SU1051414A1 - Process for determining imizin - Google Patents

Description

cl

"Li

one.

Invention | It relates to analytical chemistry, in particular, to methods for the determination of the drug imimine (1,3-dimethylaminopropylminodibenzyl hydrochloride).

A known method for the determination of imizine, which consists in the treatment of rast ™ of the drug in acetone with mercuric acid acetate, followed by titration with a solution of chloroacid C1

In the process, the sensitivity is low and the selectivity is very low, since almost all aliphatic amines are determined under such conditions.

The closest in technical essence and achieved results is the method of imimine determination by dissolving an anilizable substance in dimethylformamide, treatment with 1,3-indandoin-2-carbolic acid ethyl ester salt with heating in a water bath, followed by photometric measurement of the resulting solution 2.

The disadvantage of this method is its low sensitivity.

The purpose of the invention is to increase the sensitivity of the method.

The goal is achieved by the method of determining imiz®1 by dissolving an analyte in glacial acetic acid, treating a solution of potassium dichromate in glacial acetic acid in the presence of concentrated sulfuric acid, followed by photometry of the solution obtained, using glacial acetic acid as a solvent , a solution of potassium dichromate in glacial acetic acid is used as the xfmic reagent and the treatment is carried out in the presence of concentrated sulfuric acid.

The maximum absorption of the compound obtained by reacting imizine. With potassium dichromate in the presence of sulfuric acid lies in the region of 610 to them.

The optical density of the resulting solution does not change for 2 hours.

Example 1. Qualitative determination of imizine.

Grains of finely divided tablets or imizine powder are added to 1 ml of ice; acetic acid, shaken, then 1 ml of 0.0005 M solution of potassium dichromate in glacial acetic acid is added to the resulting solution, 0, 5 ml of concentrated sulfuric acid, resulting in an intense blue color, indicating the presence of imizine in the sample under investigation.

Example 2. Quantitative determination of imizina.

0.01 g (exact weight) of imizine powder is transferred to a 100 ml volumetric flask, 80-90 ml of glacial acetic acid is added, shaken for 10 minutes. The volume of glacial acetic acid solution is added to the mark and thoroughly mixed.

To 1 ml of the test substance solution was added 1 ml of 0.0005 M solution of potassium dichromate in glacial acetic acid and 0.5 ml of concentrated sulfuric acid - an intense blue color appeared. 2.5 ml of glacial acetic acid is added to the resulting solution, and the optical density of the resulting solution is measured at a wavelength of emitted light of 610 with it (spectrophotometric determination) or light filter No. 7 (photocolorimetric determination).

The calculation of the percentage of imizine is carried out according to the formula

ol D 5100

% g.

: 1cm

re

where O is the optical density at No. 7 light filter or wavelength;

D 610 nm;

 - layer thickness, cm;

p is the sample of the drug, g;

nineteen

Е ° - specific indicator of absorbed 1 cmV

experimentally established.

In this reaction, the photocalorimetric determination (light filter No. 7) is 530, 356; spectrophotometric determination - (L 610 nm) 621.57. The results of the determination of imizine in powder are given in Table. 1 and 2.

Example 3: Quantitative determination of imizine in tablets of 0.025 g.

About 1 g (fine weighed) of finely divided tablets was transferred into a 100 ml volumetric flask, 8090 ml of glacial, acetic acid were added, and 3-1051 chives were added for 10 minutes. Bring volume of glacial acetic acid to the mark. The solution is filtered through a folded filter into a clean, dry flask. To 1 ml of the solution obtained is added 1 ml of a 0.0005 M solution of potassium dichromate in glacial acetic acid and 0.5 ml of concentrated sulfuric acid — a deep blue color appears. Add 2.5 ml of 10 g of glacial acetic acid, mix thoroughly, and measure the density of the resulting solution using a tf 7 light filter at a photocalorimetric determination or at a wavelength of 15,610 with it (spectrophotometric determination). The amount of imizine in the tablets is calculated according to the formula YOG - (see where XD is the amount of imizine in the tablets, g; -optical density of the solution at a f 7 light filter (photocolorimetric P). Table II imiz dialing, absorption 4 definition) or at a wavelength of 610 nm (spectrophotometric determination); P is the average weight of the tablet, g; P is the weight of crushed tablets, g; 2 is the thickness of the solution layer, see t. —the specific indicator of supercuminal absorption, equal to 530, 356 in this reaction (photocolorimetric definition; with a light filter No. 7 - 621, 57 spectrophotometric definition, wavelength of 610 nm.) The results of imizin determination of 0.025 g in the flow paths are given in V. 3 and t. The proposed method of determining AI compared to the prototype does not increase the sensitivity both by 30 times, as can be seen from the ratio of specific indicators of light deflection 621, 57 19; 80 S1051 41 Results of the determination of imizine in powder. Definition) 6 Table 1 (spectrophotometric

Results of determination

Found%

Hitch, g

98.82

102 06

98.75

98.72

100.21

99.15

99.7

101.01

The results of the determination of imizina in tablets of 0.025 g (photo calorimetric determination)

Metrological characteristics

X 99.8Gl 1.22

Е +1,02

a 99.81 ± 1, 02

Table 3 Table 2 imizine powder (photo calorimetric determination).

7 lOSI + U8

Results of imiein determination in tablets of 0.025 g (spectrophotometric determination) Definition Found, g Found, g 10.02 Y89 20, 30, 0.02508 50, 6.0,

Table Metrological characteristics X 0,02480. b .0003371. E +0,0003876 3 0.02 48010,0003876

Claims (1)

METHOD FOR DETERMINING IMIZINE by dissolving the analyte in an organic solvent, treating with a chemical reagent, and then photometrizing the resulting solution, which consists in the fact that, in order to increase the sensitivity of the method, glacial acetic acid is used as a solvent, and a solution is used as a chemical reagent potassium dichromate in glacial acetic acid and the treatment is carried out in the presence of concentrated sulfuric acid. > 10500