SU1330522A1 - Method of determining hexamethylenetetramine - Google Patents

Abstract

The invention relates to analytical chemistry, in particular, the determination of hexamethylene tetramine in a sample treated with a color reagent (CR) in an organic solvent (RR) medium when heated, followed by photometry of the colored solution. Alloxanthine solution in 75-85% dimethylsulfoxyde (DaSO) is used as CR, and 80% DMSO is used as OR, and calcium salt is added to the solution before photometric measurement. The method increases the detection sensitivity to 0.77 µg / ml with a heating time of 3 minutes. 1 dw., 4 tab. S (l

Description

11330522

This invention relates to analytical chemistry, and specifically to methods for determining hexamethylenetetramine.

The aim of the invention is to increase the sensitivity of the determination and reduce the time of the anachasis.

i In the drawing, the representation of the dependence of optical density on the concentration of the solvent used. Yu

5 gd

Example 1. Qualitative definition. division of hexamethylenetetramine. About 0.5-1 mg of substance are dissolved in 1-2 drops of water, 1-1.5 ml of 80% dimethyl sulfoxide solution and 0.5-1 ml of 1% alloxanthine solution are added in 80% - dimethyl sulfoxide solution. The reaction mixture is heated in a boiling water bath for 3 minutes, cooled, and 0.5-1 ml of a 5% calcium chloride solution is added to the reaction product. An orange-yellow stain is formed, with an absorption maximum at 485 nm. Openable minimum 0.77 µg / ml. The obedience to the law of Faith is observed within the limits of concentrations of hexamethylenetetramine 0.6 - 1.2 mg / 100 ml.

Example 2, Quantitative Determination of Hexamethylenetetramine in Substance. The exact weight of the preparation in the range of 0.0144-0.0191 g is dissolved in 5 ml of water in a 100 ml volumetric flask and made up to the mark with 80% dimethyl sulfoxide solution. 1.5 ml is taken from the dilution, 1 ml is added. of a solution of alloxanthin in 80% solution of dimethyl sulfoxide. The reaction is carried out for 3 minutes at the temperature of a boiling water bath. After cooling, add 1 ml of a 5% solution of calcium chloride and a colored solution, transfer to a "25 ml. t to the mark. In parallel, under similar conditions, the experiment was carried out with a standard solution of hexamethylenetetramine (0.0150 g in 100 ml) and a background solution. The optical density of the test and standard solutions was measured using a spectrophotometer in cuvettes with a layer thickness of 1 cm against the background of the control at 485 nm.

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

WITH

D-IOO 25 C, D .P.1,5-G

where D is the optical density of the analyzed solution at

stan485 HMj

D is the optical density of

homemade solution;

C - concentration of standard

spectrophotometric solution (0.0009 g in 100 ml); P is a sample, rj 1 is the layer thickness, see. The results of the quantitative determination of hexamethylenetetramine are given in Table 1.

PRI me R 3. Quantitative determination of hexamethylenetetramine in 40% solution for injection. 1 ml of a 40% solution of hexamethylenetetramine is placed in a flask with a capacity of 100 ml and brought to the mark with water (solution A). 1 ml of solution A is placed in a volumetric flask with a capacity of 25 ml and 80% dimethyl sulfoxide solution brought to the mark (solution B). To 1 ml of solution B, 1 ml of a 1% alloxanthin solution was added and proceeded as in Example 2.

The calculation of the gram content of hexamethylenetetramine in terms of 1 ml of the solution is carried out according to the formula

Р-100-25-25-Со Р-0,5625 D 1-1-1 -ОО-- Б „

The results of the determination are presented in Table 2.

Table 3 presents the results of using various calcium salts.

Table 4 presents the comparative characteristics of the known and proposed methods. I

Thus, the proposed method is more sensitive and faster than the known method, and can be implemented in the practice of the control and analytical laboratories of pharmacy departments and the Quality Control Department of chemical and pharmacological plants.

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Claims (1)

Invention Formula The method of determining hexamethyl n-tetramine by treating the solution of the sample being analyzed with a color reagent in an organic solvent medium e when heated followed by a photometallic agent, a solution is used by alloxanising the resulting colored tin in 75-85% dimethyl sulfoxide, a solution that is different as an organic solvent, and Before photometry of the determination rate and reduction of the analysis time, calcium salt is needed as color. CAC. 485 Ca (NO,) 485 Ca (CHjCOO) j 485 bavl calcium salt. Table D Table 2 9.096.49 1.54 0.77 9.106.49 1.53 0.76 9.09 6.49 1.54 0.77 Alloxanthin + Calcium Chloride Dimethyl sulfoxide Volume and concentration | 1 ml of 1% reagent injected Heating time, min The sensitivity of the reaction, µg / ml 0.77 9Q Editor L.Povkhan Compiled by L.Rusanova Tehred A. Kravchuk. Proofreader L. Beskid Order 3575/45 Circulation 776 Subscription VNIIPI USSR State Committee for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5 . Production and printing company, Uzhgorod, Projecto st., 4 TableA Alloxantrihydrate Dima Tilformamide 2 ml of 10% solution 10-12 1.46 80 90 su.