RU2092815C1 - Method of determining anaphranyle - Google Patents

Abstract

FIELD: analytical methods. SUBSTANCE: sample is preliminarily successively treated by formaldehyde and concentrated sulfuric acid at their ratio 0.5: 2.0, whereupon analysis is performed by measuring relative fluorescence intensity of solution obtained. EFFECT: simplified procedure. 6 tbl

Description

 The invention relates to analytical chemistry, and in particular to methods for the qualitative and quantitative determination of anafranil (clomipramine).

 A known method of spectrophotometric determination of dibenzazepines.

 The disadvantage of this method is the lack of sensitivity, selectivity and duration of the analysis.

 The aim of the invention is to increase the sensitivity, selectivity and simplification of the method.

 The goal is achieved by the described method for determining anafranil (clomipramine), which consists in processing the analyzed sample with formaldehyde and concentrated sulfuric acid, taken in the ratio (0.5: 2.0), which are processed sequentially, and the analysis is carried out by measuring the relative fluorescence intensity of the resulting solution .

Significant differences are:
processing the analyzed sample with formaldehyde and concentrated sulfuric acid in a ratio of 0.5 to 2.0;
processing is carried out sequentially;
the analysis is carried out by measuring the relative fluorescence intensity of the resulting solution.

 When studying the optimal conditions for the course of the fluorescence reaction, it was found that the fluorescence intensity does not change for 24 hours (see Table 1). The dependence of the fluorescence intensity on the ratio of the taken chemical reagents (formaldehyde and concentrated sulfuric acid), see table. 2). The dependence of the fluorescence intensity on the type of solvent used to determine the final effect of this reaction (see table 3), the sequence of adding chemicals: formaldehyde and concentrated sulfuric acid (see table 4) is traced. The definition of anafranil does not interfere with ludiomil, damylene maleate, befol. The selectivity of this reaction in comparison with the prototype (see table. 5), and also presents data to simplify this method and increase the sensitivity in relation to the prototype.

 Example 1. Qualitative determination of anafranil (clomipramine) in substance, dragee, ampouled solutions.

 To 1-2 mg of powder of crushed tablets (tablets) containing the active substance anafranil, 0.5 ml of formaldehyde and 2.0 ml of concentrated sulfuric acid are added. When irradiated with ultraviolet light, green fluorescence is observed. The definition does not interfere: ludiomil, damylene maleate, befol, nialamide, fluoroacisin, cefedrine.

 Example 2. Quantitative determination of anafranil (clomipramine) in tablets (dragees) "Anafranil" (model samples).

 To 0.05 g (the so-called) powder of powdered tablets (dragees) is introduced into a 100 ml volumetric flask, dissolved in 70-80 ml of warm distilled water, shaken for 1-2 minutes. The resulting solution was adjusted to the mark with distilled water, stirred and filtered through a pleated filter. The first 5-10 ml of the filtrate is discarded (solution A).

 To 1 ml of solution A add 0.5 ml of formaldehyde, 2.0 ml of concentrated sulfuric acid and distilled water to 10 ml, mix and fluorimetrate with respect to standard solutions of anafranil. Why add 0.1 to the row of tubes; 0.2; 0.4; 0.6; 0.8; 1.0; 1,2; and 1.6 ml of a standard solution with a drug concentration of 500 μg / ml of 0.5 ml of formaldehyde, 2.0 ml of concentrated sulfuric acid and adjusted with distilled water to 10 ml, respectively, the solutions are mixed and fluorimetric simultaneously with the tested solutions at excitation wavelengths of 365 nm and fluorescence emission of 485 nm.

,
где X содержание анафранила, г;
C средняя масса (драже), г;
P объем (мл), до которого разбавляют навеску;
н исходная навеска, г;
1000000 перевод мкг в г.Calculation of the found amount of anafranil in dragee "Anafranil" in grams is carried out according to the formula:

,
where X is the content of anafranil, g;
C average weight (dragee), g;
P volume (ml) to which the sample is diluted;
n initial sample, g;
1,000,000 mcg transfer to

 The results are presented in table. 6.

было установлено, что получены условия проведения эксперимента, из которых выявлено: оптимальными условиями проведения флуоресцентной реакции являются соотношения формальдегида и концентрированной серной кислоты (0,5 2,0)
Условия проведения эксперимента:
Х1 1,0 0,5 0,5 0,4 0,25 0,1
Х2 2,5 2,2 2,0 2,0 1,90 1,8

, ср. 52,75 73,0 76,75 72,0 69,75 66,5.As a result of the study of the first stage of the fluorescence reaction, it was found that the quadratic term B3 is 0.5; it is impossible to discard it, which indicated a significant surface curvature near the optimum. Another interval was taken in stage II, the regression equation was obtained:
36.56 11.063 X1 9.69X2 2.31 X3
Based on a comparison of the values of the zero level with a coefficient of 36.56

it was found that the experimental conditions were obtained, of which it was revealed: the optimal conditions for the fluorescence reaction are the ratios of formaldehyde and concentrated sulfuric acid (0.5 2.0)
The conditions of the experiment:
X1 1.0 0.5 0.5 0.4 0.25 0.1
X2 2.5 2.2 2.0 2.0 1.90 1.8

, cf. 52.75 73.0 76.75 72.0 69.75 66.5.

Claims (1)

 The method of determining anafranil, characterized in that the analyzed sample is treated sequentially with formaldehyde and concentrated sulfuric acid, taken in a volume ratio of 0.5 to 2.0, followed by measurement of the fluorescence intensity of the resulting solution.

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