SU1236354A1 - Method of determining isoniazide and its hydrazones in officinal preparations - Google Patents

Abstract

The invention relates to pharmacy and can be used in the quantitative determination of medicinal substances - isoniazid and its hydrazones (metazid, larusan and ftivazid). The aim of the invention is to increase the sensitivity, selectivity and accuracy of determination. The definition is to dissolve the analyzed sample in an aqueous 2 M potassium hydroxide solution by heating, diluting the solution with distilled water, treating the aliquot portion of the resulting solution sequentially with a 2 M potassium hydroxide solution, 3% sodium nitroprusside solution and repeated 2 M potassium hydroxide solution in the presence of universal buffer solution with a pH of 10, followed by photoelectrocolorimetry the resulting colored solution. 10 tab. (Ls

Description

The invention relates to pharmacy and can be used in the quantitative determination of medicinal substances - isoniazid and its hydrazone (methazide, larusan and phthivazide) in pharmacopoeial preparations in central factory laboratories, in control and analytical laboratories of pharmacies, in biochemical laboratories x clinics and forensic chemical laboratories x.

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

PRI me R -1. Quantitative determination of isoniazid and its hydrazones (metazid, larusan and ftivazid in individual substances.

An exact weight (about 0.1 g) of the substance is placed in a 100 ml conical flask and 10 ml of 2 M potassium hydroxide solution are poured. The reaction mixture is heated to 30-40 ° C and the substance is completely dissolved (in the case of Larusan and Ftivazide). Cool and filter the solution through a glass filter into a volumetric flask with a capacity of 100 ml, and bring the volume of the liquid to the mark with distilled water.

2 ml of the resulting solution was placed in a 50 ml volumetric flask, 1 ml of 2 M potassium hydroxide solution, I ml of 3% sodium nitroprusside solution, I ml of 2 M potassium hydroxide solution and 1 ml of a universal buffer solution with pH 10 were added. A steady orange staining solution was obtained. At this pH, the color of the solution remains stable for a long time. The volume of the liquid is adjusted to the mark with distilled Water. The optical density of the colored solutions was measured on a FEK-M photoelectrocolorimeter with a blue filter (cuvette with a layer thickness of 5.0 mm) at 440 nm. The comparison cuvette is filled with solutions of potassium hydroxide, sodium nitroprusside and a uniform buffer solution with a pH of 10. The resulting solution is light yellow.

The determination of the percentage of substances is carried out using calibration graphs, which were plotted in 50-ml volumetric flasks with concentrations from 5 to 50 µg of substances in the sample.

S

0

five

P m

To 1 ml of each of the obtained alkaline solutions in 50 ml volumetric flasks was added 1 ml of 3% sodium nitroprusside solution, 1 ml of 2 M potassium hydroxide solution and 1 ml of a universal buffer solution with pH 10. A stable orange color is formed. The volumes of the liquid in the flasks were adjusted to the mark with distilled water and the optical density of the resulting colored solutions was measured on FEC-M as described.

The light absorption of the colored solutions of all the studied drugs is subject to the Bouguer-Lambert-Beer law, respectively, within concentrations ranging from 5.0 to 50.0 µg in the sample.

Results for constructing calibration graphs are shown in Table 1.

The content of substances (%) in pharmacopoeial preparations is calculated according to the formulas entered on the basis of processing the calibration graphs constructed using the least squares method:

 R-o. GS 100.50.100 metaeid 0.00211

m

five

rn

m

D-0.038 Ieokiaeida 0,0040

D-0.052

Weighed (µg)

100.50.100 V hinge (µg) 100.50.100

larcsana 0.0028 V-hitch (μg) D-0.040 100.50.100

0

five

Srtiya ida- 0,0038 V.sign (mkg)

In tab. 2 shows the results of the quantitative determination of metazide in individual substances.

The results of the quantitative determination of isoniazid in the individual substance are given in Table. 3

The results of the quantitative determination of larusan in an individual substance are given in Table. four.

The results of quantitative determination of ftivazid in an individual substance are given in Table. five.

PRI mme R 2. Quantitative determination of isoniazid, metazid, larusan and ftivazid tablets containing 0.1-0.2 g of the substance.

The exact weight of the powder obtained by rubbing the tablets of these preparations with a substance content of about 0.1 g for ftivazid and isoniazid, respectively, and about 0.2 g for

312363544

metazid and larusan, respectively. The proposed method is more dissolved in 10 ml of a 2 M solution that is hydrospecific, since it allows potassium peroxide and isoniazid is quantitated and its hydration is determined as in Example 1. In the presence of sugars , glucose and

In tab. 6 shows the results of 5 of the majority of vitamins, quantitative determination of metazide in tablets.

The results of the quantification of isoniazid tablets are given in Table. 7

Claims (1)

Invention Formula The method of determining isoniazid and 10 of its hydrazones in pharmacopoeial preparations by dissolving the analysis and results of a quantitative determined sample, treating the larusan preparation solution in tablets with coarse reagents, followed in Table. 8. photoelectric colorimetration of semi-tabl. 9 shows the results of a co-colored solution, about a quantitative determination of ftivazid, in that with tablets. The goal of sensitivity, selectivity and accuracy of determination. Comparative data of the proposed dissolution is carried out in aqueous 2 M and known methods are given in 20 potassium hydroxide solution with heating. 10. In a diluted solution of the distillation table. 10, it can be seen that the aliquot minimum in the proposed method that is opened by the bath with water and below the part of the solution obtained is 40 times, the limiting dilution below is a successive 2M solution 10 times. The relative error is not 25 potassium hydroxide, a 3% solution exceeds, on average, 1.52%, which is typical of sodium nitroprusside and re-tests its high accuracy, as with a 2 M solution of potassium hydroxide in a known way. universal buffer is 2.51, which is 1.65 times lower. solution with a pH of 10. most vitamins Invention Formula table 2 Table 3 Table A T b J and U a 6 Table 8 13 Relative error,% Ultimate dilution Open minimum mcg Minimum concentrations of substances, possible to determine, µg / ml 1236354 Table 10 U 1.52 2.51 1: 50,000 : 5000 5.0 200.0 5.0 200.0