SU1616936A1 - Method of extracting kartamine - Google Patents

Abstract

The invention relates to the processing of vegetable raw materials, in particular to the isolation of cartamine from the flowers of safflower, which is used in cosmetics and medicine. The goal is to increase the yield and purity of the target product, as well as simplify the process. The preparation involves the removal of a yellow pigment, extraction with 60-80% ethyl alcohol at a mass ratio of raw material — alcohol 1: 4-6. After removal of the alcohol, the aqueous extract is treated with benzene at an extract-benzene volume ratio of 1: 2-3, and the purification is carried out on a column filled with cellulose-containing compound. The method allows to increase the yield of the target product by 1.6-2.6% with the provision of high quality and eliminates the use of toxic and explosive solvents and the centrifugation stage. 2 tab.

Description

The invention relates to methods for isolating flavonoid compounds and relates, in particular, to a method for obtaining cartamine from safflower dyeing flowers (Carthamus tinctorius), which finds use in cosmetics, medicine, and the food industry.

The purpose of the invention is to increase the yield and purity of the target product, as well as simplify the process.

The method is carried out in the following way.

After the extraction of yellow pigments, 1 kg of safflower flower waste is placed in a 10-liter flask equipped with a stirrer, and 5 liters of 60-80% ethanol are poured in and extracted at room temperature for 2-3 hours. Then the extract is filtered through filter paper on a Buchner funnel. Extraction is repeated 3 times.

The obtained extracts are combined, evaporated at 40-45 ° C on a rotary evaporator until complete removal.

05

about

with

00 O5

alcohol. The evaporated extract (water residue 4.8-5.2 l) is transferred to a separatory funnel and cleaned three to four times with benzene (200-300 ml portions), shaken for 3 minutes,

At the same time, the remainder of the yellow mixtures and fatty substances are transferred to the benzene fraction. After delamination, the lower aqueous layer is dried, passed through a column filled with cellulose, the column is washed with D1 {distilled water to the full y ;; All yellow dye.

The contents in the column are washed with 7 ()% ethanol in the amount of 1.0 l. Cartamine goes into alcohol. (Solution. Alcohol is evaporated, water | 1st residue is poured into a cristoplizer, left in the fridge at A C for 30 min. After making up the scarlet-red prismatic crystals fall out.Water layer is carefully decanned - in another container

dried in REFRIGERATOR1: 1Keo

The yield of cartamine is 38–40 g (3.8–4.0% of 1 kg of raw material (Table 1), the content of the main quantity is 97%, Cartila is determined by the spectrometric method on a F: K-56M photocolorimeter, 490 nm using a calibration graph - Ki standard drug cartamine. The concentration of standard solutions is 0.04-0.20 mg / cm,

I To determine the main substance, weights, 0–2.0 mg, dissolved in 10 cm of 80% ethanol, measured optical density at a wavelength of 490, the concentration of cartamine mg / cm was calculated using a graduated graph and calculated the content of the basic substance according to the formula

y - C - t where m is the weight of the analyzed drug, mg; V is the volume of solution of the drug,

cm ,

Example 1, 1.54 mg of the analyzed preparation is dissolved in 10 cm of 80% ethanol,

D „5 0,760; Cgr 0.150 mg / cm; X 0.i50. ,,,,

Example 2, 1.42 mg of the test substance is dissolved in 10 cm of 80% alcohol.

0

0

0

  0.690; Cgr 0.138 mg / cm;

X - 97 27 l2 j D2 - y /, /: / o.

Preparation of cellulosic material.

The crushed filter paper is placed in a round-bottomed flask, equipped with a stirrer, poured over 2 N, HC1 and heated at constant

stirring until a powdered mass is obtained (about 1 hour). The contents are then filtered on a Büchner funnel through filter paper.

washed with water until neutral. The obtained cellulose is also washed with ethyl alcohol-1 in the amount of 0.5 l and then with acetone in the amount of 0.5 l. The pulp thus prepared is dried in a hood and used to fill the column. The diameter and height of the column 6.5 X 100 cm, the ratio of dry matter to the adsorbent is 1: 5,

5 To clarify the amount of loading the column with cellulose, the percentage of solids in the aqueous solution after the benzene treatment is determined, which is 1.04%. The volume of the aqueous residue is 4.8-5.2 l, the dry matter content is 50.0 -51.2 g. Thus, the column must be filled with 750 g of prepared pulp,

5 Purification of aqueous extract card.

The aqueous extract of cartamine (4.8-5.2 l) is passed through the prepared column in this way, and the column is rinsed with distilled water until the yellow pigment is completely removed (approximately 3 l of water).

The contents of the column are washed with 70% ethyl alcohol (in the amount of 1 l), Cartamine goes into the alcohol solution. The alcohol is evaporated, the aqueous residue is poured into the crystallizer, left in the refrigerator for 30 minutes. After that, scarlet-red prismatic crystals fall out. The aqueous layer is carefully decanted into another dish, and the cartamine is dried in the refrigerator. The output of the map is 38–40 g from 1 kg of raw material. Content of the basic substance is 97.1-97.4%.

The removal of alcohol from the aqueous residue is determined visually by smell, if necessary, the remaining amount of alcohol can be determined by GLC,

The purity of the target product was determined on Silufol plates using a two-dimensional chromatographic method (see Table 2).

Cartamine obtained by the proposed method in the solvent system ethyl alcohol: water 2: 1 gives one spot with Rf - O, 79 ± 0.05; in the solvent system ethyl acetate: ethyl alcohol 3: 2 gives one spot with 0.75 ± 0.03.

Cartamine obtained by the method described in the prototype in the solvent system ethyl alcohol: water 2: 1 gives 3 points with Rf - 0.79 + 0.05, Rf - 0.2110.02, Rf - 0.14 ± 0, OI In the ethyl acetate: ethyl alcohol 3: 2 solvent system, 3 spots with Rf - 0.75 ± 0.03, Rf - 0.56 to, 04, Rf - 0.45 ± 0.03 also appear.

Thus, obtaining cards by the proposed method allows to increase the yield of the target product by 1.6-2.6%, while ensuring high quality, and also to simplify the process by eliminating the use of current.

explosive solvents (tetrahydrofuran, acetone, hexane, hydrogen peroxide) and exclude the centrifugation stage at a temperature

Claims (1)

Formula isob rete n i A method for isolating cartamine from safflower dye flowers, including removing yellow pigment, extraction with an organic solvent, evaporation and purification of the target product, characterized in that, in order to increase the yield and purity of the target product, as well as to simplify the process, the extraction is carried out 60-80% ethyl alcohol at mass ratios of the raw materials: ethyl alcohol 1: 4-6 and after removal of the alcohol, the aqueous extract is treated with benzene at volumetric ratios of the extract: benzene 1: 2-3, and subsequent purification of the target product exist on a column filled with cellulose containing material. Table 1 Effect of process parameters on the output of cartamina 1 2 3 4 5 6 7 : 3: 4: 5: 5: 6: 7: 7 :: rin -... r s 3rsssrj;:; by the method a olast nkah sipu (ShShFG with non-tt-b chkl. On the tongues with ovraeshmi, obtained oo prototapu, vadmkh ptsh equal colors, which belong to the class of lipids. table 2