SU955929A1 - Method of producing chlorophyll derivatives - Google Patents

Description

(54). METHOD OF OBTAINING CHLOROPHYLL DERIVATIVES

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The invention relates to the chemical and pharmaceutical industry and relates to the preparation of biologically active preparations of the galenical type, used in perfumery and cosmetic treatment.

A method of obtaining chlorophyll derivatives from freshly harvested C13 clover plant mass is known.

However, the known method. is complex, MULTIPLE.

Closest to the invention is a method of obtaining chlorophyll derivatives from mint waste after extraction of ground oil, including extraction with an organic solvent, separating the extract, distilling the extractant from it, purifying the extract and isolating the desired product C 23.

The disadvantage of the known method is that the raw material base is rich in dried or dried peppermint and the purity of the target product is low).

The aim of the invention is to expand the raw material base and increase the purity of the target product.

The goal is achieved by the fact that in carrying out the method of obtaining chlorophyll derivatives and raw materials of plant origin, including extraction with an organic solvent, separating the extract, distilling the extractant from it, purifying the extract and isolating the target product, the raw oil raw material is used as a source of raw material. t alcohol containing from 2 to 4 carbon atoms in the chain at a temperature of 65-80 ° C, then 80-86% alcohol is distilled off, the extract is purified and saponified and non-washed chlorine is separated from it rofill15 derivatives and complexes thereof with copper.

The solvent was distilled off from the purified, concentrated alcoholic extract to obtain the unwashed chlorophyll derivatives.

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In order to obtain non-saponified chlorophyll derivatives containing complex bound copper, the purified concentrated alcohol extract is treated with a copper cup.

To obtain saponified chlorophyll derivatives, the purified concentrated alcohol extract is treated with copper sulphate and then

