RU1814057C - Method of fepranone quantitative determination - Google Patents

Abstract

Usage - in the field of analytical chemistry. The essence of the invention: the formation of the ionic associate of fepranone and acid violet anthraquinone dye, its extraction with chloroform from an acidic medium, destruction with an alkali solution, followed by measurement of the optical density of the liberated dye. 4 tab. 1 silt

Description

The invention relates to analytical chemistry, in particular to methods for the quantitative determination of fepranone - diethylaminopropiophenone hydrochloride - by the extraction-photometric method and can be used in pharmaceutical analysis for the quantitative determination of a drug in a substance, in dosage forms and in biological objects.

The aim of the invention is to increase the accuracy and sensitivity of the determination of fepranone, as well as expanding the range of analyzed objects.

For the quantification of fepranone, a standard aqueous solution containing 1 ml of 0.1 mg of this preparation is used. As a reagent, a 0.02% aqueous solution of acid violet anthraquinone dye 1-hydroxy-9,10-anthraquinone-4-amino (m-tolylsulfonic acid) is used, in an acidic medium with fepranone forming a colored ion associate, which in that chloroform is used to recover the medium. A universal buffer mixture was used to create a specific pH of the medium. In a chloroform extract, when treated with a solution of alkali, the ionic associate of fepranone and dye is destroyed. The liberated dye passes into the alkaline solution; the amount of which is equivalent to the amount of fepranone interacting with it.

Acid violet anthraquinone dye is used in analytical chemistry for the determination of inorganic substances. For the quantification of fepranone, an acid violet anthraquinone dye has been proposed for the first time.

Data on the selection of optimal conditions for the quantification of fepranone are presented in Table. T and 2.

From the results given in table. 1, it follows that the ionic associate of fepranone and the reagent in the largest quantities is extracted with chloroform at pH 2-5. Further studies used

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solution of universal buffer mixture with a pH of 3.0.

From the data given in table. 2, it follows that in order to completely form an ionic associate between fepranone and the reagent, it is necessary to add 1.4-2.4 ml of a 0.02% solution of acid violet anthraquinone dye. In further studies, 2 ml of a solution of the indicated reagent was added.

It was found that in order to achieve optimal conditions for the quantitative determination of fepranone, based on the interaction of the drug with the acid violet anthraquinone dye, it is necessary to take 1-2 ml of a solution of fepranone containing 0.02-0.1 mg of this drug in this volume, 6-7 ml of solution universal buffer mixture with a pH of 3.0, 2 ml of a 0.02% solution of reagent and 10 ml of chloroform.

The dependence of the optical density of the test solution on the amount of fepranone in it is illustrated by a calibration graph where the amount of fepranone (C) is plotted horizontally and vertical. optical density value (D).

The solution has significant differences, since the totality of analytical features in other technical solutions was not found. The proposed solution allows to increase the sensitivity of the determination and expand the scope.

The invention is illustrated by specific examples.

Example 1. Determination of fepranone in a substance.

1 ml of an aqueous solution of fepranone (0.02-0.1 ml per sample) is added to the separatory funnel, 7 ml of a universal buffer mixture with pH 3.0, 2 ml of a 0.02% aqueous solution of the reagent and 10 ml are added chloroform. The mixture was shaken for 3 minutes, then allowed to separate phases for 10 minutes. After phase separation. the chloroform layer was transferred to a separatory funnel containing 12 ml of 0.1 N. sodium hydroxide solution and shaken for 10-15 seconds. After the phases have settled, the colored alkaline solution is separated. The optical density of the colored alkaline solution was measured using a KFK-2 photoelectrocolorimeter (light filter at A 590 ± 10 nm, cuvette 20 mm). As a comparison solution, 0.1 N was taken. sodium hydroxide solution.

Construction of a calibration graph. 0.2 are added to the separatory funnels; 0.4; 0.6; 0.8: 1.0 ml of a standard solution of fepranone, 1 ml of which contains 0.1 mg of the drug. Then, BC solution (pH 3.0) up to 8 ml, 2 ml of a 0.02% solution of reagent, 10 ml of chloroform are added to all separatory funnels, and proceed as described above.

Use the obtained optical density values (Table 3), and build a calibration graph. Subordination to the Bouguer-Lambert-Beer law is observed in the range of fepranone concentrations from 0.02 to

0.1 mg / ml.

Using a calibration graph, the amount of drug to be analyzed is determined. This method can be used to quantify fepranone.

both in substance and in tablets.

Example 2. Quantitative determination of fepranone in pellets at 0.025. One dragee is weighed and placed in a volumetric flask: a 250 ml flask, dissolved and adjusted to the mark with distilled water.

1 ml of a solution of the analyzed preparation, 7 ml of UBS (pH 3.0) and 2 ml of a 0.02% reagent solution are introduced into the separatory funnel. Then proceed analogously to example 1,

The calculation of the concentration of fepranone in pills can be made not only according to the calibration schedule, but also according to the following formula:

thirty

Oh

Dx a0

Do

where Do is the optical density of the standard solution;

Dx is the optical density of the test sample;

a0 is the content of fepranone in 1 ml of a standard solution.

Preparation of a standard solution.

0.025 g of the substance fepranone is placed in a 250 ml volumetric flask and dissolved in 100 ml of distilled water, the volume of the solution is adjusted to the mark with water. 1 ml of standard solution was taken for analysis.

The assessment of the quantitative determination of fepranone in the substance and pellets of the proposed method is presented in table. 4.

PRI me R 3. The definition of fepranone in biological material.

10 mg of fepranone was added to 100 g of the finely divided corpse liver and left for 1 day with periodic stirring.

The studied preparation was isolated from the liver three times with water acidified with oxalic acid to pH 2.0. The combined extracts were filtered through 4-5 layers of gauze and centrifuged. Fepranone from extracts was extracted with chloroform from an alkaline medium (pH 8.0–9.0). The dry residue of the extracts after distillation of chloroform was dissolved in 20 ml of universal buffer mixture (pH 3.0). For quantification, 1-2 ml of this solution was taken and then acted as described in Example 1. After determining the optical density, the amount of fepranone extracted from the biological material was calculated according to a calibration graph. Impurities isolated together with fepranone from biological material do not interact with the reagent and do not interfere with the determination of fepranone isolated from biological material.

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Claims (1)

SUMMARY OF THE INVENTION A method for quantitative determination of fepranone by dissolving an analyzed sample in water, processing the resulting solution with a color reagent, followed by extraction with chloroform and photometric measurement, characterized in that, in order to increase the accuracy, sensitivity and expand the scope of the method, acid violet anthraquinone is used as a color reagent. dye, processing it is carried out in the presence of a universal buffer solution at pH 2.0-5.0, the chloroform extract is treated with water th hydroxide solution and subjected to photometry sodium aqueous layer. .Table 1 The dependence of the optical density on the pH of the universal buffer mixture (UBS) Table 2 The dependence of the optical density on the volume of a 0.02% reagent solution Table 3 The dependence of the optical density of the colored solutions on the amount of fepranon TABLE 4 Results of determination of fepranone in the substance of willows and pellets at 0.025  A sample of the preparation, determined in the substance, was dissolved in 100 ml of water, 1 ml of the resulting solution was taken for analysis.