SU1695191A1 - Method for determining 6-(phenoxyacetoamido)-penicilane acid - Google Patents

Abstract

The invention relates to analytical chemistry, to a method for the determination of 6- (phenoxy-acetamido) -penicillanic acid. The purpose of the invention is to increase the sensitivity, accuracy and selectivity of the determination. For this, the analyzed sample is dissolved in chloroform, treated with an aqueous solution of N, N, N1, N1 - tetramethylthionine chloride at pH 6.5-6.7, the colored product is extracted with chloroform, the extract is separated and photometric.

Description

This invention relates to analytical chemistry, and specifically to methods for determining 6- (phenoxyacetamido) -penicillin therapy, and can be applied to. the practice of factory control and analytical laboratories, central factory laboratories of chemical enterprises.

The purpose of the invention is to increase the sensitivity, selectivity and accuracy of determination.

The method is carried out as follows.

The sample to be analyzed is dissolved in chloroform, treated with 0.05% N, N, N1 aqueous solution, in α-tetramethyltionine chloride at pH 6.5-6.7, the colored product formed is extracted with chloroform, the extract is separated and photo is metric.

PRI me R 1. Qualitative determination of 6- (phenoxyacetamido) -penicillanic acid.

About 2 mg of 6- (phenoxyacetamido) penicillanic acid was added to the tube and dissolved in 5 ml of chloroform. To the resulting solution was added 1 ml of a 0.05% solution of N, N, N, N-tetramethylthionine chloride, 9 ml of a buffer solution with a pH of 6.5-6.7 and shaken the reaction mixture for 3 minutes. The chloroform layer thus acquired a blue color. Sensitivity reaction 0.5 µg / ml.

PRI mme R 2. Quantitative determination of 6- (phenoxyacetamido) -penicillanic acid.

Build a calibration graph.

9.75, 9.50, 9.00, 8.50, 8.00, 7.50 ml of chloroform were added to the six separatory funnels, respectively, 0.25, 0.50, 1.00, 1.50, 2.00, 2.50 ml 0.25% solution of 6- (phenoxyacetamido) -penicillanic acid in chloroform, 4 ml of a buffer solution each with a pH of 6.5-6.7 and 1 ml of a 0.05% solution of M. Mm. M-tetramethylthionine chloride , Contents of funnels inhiva (L

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3 min, stained with chloroform. The extracts were separated and photometrized at a wavelength of 590 nm (light filter No. 7) on a KFK-2 instrument. Measurements were carried out in cuvettes with a working layer thickness of 20 mm against the background of the solution obtained in the control experiment. According to the measurement results, a calibration graph was built. The light absorption of the colored solutions follows the Bouguer-Lambert-Berz law in the concentration range of 0.5-5.0 μg / ml. Using the least squares method, we calculated the equation kafln6poB04Horo of the graph, which in this Case was:

D - 0.0564-0 + 0.0498, where D is the optical density;

C is the concentration of the analyte in the photometric solution in µg / ml.

- Method of quantitative determination.

About 0.025 g of 6- {phenoxyacetamido) -phenyl and cyllanic acid (exact weight) were dissolved in chloroform in a 100 ml volumetric flask. 1.5 ml of the resulting solution was added to a separatory funnel, to which 8.5 ml of chloroform was previously introduced. To the solution in the funnel was added 4 ml of a buffer solution with a pH of 6.5-6.7, 1 ml of a 0.05% solution of N, N, Nl, N-tetramethylthionine chloride and further operations were carried out according to the scheme described to build a calibration graph. Determination of the amount of 6- (phenoxyacetamido) -penicillan

the acids were carried out according to the equation of the calibration graph and recalculated to the weighed. The relative determination error was ± 3.36%.

The method allows to determine 6- (phenoxyacetamido) -penicillanic acid in the presence of a number of structurally derived 6-aminopenicillanic acid: disodium salt of 6- (a-carboxyphenylacetamido) -phenicillanic acid; sodium salt of 6- (2,6-dimethoxybenzamido) -penicillanic acid; 6- (a-amino-phenylacetamido) -penicillanic acid; sodium (potassium) salt of 6- (phenylacetamido) -penicillanic acid,

Claims (1)

Claims of Invention A method for determining 6- (phenoxyacetamido) -penicillanic acid, including preparing a solution of an analyzed sample, adding a color reagent, extracting the colored reaction product with chloroform, and measuring the optical density of the extract, which determines the concentration of the analyte in the sample, characterized by that, in order to increase the sensitivity, accuracy and selectivity of the determination, a solution of the sample being analyzed and chloroform is prepared and to the resulting solution is added as a color the reagent is a 0.05% aqueous solution of N, N, N, m-tetramethylthionine chloride at pH 6.5-6.7, and the optical density of the extract is measured at 590 nm.