SU1617333A1 - Method of determining derivatives of amide sulphanilic acid - Google Patents

Abstract

The invention relates to analytical chemistry, in particular the determination of sulfanilic acid amide derivatives, which can be used in their manufacture. The goal is to increase the sensitivity of the analysis. The latter is treated with a sample dissolved in HCL-acid with a solution of potassium chlorate, followed by extraction of the obtained product, treatment with sodium reagent N, N-diethyldithiocarbaminate in acetone and photometric measurement of the colored solution. In this case, the sensitivity of the analysis is increased by a factor of 20 while the amount of the substance analyzed is reduced by a factor of 6. 4 tab.

Description

The invention relates to analytical chemistry, in particular to the analysis of sulfanilic acid amide derivatives, and can be used in factory control and analytical laboratories, central factory laboratories of chemical enterprises.

The method is a mass one.

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

Example 1. Definition 2 - ((1-aminobenzene-sulfamido) -thiazole (norsulfazole)

1. Qualitative definition.

About 2 mg of 2- (p-aminobenzenesulfamide) -thiazole is dissolved in 5 ml of 10% hydrochloric acid solution, 1 ml of a saturated solution of potassium chlorate is added and the reaction mixture is heated in a water bath at 100 ° C for 10 -15 minutes. The resulting product is extracted with 2 ml of chloroform. The chloroform extract is separated, and after the color disappears, 3 ml of acetone and 2 ml of a 0.1% solution of sodium M, N-sodium diethyldithiocarbaminate in acetone are added. Appears yellow orange.

2. Quantitative determination.

Build a calibration graph.

0.5 tubes are added to five tubes; , 0; 2.0; 3.0; 4.0 ml of a standard (0.02%) solution of 2- (l-aminobenzenesulfamido) -thiazole in a 10% solution of hydrochloric acid, respectively 4.5; 4.0; 3.0; 2.0; 1.0 ml of 10% hydrochloric acid solution and 1 ml of saturated solution of potassium chlorate. The solution tubes are heated in a water bath at 100 ° C for 15 minutes, cooled, 5 ml of chloroform are added to each solution, and the reaction product is extracted. The chloroform extracts are separated, transferred to evaporating dishes, and after the yellow color disappears, the chloroform extracts are filtered through a filter paper into 25 ml volumetric flasks. The residues of chloroform extracts in each bag are washed with 2.5 ml portions of chloroform and the washings are filtered in the same volumetric flasks. To content of measure05

oo oo with

10 ml of acetone, 2 ml of 0.1% acetone solution N, N-diethyldithiocarbaminate sodium are added to each flask and the total volume is made up to the mark with acetone. The optical density of the resulting colored solutions was measured on a KFK-2 test tube at a No. 4 light filter (440 nm wavelength) in cuvettes with a 50 mm working layer thickness against the background of the solution obtained in the control experiment. Based on the measurement results, a calibration graph is constructed. Absorption of diluted solutions complies with the Bouguer-Lambert-Beer law in the concentration range of 4-32 µg / ml. The least squares method calculates the equation of the calibration graph, which in this case has the form, 02161 C + 0.02802, where D is the optical density; С - concentration of the solution in solution, µg / ml.

Quantitative determination method. About 0.05 g (precise weight) of 2- (p-aminobenzenesulfamido) -thiazole is dissolved in a 10% solution of hydrochloric acid in a 50 ml volumetric flask (solution A). 10 ml of solution A are placed in a 50 ml measuring flask and the total volume of the solution is made up to the mark with hydrochloric acid solution (solution B). 2 ml of solution B are introduced into a test tube, 3 ml of hydrochloric acid solution (10%) is added, 1 ml of a saturated solution of potassium chlorate and further operations are carried out according to the scheme described for the construction of a calibration graph. The determination of the quantitative content of 2- (p-aminobenzenesulfamido) -thiazole is carried out according to the equation of the calibration graph and recalculated to the sample. The results of the determination and metrological characteristics are presented in Table. . The sensitivity of the reaction is 2.5 µg / ml.