30 of them are silk. The method is carried out in a puffy manner. Spirits are extracted with alcohols of all types of waste aboveground plant mass of any herbal essential oil raw material (mint, sage, eugenic basil geranium, etc., in a wet, dry or ensiled form. Extraction is carried out with alcohols of C at a temperature b5-80 ° C. extraction results in obtaining cella, 80-86% of solvent is distilled off and a concentrated alcoholic extract is obtained. The latter is purified by filtration, filtration or centrifuging, and a purified concentrated extract is obtained, which, depending on the The most recent processing method is a semi-finished product for the preparation of several preparations of a galenic type, containing neomylene chlorophyll derivatives, unwashed Ck-chlorophyll derivatives, saponified chlorophyll derivatives as a solid product or an aqueous paste. preparation containing chlorophyll derivatives, soluble in alcohol, fats and vegetable oils. Output 3.5-6% calculated on the dry weight of plant waste. The content of chlorophyll derivatives 2-6% per dry substance in the preparation. To obtain the unwashed Ch-phlo-derivatives, the purified concentrated alcohol extract is treated with an aqueous solution of copper sulphate, after which the alcohol is distilled off and a beautiful emerald-green preparation is obtained, dissolved in alcohol, fats and vegetable oils. Yield 3.5-6% per dry weight of plant waste. The content of chlorophyll DERIVATIVES 2-6% calculated on the dry weight of the preparation. To obtain the saponified chlorophyll derivatives as a solid. . of the product or aqueous paste, the purified concentrated alcohol extract is treated with an aqueous solution of copper sulphate and washed. In order to liquify alkaline waste water, the purification of the purified alcoholic extract after treatment with vitriol is carried out with alkali, the amount of which. calculated by the number of saponification and the mass of the alcoholic extract at a temperature of 60-80 ° C for 1 h, thus obtaining the saponified alcoholic extract without alkaline wastewater. . Lumpy alcoholic ecg; the tract is concentrated to a pasty state (mass fraction of dry residue 50-60%). Two types of galenic preparations containing chlorophyll saponified derivatives can be obtained from a pasty product. A dark-green, porous solid product, readily soluble in water and alcohol (sodium chlorine), is obtained by vacuum drying, pasty production (yield 1.5-6%, calculated on the dry weight of the raw material, chlorophyll derivatives 2-5% ; A dark-green aqueous paste, soluble in water and alcohol, is obtained by azeotropic distillation of alcohol with water (water is taken in excess / or direct steam. The yield of the desired product is 4-18% calculated on the dry weight of plant residues. Content dry residue in the preparation of 25-65%. The content of chlorophyll derivatives 2–5% based on dry weight. P e m – m 1. Sapted peppermint waste after separation of ground oil by steam distillation (humidity 71.6%, content of chlorophyll derivatives 0.29%) ethyl alcohol at the rate of (1: 5 and carry out the extraction for 1 h at 65 ° C. The resulting alcohol miscella is concentrated, distilling off 80% of alcohol, filtratot. The precipitate is washed with 9% ethyl alcohol, mixed with a filtrate, solvent is distilled off and a galenic type preparation containing non-saponous chlorine derivatives is obtained. Profil in the amount of 6%. . The yield of the drug is 3.5% calculated on the dry weight of waste mt. The product is burying soluble in alcohol, fats and vegetable oils. EXAMPLE 2: Silted waste of peppermint after separation of ground oil (humidity 77.6%, content of chlorophyll derivatives 0.297%) is extracted with iso-propyl alcohol at 70 s at the rate of (1: 5). The resulting sponge miscella is concentrated, 86% alcohol is distilled off, then the alcohol-insoluble precipitate is separated using a centrifuge. Copper sulphate is added to the purified concentrated alcoholic extract at the rate of 0.005 parts by weight. on 1 weight. dry residue. In the bottom residue, a preparation of a galenical type is obtained containing 5% of the unsaturated C-derivatives of chlorophyll. The yield of the drug is 4% based on the dry weight of waste mt. The product is emerald green, well soluble in alcohol and vegetable oils. Example 3. The silo waste of E1 peppermint mite is strained with n-butanol at a temperature. The butanol miscella is concentrated by distilling off 85% of buTanol, washed with water, copper sulphate is added and solvent residues are completely distilled off. A galenic-type preparation containing non-cleavable chlorophyll derivatives containing 5% of copper is obtained. Output b% in the calculation of the dry weight of vegetable raw materials. The drug is an emerald green product, highly soluble in alcohol, fats and vegetable oils. PRI me R 4. Dried sage waste after extraction with petroleum ether (chlorophyll content 0.175%) is extracted with butanol 1: 5 at a temperature of 80 ° G. The resulting butanol miscella is concentrated, the distillate is distilled with 80% butanol, and water is applied to form a purified concentrated butanol extract (M), in which the saponification number (, p. O) is determined. The amount of alkali (P) is then calculated, which is necessary to omniplate the extract according to the following formula: p - h. X 0.71 M IQOO where P is the weight of NaOH, g (the calculated amount of alkali for saponification) part. - saponification number, mg / g} M - the weight of the purified concentrated butanol extract, g. To the purified concentrated butanol extract, add the added vitriol (based on 0.005-0.01 for 1 hour, dry residue), the calculated amount of alkali and sap at a temperature of 60-70 ° C for 1 hour. The washed-through butanol extract is concentrated to a state of butanol paste, then 2-2.5 volumes of softened water are poured and butanol is removed as azeotropic butanol: water mixture. In the cube, there remains a marketable product — aqueous sodium chlorine paste. The yield of 4.43% based on the dry weight of plant waste. The dry matter content is 49.1% in sodium chlorine paste. The content of chlorophyll derivatives in the paste is 4.15% calculated on the dry weight. EXAMPLE 5: Silted waste of peppermint after separation of ground oil (humidity 71.6%, content of chlorrillin derivatives Q, 297%) is extracted with n-butanol at. The resulting butanol miscella is concentrated by distilling off 85% of butanol, washed and saped as in Example 4. The washed butanol extract is concentrated to a paste. The butanol paste is dried in a vacuum oven (t. 60-80s, residual, pressure 100-600 mm Hg) without the smell of butanol. You get a solid product of dark green color, soluble in water and alcohol; pH of an aqueous solution of 8.5; the content of saponified chlorophyll derivatives is 5.1%. The yield of the target product. 4,2% based on the absolutely dry weight of plant waste. Example 6, Dried vegetable waste — The transient mint is extracted with butanol (1: 5) at temperature. The resulting butanol miscella is concentrated, 80% butanol is distilled off, washed with water, then washed as in Example 4. The washed up butanol extract is concentrated to a paste, 2-2.5 parts of water are poured into the obtained butanol paste and distilled butyl. alcohol in the form of an azeotropic mixture (water: butanol) to the absence of the smell of butanol. In this case, a preparation is obtained in the form of an aqueous paste containing 50% water and 2% of the total chlorophyll derivatives (4% calculated on the dry weight of the paste). The yield of the target product is 8.5% based on the dry weight of the raw material. Other examples illustrating the possibility of obtaining preparations containing chlorophyll derivatives from various types of plant waste of herbal essential oil raw materials using various solvents are given in Table. one.

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The proposed method, in addition to expanding the raw material base, allows to obtain a product of higher purity.

The purity indicators of preparations containing chlorophyll are the clear nature of the major peaks, in particular for water-soluble chlorophyll derivatives containing complex-bound copper (chlorine

sodium) the first maximum (L) in the region of 405 i 5 nm and the sec, the second maximum in the region of 630 ± 5 nm, as well as the magnitude. 3.4 to 3.9 na

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in tab. 2 shows a comparative description of the preparations obtained by the known and proposed methods. Both samples are obtained from the same raw material.

Table 2

Claims (4)

Claim 1. A method of obtaining derivatives of chlorophyll IE of raw materials of plant origin, including extraction with an organic solvent, separating the extract, distilling the extractant from it, purifying the extract and isolating the target product, characterized in that, in order to expand the raw material base and increase the purity of the target product, the source of raw materials use wastes of essential oil raw materials, while the extraction is carried out with alcohol containing in the chain from 2 to 4 carbon atoms at 65-80 ° C, then 80-86% alcohol is distilled off, the extract is purified and isolated and It contains pollinated, unsaponifiable derivatives of chlorophyll and its complexes with copper. 2. The method of pop. 1, characterized in that, in order to obtain unsaponifiable derivatives of chlorophyll, from a purified concentrated alcohol solvent. 3. The method according to which the unsaponified phyll containing complex-bound copper is purified, the purified concentrated alcoholic extract is treated with copper sulfate. 4. The method of pop. 1, it is distinguished by the fact that, in order to obtain saponified chlorophyll derivatives, the purified concentrated alcoholic extract is treated with copper sulphate and then saponified with alkali.