of the invention is to improve the quality of the separation of lipids and polyethylene oxides. This goal is achieved by the fact that, according to the method of separation of lipids and polyethylene oxides using a two-phase solvent system extraction, a mixture of petroleum and diethyl ethers is used as a two-phase solvent system at a volume ratio of 1: / 0.3-1 and aqueous 35-100% of obscene A solution of CACEPI with a volume ratio of the phases of organic and inorganic solvents of 1: 0.5–5–5. An emulsion containing lipids and polyethylene oxide of 400-40000 mol. Weight is mixed with petroleum and diethyl ether at a solvent ratio of 1: 0.3-1 and the mixture is diluted with 0.5-5 volumes of a saturated solution of inorganic acid. . The mixture was shaken for 5-10 minutes and allowed to settle. After the solvents were settled, the lower layer was removed and the upper layer was washed with a fresh portion of 40-100% of the inorganic acid salt solution. The solution of lipids in the composition of the upper layer of solvents is freed from the solvent by evaporation in a stream of nitrogen. The water-salt solutions of polyethylene oxides in the composition of the lower layer of solvents and the washing liquids are evaporated. The polyethylene oxides are dissolved in alcohol and evaporated. Example. An emulsion of lipids (30 mg each of lactic acid, neutral fats, cholesterol) and polyethylene oxides (PEO) (90 mg of a mixture of 400, M..V, 6000, mv, 40,000) in 200 mg of water is placed in a separating funnel, mixed with 10 ml of petroleum and 10 ml of diethyl ether and 20 m of 35% sodium chloride solution are added, the mixture is shaken for 5 minutes, settled for 15 minutes, then the lower layer is drained and the upper layer is washed with an equal volume of 35% NC C. The ether solution of pipids is evaporated into a stream of nitrogen to obtain a lipid mass in the amount of 99.5% of the original. The water-saline solution of PEO is evaporated, and the residue is dissolved in alcohol and evaporated to obtain ROG in the amount of 99.2% of the original. Table 1 shows the distribution of lipids and polyethylene oxide B (PEO) two-phase solvent systems. The residue obtained after evaporation of the organic solvent phase is suspended. The sample is extracted twice (1:10) with petroleum ether and centrifuged. The petroleum extract is soared until the solvent contains non-polar lipids weighed. The centrifugal pellet is dissolved in 10 ml of chloroform and samples of 0.5i ml are collected. determination of ectin on phosphorus and cholesterol on the reaction with acetic anhydride. On the basis of the data obtained, the lipid content in the polar and non-solubilized phases is calculated. A phase of an incomplete solvent upper ether layer: L 10 (a-b) + D P I - L Phase of polar solvents Bottom NII water-salt layer: lCo-l where L and L are mg of lipids; P - P- mg PEO; a - mg of licitin in a sample of chloroform. in - mg of cholesterol in a sample of chloroform: d - mg of lipids in a petroleum extract; n - mg residue from the solvent. The results of Table 1 show that in a known method the separation of lipids is not achieved (in the phase of the non-Phixix solvent there are 84.6% and in the phase of polar solvents 15.4%). Also, separation of polyethylene oxides is not achieved (in the phases, respectively, 35.4% and 64.6% are contained). In the proposed method, almost complete separation of lipids and polyethylene oxides is achieved. Table 2 presents the distribution of lipids and polyethylene oxides (PEO | in the solution system Petroleum ether-diethyl ether-an aqueous solution of sodium chloride. Thus, the method provides a quantitative separation of lipids and polyethylene oxides and is carried out for 40-60 minutes with inexpensive reagents and without the use of sophisticated equipment.

Solvents and the ratio of their volumes

1. Known solvent system for lipid isolation: chloroform-methanol-water (1: 1: 0.9)

2. Solvent system of the proposed method: petroleum ether-diethyl ether-saturated solution of sodium chloride (1: 0.5-5)

Table 1

Phase

solvent solvents

lipids,% I PEO, X,

PEO,%

84.6

35, 4

64.6

15.4

99.5

0.8

99.2

0.5

Table 2

Claims (1)

saturation of NaCC solution with a volume ratio of phases of organic and inorganic solvents 1: 0.5-5. A method for the separation of lipids and polyethylene oxides using extraction with a two-phase solvent system characterized in that, in order to improve the quality of separation of these substances, a mixture of petroleum and diethyl ethers is used as a two-phase solvent system with a volumetric ratio