Example 2. Determination of 2- (p-aminobenzenesulfamido) -4,6-dimethylpyrimidine (sulfadimezine). 1. Qualitative definition. About 2 mg of 2- (p-aminobenzenesulfamido) -4 6-dimethylpyrimidine is dissolved in 5 ml of 10% hydrochloric acid solution, 1 ml of a saturated solution of potassium chlorate is added and the reaction mixture is heated in a water bath at 100 ° C for 10 -15 minutes. The resulting product is extracted with 2 ml of chloroform. The chloroform extract is separated and after the disappearance of its color, 3 ml of acetone and 2 ml of a 01% solution of M, S-diethyldithiocarbamine sodium inate in acetone are added. Appears yellow orange.

2. Quantitative determination. Build a calibration graph. 0.5 tubes are added to five tubes; 1.0; 2.0; 3.0; 4.0 ml of a standard (0.02%) solution of 2- (p-aminobenzenesulfamido) -4,6-dimethylpyrimidine in a 10% solution of hydrochloric acid, respectively 4.5; 4.0; 3.0; 2.0; 1.0 ml of 10% hydrochloric acid solution and 1 ml of saturated solution of potassium chlorate. The tubes with solutions are heated in a water bath at 100 ° C for 15 minutes, cooled, 5 ml of chloroform are added to each solution and the reaction product is extracted. The chloroform extracts are separated, transferred to evaporating dishes, and after the yellow color disappears, the chloroform extracts are filtered through a filter paper into 25 ml volumetric flasks. The residues of chloroform extracts in each lump are washed with 2.5 ml portions of chloroform, and 5 filter washes are washed into the same volumetric flasks. 10 ml of acetone, 2 ml of a 0.1% acetone solution of N, N-sodium diethyldithiocarbaminate are added to the contents of the volumetric flasks and the total volume is made up to the mark with acetone. The optical density of the resulting colored solutions was measured on a KFK-2 instrument using a No. 4 light filter (440 nm wavelength) in cuvettes with a working layer thickness of 50 mm against the background of the solution obtained in the control experiment. According to the results, 25 scientific research institutes construct a calibration graph. The light absorption of the colored solutions follows the Bouguer-Lambert-Beer law in the concentration range of 4-32 µg / ml. The method of least squares calculates the equation of the calibration graph, which in this case has the form, 01810-C + 0.0341. where D is optical density; C is the concentration of the colored solution, µg / ml.

Quantitative determination method. About 0.05 g (precise weight) of 2- (p-aminobenzenesulfamido) -4,6-dimethyl pyrimidine 35 is dissolved in a 10% solution of hydrochloric acid in a 50 ml volumetric flask (solution A). 10 ml of solution A are placed in a measuring flask with a capacity of 50 ml and the total volume of the solution is brought to the mark with a 10% hydrochloric acid solution (solution B). 2 ml of solution B are added to the tube, 3 ml of hydrochloric acid solution (10/0) are added, 1 ml of a saturated solution of potassium chlorate is added, and further operations are carried out according to the scheme 45 described for the construction of a calibration graph. The determination of the quantitative content of 2- (p-aminobenzenesulfamido) -4,6-dimethylpyrimidine is carried out according to the equation of the calibration graph and recalculated for the weight. The results of the determination and the metrological characteristics are presented in Table. 2. Sensitivity of the reaction 2.5 μg / ml, Example 3. Determination of p-aminobenzene - sulfamide (streptocide), i. Qualitative definition. About 2 mg of p-aminobenzenesulfamide is dissolved in 5 ml of 10% hydrochloric acid solution, 1 ml of a saturated solution of potassium chlorate is added and heated on a water bath at 100 ° C for 10-15 minutes. The resulting product is extracted with 2 ml of chloroform. The chloroform extract is separated and after the disappearance of its color, 3 ml of acetone and 2 ml of a 0.1 / solution solution of Na, N-sodium diethyl dithiocarbamine sodium in acetone are added. Appears yellow orange.

