SU826218A1 - Method of quantitative determining of 1,2-dimethyl-3-carboethoxy-5-oxyindole - Google Patents

Description

one

This invention relates to analytical chemistry, namely, to methods for the quantitative determination of dimecarbine (1,2-dimethyl-3-carboethoxy-5-hydroxyindole).

A known method for the quantitative determination of dimecarbine by spectrophotometry of the sample being analyzed at a wavelength of 290 km 1.

The disadvantages of the method are low sensitivity — we determine, a concentration of 1.8 mg / ml and poor selectivity — diazolin and indopan interfere with the determination.

The closest to the present invention is a method for the quantitative determination of dimecarbine, which consists in the sequential processing of the analyzed sample with silicic molybdenum ACID. THAT and ammonia in the medium of methyl alcohol, followed by spectrophotometric analysis of the obtained colored solution 2.

The disadvantages of the method are low sensitivity - a detectable concentration of 2 µg / ml and poor selectivity, since many indole derivatives interact with the indicated ones. KXU reagents.

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

This goal is achieved by the method of quantitative determination of dimecarbine, which consists in sequential processing of the analyzed sample with a solution of hydrogen peroxide and a solution of formaldehyde in an alcohol medium at a temperature of 99-100 ° C, followed by measuring the fluorescence of the solution obtained.

An example. Determination of dimecarbine in tablets of 0.02 g.

A fine sample (0.1 g) of finely divided tablets is transferred into a 100 ml volumetric flask, 6070 ml of ethyl alcohol is added and boiled in a water bath for 10 minutes, then the solution is cooled to room temperature and the alcohol is added to the mark

To 1 ml of this solution was added 2 ml of a 5% hydrogen peroxide solution, 7 ml of a 20% formaldehyde solution, heated for 25 minutes in a boiling bath, cooled, and the fluorescence intensity of the resulting solutions was measured compared to a standard solution containing 10 µg / mp, for which to 1 MP solution containing 100 µg of dimecarbon, 2 MP of 5% i solution of hydrogen peroxide, 7 ml of 20% formaldehyde solution are added, heated in a boiling bath at -999 ° C 25 min, cooled and fluorimetric. simultaneously with prototypes V

Dependence of fluorescence intensity; Table 2 shows the concentration of formaldehyde, hydrogen peroxide and the time of heating in a boiling water bath (dimecarbine) (10 µg / ml). 3, 4 and 5.J

Claims (2)

- Table 3 between the intensity of fluorescence and the concentration of dimecarbine from 0.1 to 30 µg / ml. I The sensitivity of the known cnoco ba is 2 µg / ml, preliminary 0, 1 µg / ml. The fluorescence spectrum of the solution obtained in this case lies in the region from 420 to 530 nm, with a maximum of 470 nm, and the excitation spectrum from 320 to 440 nm, with a maximum of 412 nm. The use of the present invention allows, without separation of the accompanying ingredients, to carry out the determination of dimecarbin in medicinal preparations,. The invention of the method of quantitative determination of 1,2-Dimethyl-3-carboethoxy-5-oxylindone by sequential processing of the analyzed sample with chemical reagents in an alcohol medium, characterized in that, to increase the sensitivity and efficiency of the determination, peroxide solution is used as chemical reagents. hydrogen and formaldehyde solution, processed at 99-100 ° C, and the fluorescence of the solution obtained during processing is measured. Sources of information taken into account in the examination 1. T. Archipova, Yu., Belikov VG and Verechik, E.N., Spectrophotometric analysis of diazolin, dimecarbine, -indopan and adip ;: Nata serotonin. Pharmacy, 1977, 26 6, p. 64-66. 2. Rogovsky D.Yu., Kramarenko V.P. and .Gzhegotsky P.M. K1ln1snogo znachchennn dimekarb1n in drug 1 tablets. -Pharmaceutical Journal, 1977, No. 3, p. 48-51 (prototype).