SU1719972A1 - Method of quantitative determination of furadonin - Google Patents

Abstract

The invention relates to analytical chemistry, in particular the determination of furadonin in its dosage forms or in pure form. The purpose of the invention is to improve the accuracy and sensitivity of the analysis. To do this, the sample is treated first with pyrogallol A, then with concentrated sulfuric acid, followed by photometry of the resulting solution. In this case, the analysis error is reduced from + 2.2 to ± 2.9. 10 tab.

Description

This invention relates to analytical chemistry and can be used to quantify furadonin, both in pure form and in dosage forms.

A known method for the quantitative determination of drugs based on 5-nitrofuran derivatives. by processing the sample of the analyte with alkali, followed by photometric measurement of the resulting solution.

However, this method is characterized by a low stability of the colored product (4 minutes) and the associated difficulty in obtaining reproducible results.

. The closest to the proposed one is the method in which the goal is achieved by treating the sample being analyzed with a 50% solution of sulfuric acid: Optical density

the colored product is measured at b. 227 nm.

However, when analyzing furadonin by this method, in a pure form and in dosage forms, a high consumption of reagent, low accuracy and sensitivity of detection were revealed.

The purpose of the invention is to improve the accuracy and sensitivity of the determination of furadonin in pure form and in dosage forms.

The goal is achieved by the fact that a sample containing furadonin is treated with a chemical reagent, followed by photometry of the resulting colored solution. A 0.2% aqueous solution of pyrogallol A is used as a chemical reagent, and the treatment is carried out in a sulfuric acid medium. A blank solution is used as a comparison solution.

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the solution of the proposed reagent - the thief by adding conglomerate.

optimal definitions of specific specific and light absorbing

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The chemistry of the quantitative furadonin assay is presumably based on the formation of the dye Stenhaus. In the medium of 50% sulfuric acid, the furandonin furanonine ring opens and the resulting product condenses with pyrogallol A to form a colored solution.

In tab. Figure 7 shows the conditions for the quantitative determination of furadonin with phenol derivatives, the use of which provides for the conversion of furadonin into a colored compound, the corresponding values of the molar and specific absorption coefficients. For furadonin, the optimal phenol is ow - A.

pyrogallol is

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Quantitative photometric determination of furadonin.

Build a calibration graph.

About 0.01 g of the Sludge suspension of furadonin powder is quantitatively transferred into a 100 ml volumetric flask, about 80 ml of distilled water is added and heated in a boiling water bath until completely dissolved.

After cooling, the volume of the resulting 4 solution is brought to the mark with distilled water and stirred. Solution A is prepared, in 1 ml of which 100 µg of furadonin is contained.

20 ml of the obtained solution A is transferred to a 100 ml volumetric flask and the volume of the solution is made up to the mark with distilled water. Solution B is obtained, in 1 ml of which 20 µg of furadonin is contained.

Starting from a standard solution B, a series of solutions with a content of the test substance from 10 is prepared.

up to 40 mcg. For this, 25.0 ml volumetric flasks are placed respectively. 0.5; 1, OJ 1.25; 1t5 and .2.0 ml of standard solution B and a volume of distilled water missing up to 5.0 ml. TO

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solutions in flasks were added with 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol A and 12.0 ml each with concentrated sulfuric acid. The volume of the solutions in flasks was made up to the mark with distilled water and mixed thoroughly. After cooling, the volume of the solutions in flasks is again brought to the mark with water and stirred. The optical density of the obtained colored solutions was measured using a KFK-2 photoelectric colorimeter with a 440 + 10 nm light filter in a cell with a working layer thickness of 50.0 mm.

A cooled mixture consisting of 11.0 ml of water, 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol A and 12.0 ml of concentrated sulfuric acid is used as a comparison solution.

In tab. Figure 2 shows the dependence of the optical density of the product of the interaction of furadonin with pyrogallol A on the amount of furadonin taken per reaction.

The calculation of the calibration graph equation for photoelectrocolorimetric determination of furadonin is as follows:

 - 125x2A09 5x3625 - (725) ™

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 0,0169J

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 3625x2209 - 60.7x | 25

 - (125) 2 -0.0045.

From the data table. 2 it follows that the absorption of colored furadonin solutions follows the Bouguer-Lambert-Beer law at concentrations of 10.0 - 40.0 µg furadonin in 25 ml of the final photometric solution. These dependences of the light absorption of the colored solutions of furadonin, taken to the performance of the reaction, were used to calculate the parameters of the direct equation corresponding to the rectilinear section of the calibration graph having a general view

D CC - B,

where D is optical density;

K - coefficient of proportionality, equal to the tangent of the angle of inclination of the calibration graph to the abscissa axis;

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X is the content of the analyte in the analyzed sample µg

about

B is a constant indicating where in the chart the axis of ordinates crosses.

Taking into account the calculated parameters K and B, the equation of the straight line corresponding to the rectilinear portion of the calibration graph for the photoelectric polarization determination of furadonin has the following form:

D - 0.0169 X - 0.0045.