2. Quantify the Oldelekie. Build a calibration graph. 0.5 tubes are added to six tubes; 1.0; 1.5; 2.0; 2.5; 3.0 ml of a standard (0.02%) solution of p-aminobenzenesulfamide in a 10% solution of hydrochloric acid, respectively 4.5; 4.0; 3.5; 3.0; 2.5; 2.3 ml of 10% hydrochloric acid solution and 1 ml of saturated potassium chlorate solution. The tubes with solutions are heated in a water bath for 15, cooled, and to each solution, 5 ml of chloroform are extracted into the solution and the reaction product is extracted. The chloroform extracts are separated, transferred to evaporating dishes, and after the yellow color disappears, the chloroform extracts are filtered through a filter paper into 25 ml volumetric flasks. The residual chloroform extracts in each dish are washed with 2.5 ml portions of chloroform and the washings are filtered in the same volumetric flasks. To the contents of the volumetric flasks, add 0 ml of acetone, 2 ml of a 0.1% acetone solution of N N diethyl sodium thiocarbaminate, and add the total volume to the mark with acetone. The optical density of the resulting colored solutions was measured on a KFK-2 instrument with a No. 4 light filter (440 nm wavelength) in cuvettes with a working layer thickness of 50 mm against the background of the solution obtained in the control experiment. Based on the measurement results, a calibration graph is constructed. The absorption of the colored solutions is in accordance with the Bouguer-Lambert-Behr law in the concentration range of 4-20 µg / ml. The method of least squares calculates the equation of the calibration graph

fika, which / e in this case, has the form, 03360. C + 0.0157, where 6 is optical density; C is the concentration of the colored solution, µg / ml.

Quantitative determination methodology. About 0.05 g (exact weight) of the l-a mineral-benzoyl sulfamide is dissolved in a 0% solution of hydrochloric acid in measure-: (50 ml flask with a capacity of 50 ml (solution p A). 10 ml of solution A A flask with a capacity of 50 ml was adjusted to bring the total volume of the solution to the mark with a 10% hydrochloric acid solution (solution B). .5 ml of solution B was transferred into a test tube, 3 ml of 10% hydrochloric acid-15 solution was added. ml of saturated potassium chlorate solution and further operations are carried out according to the scheme described for the construction of the calibration graph. division quantitative content of n-aminobenzol- sulfamkda carried out according to equation 50 rovochnogo calibrated and converted to graphics weighed. Results and determining metrological h..rakteristiki presented in Talbov. 3. The sensitivity of the reaction of 1.5 g / ml.

The proposed method, compared to the known 25, increases the detection rate by a factor of 20, and reduces the consumption of the analyte by 6 times.

Comparative characteristics of the proposed and known methods are given in table. i. 0

Claims (1)

Invention Formula A method for determining sulfanilic acid amide derivatives by dissolving an analyzed sample in hydrochloric acid, treatment with potassium chlorate solution with heating, extracting the resulting product, processing it with a photo reagent, and photometry the colored solution, in order to increase the sensitivity of the method as the color reagent uses a solution of M, S-sodium diethyldithiocarbaminate in acetone. 0 Table 1 Results 2- (p-aminobexzolsulfamido) -thiazole The results of quantitative determination of 2- (p-aminobenzenesulfamido) -A, 6-dimethylpyrimidine Found Metrology 1characteristics g J% 0.0485093.99X 98 71 0.05281101.08 b 2.96 0.0502297.71b, - - U21 0.05022100, 3, O 0.04936101.78A 3 14 0.0498897.04 a 8 ,, And Table3 Results of quantitative determination of p-aminobenzenesulfamide NavdoMetrological Characteristics I g I% 0.0445693.51X 98.58 0.0445693.61b 3.98 0.05138102,556 62 0.04952101 ,, 0.0507699 .. d 0.04704100.72. a 98.58-4.24 Table 4 Comparative characteristics of the proposed and known methods -.--. .iТ pg, oppo - e 3.0 10 - 5.0 1 o l- 1, e lu z, 3-iu alyve-Q 30 u, uj Table 2