SU759923A1 - Method of quantitative determining of hexamethylenetetramine - Google Patents

Description

The invention relates to the field of analytical chemistry, and in particular to methods for the quantitative determination of hexamethylenetetramine. /

There is a method of quantitative determination of hexamethylenetetramine by measuring the IR spectra of the analyzed solutions [1].

The disadvantage of this method is the low detection sensitivity.

Closest to the described technical essence and the achieved result, the method of quantitative determination of hexamet-, lentetramin in substance tablets and solution for injection, which consists in processing the analyzed sample 0.1 n. sulfuric acid solution at boiling, the excess of which is then titrated with 0.1 and. sodium hydroxide solution in the presence of methyl ¹ red indicator (21.

The disadvantage of this method is a low _ sensitivity, in particular, when analyzing hexamethylenetetramine in the substance and tablets, we used 0.12 g or 5 ml of the sample in the study of the solution for injection. Kie2 way

(lotus-based titration in this case is very cumbersome.

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

This goal is achieved by the described method of quantitative determination of hexa methylenetetramine, which consists in processing the analyzed sample in dimethylformamide medium with a solution of alloxanterhydrate in dimethylformamide when heated in a boiling water bath followed by spectrophotometry of the colored solution obtained.

A distinctive feature of the method is the use of alloxantryhydrate as a chemical reagent, processing in the presence of dimethylformamide, spectrometry measurement of the obtained colored solution.

Example 1. Quantitative determination of hexamethylenetetramine in substance and tablets. The exact weight in the range from 0.0090 to 0.0200 g of the preparation or carefully crushed tablet mass is dissolved in 20-30 ml of dimethylformamide with agitation. The solution is quantitatively transferred to a 50 mL volumetric flask.

759923 4

6 - layer thickness, cm;

P — weight, g; average tablet weight 0.5 g

PRI mme R 2. Quantitative determination of hexamethylenetetramine in 40% solution for injection.

and mark up with dimethylformamide. Take 2 ml of dilution, the solution is placed in a test tube, add 2 ml of 10% alloxantrihydrate solution. The mixture is heated in a boiling water bath for 10-12 minutes. In parallel, conduct a control experiment. Then the liquid is cooled and transferred quantitatively into a 25 ml volumetric flask, made up with dimethylformamide to the mark. The colored solution is spectrophotometrized at A 532 nm using

'quartz, cuvettes with a layer thickness of 1 cm.

Calculation 'percentage of hexamethylenetetramine in substance or gram tablets using the formula: _{a, c,}

E “’ pD1

ten

15

0.1 ml of a solution of hexamethylenetetramine is placed in a volumetric flask of 100 ml and dimethylformamide is adjusted to the mark. 1.5 ml are taken from the dilution, the solution is placed in a test tube, 0.5 ml of dimethylformamide is added,

2 ml of 10% alloxantrihydrate solution and then the experiment is carried out as in example 1.

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

4a *

where ϋ .1¾ „

4 cm

optical density at A

Max

C = 532 nm; specific absorption rate of 320 at Adlskg 532 nm;

20

3-100-25

e1 ⁷ ° -O, 1-1.5-1ОО6

The results of the determination are shown in table 1.

• ·. · ..-. V. ·. . ... - - · - - · - · ·. ···. ·>. . 7 ^{T 3} blitz 1 . A drug Hitch, g Optical density, ϋ Found% .λ './' -ϊ / - u. ·). . -,. · '. · ✓ ^; -Λ; /. . '. Solution '0.0087' · 0.450 ^; 101.01 for injection '0,0124 0.640 100.80 -L ·: / "L ----- 0,0150 0.770 100.25 λ. ··, - · Ζ ..... 0,0174 ' 0.880 98.77 ·. · '. . -. '.GL · .... '0,0194 0.980 98.65 ... '. 0.0200 1,030 100.58 . <..... . .:. -.

and the present methods are given in table. 2 and 3. '

Thus, the proposed method for the quantitative determination of hexamethylenetetramine in a substance, tablets, injection solution is more sensitive, 6 times in the analysis of the substance and tablets, 50 times in the analysis of the solution for injection. The method is simple to perform and can be used in 50 control-analytical laboratories of chemical-pharmaceutical factories and pharmacy departments

The described method is more sensitive ..

According to the proposed method, weights are used in the range of 0.0090–0.0200 g or 0.1 ml of the solution, while in the known 0.12 g or 5 ml of the solution. In addition, the method for determining hexamethylenetetramine differs favorably from the known technique of execution, namely its simplicity.

Comparative data of the quantitative determination of hexamethylenetetramine in substance, tablets, injection solution by known

45

A drug Known method Hitch, g Found% Heating time, min ’. 0.1200 99.12 10

Pills

0.1200

98.83

ten

759923

6

Continued table. 2

A drug

-—- g · ...... "Τ '

Known method

Hitch, g Found% Heating time min 0.1200 99.42 ten 0.1200 99.42 ten 0.1200 99.67 ten 0.1200 99.01 . ten 0,0150 99.60 ten 0,0150 98.95 ten 0,0150 100.25 ten 0,0150 100.77 Yu 0,0150 100.54 ίο 0,0150 98.69 ten 0,0150 100.25 ten 0,0150 100.64 ten 0,0150 101.29 ten 0,0150 100.25 Yu 0,0150 101.55 ten

. (Table 3

A drug Hitch, g Found, g Heating time, min BUT 2. · - ·· - uh four Pills 0.1200 0.4885 ten 0.1200 0.4964 ten ! 0.1200 0.4950 ten 0.1200 0.4896 ten 0.1200 0.4958 ten 0.1200 0.4958 ten

> uh! I5 £ nd «& $ Le24 'K5'

759923

eight

Continued table. 3

...... ι. *

^ F ^^ -? 1 = -y ·. -'- ;: ·

four 2 ' '3 - four "* , · .-., .. ·. -. -.7 /. ί ./Λ,"·· -7- '. · ' . "··, · · 7 ’G-’ ·· ........ - ' -  ** - · ή ' 0,0180 0.4936 ten 7 '. -77-7 ...; - ' _: . .- / - 7 • 7-7 - ·. ’ 0,0180 0.4909 ten . . ·. V .. 0,0180 0.5067 ten ο, ό? 8ο ~ 0.5126 7 ' ten 0,0186 ⁷ 0.5023 ten • 0.0180 0.5067 ten 0,0180 0.5067 ..... ten ο, οίδό ’ 0.5126 ten · Λ ^; '· 2 "-G ο; οΐ8ο 0.5126 ten ·. . - l 1.- '4 · -. 4 ·· -> - - • .-.. · ··· 00180 0.5064 ten 0,0180 ’- 0.5191 ten

Direct analysis (chemical and pharmaceutical) 'Hexamethylenetetramine in substance, tablets, injection day solution.

The results of quantitative determination of hexa, methylenetetramine at λ = 532 nm.

Claims (1)

Claim A method of quantitative determination of "hexamethylenetetramine by treating the sample analyzed ⁴⁵ Rui chemical at boiling from l and h and w u s by the fact that, 'with increasing tsytgo chuvstvYtoynosty definitions 40 Alloxantrihydrate is used as a chemical reagent and the treatment is carried out in dimethylformamide, followed by spectrophotometry of the solution obtained. ~