Photoelectrocolorimetric determination of furadonin in powders.

In a volumetric flask of 25.0 ml is placed 2.0 ml of an aqueous solution of furadonin (10.0 μg in 1 ml) and 3.0 ml of distilled water. To the resulting solution was added 4.0 ml of 0.2% freshly prepared aqueous solution of pyrogallol A and 12.0 ml of concentrated sulfuric acid, the volume of the solution in the flask was made up to the mark with water, cooled. After cooling, the volume of the solution in the flask is made up to the mark with water and again mixed.

The optical density of the obtained colored solution was measured using a KFK-2 photoelectrocolorimeter at a light filter of 1,440 ° C nm in a cuvette with a working layer thickness of 50.0 mm. A cooled mixture consisting of 11.0 ml of distilled water, 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol A and 12.0 ml of concentrated sulfuric acid is used as a comparison solution.

The calculation of the drug content in the samples is calculated according to a pre-built calibration graph or by the direct equation corresponding to the straight line section of the calibration graph.

In tab. Figure 3 shows the results of the quantitative determination of furadonin in powders by the photoelectric colorimetric method.

The data given in table. 3 indicate that using this method it is possible to determine the furadonin content in powders with a relative error A i 1.6%.

Photoelectrocolorimetric determination of furadonin tablets of 0.05 and 0.1 g.

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A precise weight of powdered furedonin tablets was quantitatively transferred to a 250.0 ml volumetric flask, 200 ml of distilled water was added, and the contents of the flask were heated in a boiling water bath until complete dissolution. After cooling, the volume of the solution in the flask is brought to the mark with water and mixed thoroughly. The required volume of the sample obtained by dissolving the weighed tablets of furadonin, 0.1 or 0.05 g each, is placed in a 25.0 ml volumetric flask, up to 5.0 ml of distilled water, 4.0 ml of 0.2% strength are added. a freshly prepared aqueous solution of pyrogallol A and 12.0 ml of concentrated sulfuric acid is stirred and the mixture is made up to the mark with water. After cooling, the mixture is again brought to the mark with water and stirred.

The optical density of the obtained colored solution was measured using a KFK-2 photocolorimeter with an Aesf 440 ± 10 nm light filter in a cell with a working layer thickness of 50.0 mm. A cooled mixture consisting of 11.0 ml of distilled water, 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol A and 12.0 ml of concentrated sulfuric acid is used as a comparison solution.

In tab. Figures 4 and 5 present the results of quantitative determination of furadonin in tablets of 0.05 (series 180187) and 0.1 g (series 260185), respectively, using the photoelectric colorimetric method.

The data table. 4 and 5 indicate that the error in the determination of furadonin in tablets is 0.05 or 0.1 g each in the proposed method does not exceed А ± 1.83%.

Quantitative spectrophotometric determination of furadonin.

Build a calibration graph.

Starting from standard solution A, a series of solutions is prepared with the content of the test substance from 50.0 to 200.0 µg. For this purpose, 0.5 1.0 1.2 1.2 1.5 and 2.0 ml of standard solution A are placed into 25.0 ml volumetric flasks and the volume of distilled water that is missing up to 5.0 ml is added. To the solutions in flasks, add 4.0 ml of 0.2% freshly prepared aqueous solution of pi: 1719972

A and 12.0 ml each of concentrated concentrates

sulfuric acid. The volume of the solutions in flasks was made up to the mark with water, mixed thoroughly and cooled. After cooling, the volume of the solutions in flasks is again brought to the mark with water and stirred.

The optical density of the obtained colored solutions was measured using an SF-46 spectrophotometer at a wavelength of 7,468 nm in a cuvette with a working layer thickness of 10 mm. Mm. As a comparison solution, a cooled mixture of 11.0 ml of water, 4.0 ml of a 2.0% freshly prepared aqueous solution of pyrogallol A and 12.0 ml of concentrated sulfuric acid is used.

In tab. 6 shows the dependence of the light absorption of the colored solutions on the amount of furadonin in the samples.

The calculation of the calibration graph equation for the spectrophotometric determination of furadonin is as follows:

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0.00375

89400X2 299 - 620x3314 5789400 TB2BU ™

97

 -0,00465.

From the data table. 6 it follows that the absorption of the colored solutions of furadonin follows the Bouguer-Lambert-Beer law at concentrations of 50.0 - 400.0 µg furadonin in 25.0 ml of the final photometric solution.

These dependences of the light absorption of the colored solutions of furadonin, taken to the performance of the reaction, were used to calculate the parameters of the direct equation corresponding to the rectilinear section of the calibration graph having a common fork:

D CC + B,

where D is optical density, 1,

K - coefficient proportional to the power, equal to the tangent of the angle of inclination of the calibration graph to the x-axis

X is the content of the analyte in the sample being analyzed, μg;

B is a constant indicating in which place the graph intersects the y-axis.

