SU834468A1 - Method of nicotin amide quantitative determination - Google Patents

Description

(54) METHOD FOR QUANTITATIVE DETERMINATION OF NICOTINAMIDL

one

This invention relates to analytical chemistry, in particular to methods for the quantitative determination of nicotinamide.

There is a method for the quantitative determination of nicotinamide by titrating the sample being analyzed, dissolved in acetic acid with an aqueous solution of perchloric acid in the presence of an indicator 13.

The disadvantage of the method is low selectivity of determination.

The closest to the described invention according to the technical essence and the achieved result is a method for quantitatively determining 1 € of icotinamide by treating the sample being analyzed in an alkaline medium with a mixture of hydrocyanic acid solution and chloramine T and then measuring the fluorescence of the solution thus obtained 2.

The disadvantage of this method is low sensitivity (50 µg / ml),

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

This goal is achieved by the fact that in the method of quantitative determination of nicotinamide, the analysis of the sample under analysis in an alkaline medium is carried out with chloralgide) atrm at 99, followed by measuring the fluorescence of the resulting solution.

Upon radiation of the optimal reaction conditions, a linear dependence of the fluorescence intensity on the concentration of the preparation was found, which lies in the range of 0.7-50 μg / ml and is given in Table. one. ,

Table 1

The sensitivity of the reaction described in the invention is 0.7 µg / ml, which makes it possible to determine the preparation of medicinal mixtures.

The determination is carried out on a domestic electronic fluorimeter. Optimal concentrations of the reagents are a 5% caustic soda solution and a 5% solution of chloroalhydrate, 5 ml per treatment of one analyzed sample with a volume of 1 ml. The optimal boiling time of the studied solutions was determined on a boiling water bath. The dependence of the relative fluorescence intensity on the boiling time in a water bath is given in Table. 3. Table Boiling time, min 0,20,5 1 2 3 Relative fluorescence intensity,% 1 7 27 62 60 6

8344684

Continued table. one

PE EF-ZMA with filters FK-1 and Bi - 2.

When studying the optimal conditions of 2Q for conducting a fluorescent reaction to nicotinamide, optimal concentrations of caustic soda and chloral hydrate were found, which are listed in Table. 2

Table2 The processing time of the analyzed sample in a boiling water bath is 0.2–10 min. The optimal values for this interval are 2-10 minutes. In the determination, a boiling time of 5 minutes was used. The definition of nicotinamide in medicinal mixtures does not interfere with cyanocobalamin, thiamine, folic acid, ascorbic acid. Nicotinic acid processed by the method does not give a fluorescence characteristic of nicotinamide. Example 1. Determination of nicotinamide in the injection of 1% solution. 1 ml of a 1% solution from the ampoule is transferred into a 100 ml volumetric flask, made up to the mark with water and stirred. To 1 ml of the resulting solution was added alternately 2 ml of 5%

caustic soda solution and 2 ml of 5% solution of chloral hydrate. The sample to be analyzed is placed in a boiling water bath for 5 minutes. After cooling, the solution is transferred to a cuvette and fluorimetry. The content of nicotinamide is determined by the standard solution, for preparation of which to 1 ml of a standard aqueous solution of nicotinamide containing the preparation

Example 2. Determination of nicotinamide tablets of 0.015 g.

0.1 g (exact weight) of finely divided nicotinamide tablets are placed in a 100 ml flask, made up to the mark with distilled water and stirred. To 1 ml of the resulting solution is poured alternately 2 ml of 5% aqueous solution of sodium hydroxide and 2 ml of 5% aqueous solution of chloral hydrate. The sample is placed in a boiling water bath for 5 min. After cooling, the solution is transferred to a cuvette and fluorimetry. The content of nicotinamide tablets is calculated

0.09619.3

0.096 - 18.6

100 μg / ml alternately pour 2 ml of 5% sodium hydroxide solution and 2 ml of 5% aqueous solution of chloral hydrate. The resulting solution is placed in a boiling water bath for 5 minutes and, after cooling, is fluorimetric simultaneously with the solutions of the test samples.

The results. Fluorimetric determination of nicotinamide in a 1% solution is given in Table. four.

Table4

according to the standard solution, for the preparation of which 2 ml of a 5% aqueous solution of sodium hydroxide and 2 ml of a 5% aqueous solution of chloral hydrate were alternately added to 1 ml of a standard aqueous solution of nicotinamide with a preparation content of 100 µg / ml. The standard sample is placed in a boiling water bath for 5 minutes and, after cooling, the solution is fluorimetry simultaneously with the test samples.

The results of the determination of nicotinamide tablets are presented in Table. five.

Table.5

0,01458

O, 01404 0,0139 Example 3, Determination of nicotinamide in dragees Dekamevit-2, 0.08 g (exact weight) of finely ground dragees is transferred into a 50 ml volumetric flask, dissolved in distilled water and made up to the mark. The resulting pScTBOp is filtered through. paper filter. Alternately, 2 ml of a 5% sodium hydroxide solution and 2 ml of a 5% aqueous solution of chloral hydrate are alternately added to 1 ml of the filtrate. The tube is placed in a boiling water bath, where the sample is located 5 min. After cooling, the solution is transferred to a cuvette and fluoridated simultaneously with the Continued Table. 5 dartny samples. The amount of nicotinamide in the test solution is calculated according to a calibration graph, to build which into a tube, add 1.0; 0.5; About, 25 ml of a standard aqueous solution of nicotinamide with a preparation concentration of 100 µg / ml, add 0.0 / 0.5 and 0.75 ml of distilled water alternately, reagents are poured into each tube as indicated above and fluorimetric simultaneously with the solutions of the studied samples, Data by definition, nicotinamide in dragee Decamevit-2 is presented in Table. b. Table b Example 4. Definition of nicotinamide in Pentonite dragee. 0.075 g (fine weighed) finely ground dragees are transferred into a measuring dish a 50 ml flask, dissolved in distilled water, and brought to the mark with water. To 1 ml of the solution obtained, 2 ml of 5% sodium hydroxide solution and 5% solution of chloral hydrate are added alternately, mixed, mixed, and the sample is mixed with boiling water. uvjnnnyt4 liilschuy banyun5min. After cooling the spread table, the thief is transferred to a cuvette and fluorimetric simultaneously with standard specimens. The amount of nicotinamide in the test solution is calculated according to a calibration graph, for the construction of which standard samples with a nicotinamide content of 5 are prepared; 10 and 20 µg / ml as described above. Data on the definition of nicotinamide in Pentonite dragee are presented in “f. Table 7.

Claims (1)

Claim A method for the quantitative determination of nicotinamide by treating the analyzed sample with a chlorine-containing organic reagent in an alkaline medium followed by measuring the fluorescence of the resulting solution, characterized in that, in order to increase the sensitivity of the determination, chloral hydrate is used as a chlorine-containing organic reagent and 45 treatment is carried out at a temperature of 99-100 ° C.