SU1182351A1 - Method of quantitative determination of metaside and/or larusan - Google Patents

Abstract

METHOD FOR QUANTITATIVE DETERMINATION OF METASID AND / OR LARUSAN by dissolving the analyzed sample, processing with a color reagent followed by photometric measurement of the resulting solution, characterized in that, in order to improve the sensitivity and accuracy of the method, the dissolution is used in an alkali solution, using the color reagent, I use the color reagent to use the reagent in an alkali solution, use the reagent in an alkali solution, use color reagent. A 5% solution of ammonium molybdate in 50% sulfuric acid and treatment with a color reagent is carried out by neutralization obtained to pH 6-7 in the presence of a universal buffer solution.

Description

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ND CO SP

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This invention relates to pharmaceutical analysis and concerns the development of a method for the quantitative determination of medicinal substances derived from isonicotinoyl hydrazones (methazide and larusan) - 1,1-methylene bis- (isonicotinoyl hydrazone and furfurals iseton ison.icotinoiphydrazone).

The aim of the invention is to increase the sensitivity and accuracy of the determination.

The method is carried out as follows.

Example 1. Quantitative determination of metazid and larusan in individual substances.

The exact sample (about 0.1 g) of the plant is placed in a 100 ml conical flask and 10 ml of 2N are poured. hydroxy solution, and potassium. The reaction mixture is heated to a temperature of 30-40 ° C and until the substance is completely dissolved. Cool and filter the solution through a glass filter into a 100 m volumetric flask and bring the volume of the flask to the mark with distilled water. . I

1 ml of the solution obtained is placed in a 50 ml volumetric flask. 2 ml of a 0.5% aqueous solution of ammonium molybdate in 50% sulfuric acid is poured, prepared by dissolving 10 g of ammonium molybdate in -100 ml of concentrated sulfuric acid in a 200 ml measuring flask ml and bringing the volume of the flask to the mark with distressed water.

Then gradually pour 2 n. t acTBOp potassium hydroxide to pH 4-5. 2 ml of universal buffer solution with pH 7 is added and neutralized with 2N. KGSHI hydroxide solution on a universal indicator paper to pH 6-7. An intense blue staining of the solutions is formed, which is stable for a long time at the indicated pH values. The volume of the flask is adjusted to the mark with distilled water. Optical density is measured on a FEK-M photoelectric colorimeter with a red light filter (cuvette with a layer thickness of 5.0 mm) at i 630 nm. The comparison cuvette is filled with an aqueous solution of ammonium molybdate in sulfuric acid, a solution of potassium hydroxide and a universal buffer solution with a pH of 7. The resulting solution is colorless.

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Quantitative determination of substances is carried out using calibration graphs, which are prepared in volumetric flasks with a capacity of 5 to 50 ml of a series of solutions with concentrations of 3-25 µg in the sample for metazide and 20-37.5 µg in the sample for larusan. To the obtained alkaline solutions add 2 ml of 0.5% aqueous

0 solution of ammonium molybdate in 50% sulfuric acid, neutralized with 2N potassium hydroxide solution to pH 4-5, 2 ml of universal buffer solution with pH 7 was added and again neutralized with 2N. solution of potassium hydroxide to pH 6-7 with the formation of intense blue staining of the solutions in flasks, bringing the volumes of flasks to the mark with distilled water, then

0, the optical density of the colored solutions was measured on FEC-M as described by Bbmie.

The light absorption of the colored solutions of metazide and larusan obeys

5 according to the Buger-Lambert-Beer law, respectively, within the concentration limits for metazide, 3.6-25.2 μg in the sample, and for Larusan - 20.2-35.3 μg in the sample. The content of metazide and larusan in

Q percent; in pharmacopoeial preparations calculated according to the formulas entered on the basis of processing the calibration graphs constructed by the method of least squares.

D-0,026 100g50 100

that

AtyaziAo 0.0053 V. hinge / µg

Р-0.06, 100-50 100 ,,

m JSC pij sa and - o, 0033 V. hitch / µg

In tab. Figure 1 shows the results of quantifying metazide in an individual substance.

In tab. 2 shows the results of a quantitative determination of larusan in an individual substance.

Example 2. Quantification of metazid and larusan in

tablets containing 0.5 g of the substance. A precise weight of the powder obtained by grinding the methazide or larusan tablets with a substance content of about 0.1 h is dissolved in 10 kp 2 n. potassium hydroxide solution and quantified as in example 1. 31 in Table. Figure 3 shows the results of quantifying metazid tablets. In tab. 4 shows the results of a quantitative determination of larusan. in pills. The proposed method for the quantitative determination of metazide and larusan in pharmaceutical preparations has a high sensitivity, since the staining reagent has a good coloring effect for the indicated 514. substances, as can be seen from the parameters of the opening minimum, the limiting dilution and the minimum concentrations of substances that can be determined using it. The opening minimum in the proposed method is 25 times lower, the limiting dilution is 50 times lower. The relative error does not exceed on average 1.85%, which characterizes its high accuracy (it is 2.8% in the known method, which is 1.51 times lower). Table 1

Table 3

Table 4

Claims (1)

METHOD OF QUANTITATIVE DETERMINATION OF METAZIDE AND / OR LARUSAN by dissolving the analyzed sample, processing with a color reagent followed by photometric measurement of the resulting solution, characterized in that, in order to * increase the sensitivity and accuracy of the method, the dissolution is carried out in an alkali solution, using 0 as a color reagent , A 5% solution of ammonium molybdate in 50% sulfuric acid and treatment with a color reagent are carried out by neutralizing the resulting solution to pH 6-7 in the presence of a universal buffer 1 .1 182351