SU1744603A1 - Method of determination of analgin - Google Patents

Description

The invention relates to pharmaceutical analysis, namely to methods for determining analgin-1-phenyl-2,3-dimethyl-4-methylaminopyrazolone-5-M-methanesulphate sodium, and can be used in pharmaceutical analysis for qualitative and quantitative drug determinations.

Most methods of determining analgin are based on its oxidation with iodine, permanganate, iodate. iodine monochloride, silver nitrate, phosphomolybdic acid, cerium sulfate and DR.

The disadvantages of these methods are their low sensitivity, non-selectivity, low stability of many titrants, insufficient reproducibility of the analysis results.

The known method for the qualitative determination of dipyrone using dye bindones as a reagent.

The disadvantage of this method is the low sensitivity of the reactions.

The closest to the proposed technical essence and the achieved result is the method of quantitative determination of analgin, which means that 2 ml of 0.02 M of freshly prepared sodium 1.2-naphthoquinone-4-sulfanate solution is added to 2 ml of the analyzed solution, heated in boiling water bath for 1 min, cooled, transferred to a 50 ml volumetric flask, made up to the mark and photometric at 495 nm. In parallel, experiments were carried out with a standard solution of dipyrone and a background solution not containing the test substance.

The disadvantages of this method are not sufficiently high sensitivity (lower detection limit of 2.67 µg / ml), a narrow concentration range of analgin obeying the law of light absorption (0.0125-0.0430 g), insufficient selectivity.

 About About 00

The effectiveness of the reaction, idle experience has a significant background (color), which makes it difficult to use this method for the qualitative determination of analgin.

 The purpose of the image: g PMM increase the vitality and selectivity of the analysis.

For this, the analyzed sample is treated in the presence of hydrochloric acid with chloramine, then with phenol and alkali, followed by heating and photometry of the obtained colored solution at 395 nm.

In tab. Figure 1 shows the effect of reagent concentration on optical density (D) of colored solutions.

The sensitivity of the method is 0.2 µg / ml.

Submission to the basic law of light absorption is observed in the range of concentrations of dipyrone 0.5-10.0 µg in 1 ml of the final volume of the reaction mixture.

The method allows serial analyzes.

The method is based on a newly developed color reaction and can be used in factory laboratories, control and analytical laboratories of pharmacy institutions, in biochemical laboratories in the qualitative and quantitative work on the distribution of analgin in the presence of a bromine / barbitzle, barbithy-iatry, butadiene / Ooga, glyukoza-, dibasol, diphenhydramine diprof lllina, codeine to ode u na-phosphate., caffeine, caffeine sodium benzoate and salicylic acid tsatil, metiluratsilz, papaverine gmdrohloride, promedol, theobromine, theophylline, thia- minbro DHS, phenacetin, phenobarbital, aminophylline.

Note: Prepare a solution of a medicine within 10 mg in a 100 ml volumetric flask and make up to the mark with water. 0.5 ml of the solution obtained is taken, 0.25 ml of 0.1 is added and. hydrochloric acid, up to 7 ml of water, 1 ml of a 0.7% solution of chloramine, stirred, 1. ml of a 6% phenol solution was added, stirred, 1 ml of 0.1 N was added. The sodium hydroxide solution is stirred and placed in a boiling water bath for 1-2 minutes. The colored solutions are cooled and the optical density is measured on a spectrophotometer or

photo-light colorimeter, for example FEC-56M (light filter No. 3), relative to distilled water. The content of analgin in the solution is found according to the calibration, raffik or formula

Cx

PxC

DC

st

where Cx is the content of analgin in the analyzed sample, µg;

DX is the optical density of the sample being analyzed,

Set - the content of analgin in a sample of a standard solution, µg;

DCT is the optical density of the standard solution.

The standard solution is prepared by dissolving 10 mg of dipyrone in distilled water in a 100 ml volumetric flask. Certain volumes of the standard solution in the range of 0.05-1.0 mm are transferred to test tubes, and then proceed as described.

In tab. 2 shows the results of the determination of analgin by the proposed method and the statistical processing of the results obtained.

Claims (1)

Claims. . The method of determining analgin, which consists in dissolving the sample in water, reagents are introduced into the solution, to obtain a photometric solution, it is heated in a boiling water bath, cooled and photometrically characterized in that, in order to increase the sensitivity and selectivity of the method, the sample is dissolved in water to a content of 10.0 mcg of analgin per 1 ml of photometric solution; hydrochloric acid, chloramine, phenol and sodium hydroxide are successively introduced to concentrations in 1 ml of photometric solution, respectively, 0.08-0.14 mg, 0.56-0.77 mg, 4.8-10.8 mg, 0.3-1.2 mg, heated in a water bath for 1-2 minutes and then photometrically at a wavelength of 395 nm. Table 1 Note. The indicated quantities of reagents refer to the total final volume of the reaction mixture — 10 ml, which is subjected to photometric measurement. table 2