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Taking into account the calculated parameters K and B, the equation of the straight line corresponding to the linear portion of the calibration graph for the spectrophotometric determination of furadonin is as follows:

D 0.00375 - 0.00465.

Spectrophotometric determination of furadonin in powder.

In a 25.0 ml volumetric flask, place 2.0 ml of an aqueous solution of furadonin containing about 100 μg of the preparation in 1 ml and 3.0 ml of distilled water. To the resulting solution was added 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol A and 10.0 ml of concentrated sulfuric acid. To the resulting solution were added 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol and 12.0 ml of concentrated sulfuric acid. The contents of the flask are thoroughly mixed, the volume of the solution in the flask is brought to the mark with water, and cooled. After cooling, the volume of the solution in the flask is brought to the mark with water and stirred again.

The optical density of the obtained colored solution was measured using an SF-46 spectrophotometer at a wavelength of ft 8 nm in a cell with a thickness of a working layer of 10.0 mm.

A cooled mixture consisting of 11.0 ml of distilled water, 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol A and 12.0 ml of a concentrated sulfuric lot is used as a comparison solution.

The calculation of the drug content in the samples is calculated according to a previously constructed calibration graph or by the direct equation corresponding to the linear portion of the calibration graph.

The results of quantitative determination of furadonin in powders by spectrophotometric method are presented in Table. 3, it can be concluded that using this method it is possible to determine the furadonin content in powders with a relative error A ± 1.29%.

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Spectrophotometric determination of furadonin tablets (0.05 g and 0.1 g).

Accurately weighing powdered furadonin tablets was quantitatively transferred to a 250.0 mL volumetric flask; 200 ml of distilled water is added and the contents of the flask are heated on a boiling water bath until complete dissolution. After cooling, the volume of the solution in flask. Is brought to the mark with distilled water and mixed thoroughly.

The required volume of the sample obtained by dissolving the suspension of furadonin tablets of 0.1 or 0.05 g each is placed in a 25.0 ml volumetric flask, up to 5.0 ml of distilled water is added, 4.0 ml of 0.2% - A freshly prepared aqueous solution of pyrogallol A and 12.0 ml of distilled sulfuric acid are mixed and the mixture is made up to the mark with water. After cooling, the mixture is again brought to the mark with water and stirred.

The optical density of the obtained colored solution was measured using an SF-46 spectrophotometer at a wavelength of 468 nm in a cuvette with a working layer thickness of 10.0 mm. As a comparison solution, a cooled mixture of 11.0 ml of distilled water, 4.0 ml of a 0.2% freshly prepared aqueous solution of pyrogallol A and 12.0 ml of concentrated sulfuric acid is used.

The results of the quantitative determination of furadonin in tablets of 0.05 or O, 1 g are spectrophotometrically shown in Table. 4 and 5, the data of which indicate TOMJ that the error in the determination of furadonin in tablets of 0.05 and in O, 1 g by the proposed method does not exceed A 11.29%.

In tab. 8 shows the dependence of the optical density of the product of the interaction of furadonin with pyrogallol A on the sequence of addition of pyrogallol A and concentrated sulfuric acid.

Conclusion Table. 8: on the value of optical density sequence

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adding reagent and concentrated sulfuric acid is not affected.

In tab. Figure 9 shows the dependence of the optical density of the product of the interaction of furadonin with pyrogallol A, depending on the amount of pyrogallol A, taken on the reaction.

Conclusion Table. 9: The optical density of the product of the interaction of furadonin with pyrogallol A is maximum, if the analysis is based on a 0.2% aqueous solution of pyrogallol A from 0.6 to 4.2 ml for 50.0 µg furadonin, and from 2.0 to 4 , 0 ml of a 0.2% aqueous solution of pyrogallol A, if 200.0 µg of furadonin is taken for analysis.

In tab. 10 shows the dependence of the optical density of the product of the interaction of furadonin with pyrogallol A depending on the amount of concentrated sulfuric acid taken per reaction.

Conclusions table. 10: The optical density of the product of the interaction of furadonin with a 0.2% aqueous solution of pyrogallol A is maximum, if the analysis is based on concentrated sulfuric acid in the range of 9-14 ml.

The data table. 1-10 makes it possible to conclude that the proposed method is useful for the quantitative determination of furadonin, both in pure form and in dosage forms. The proposed method in comparison with the known increases the sensitivity and accuracy of determination.

Claims (1)

The invention The method of quantitative determination of Furadonin by treating an analyzed sample with a chemical reagent followed by photometry of the solution obtained, characterized in that, in order to increase the accuracy and sensitivity of the determination, the treatment is carried out first with pyrogallol A, then with concentrated sulfuric acid. Table 1 uradonin m   23696.91 C - 925.01 468 nm -. (   8061.47 it / 314.68 ft 227 nm Errors of the method Powder A ± 1.29 Powder A ± 2.2 Tablets of 0.01 A ± 1.8 10.0 20.0 25.0 30.0 40.0 , 09, 7. -. (   8061.47 it / 314.68 Tablets of 0.05 A i 2,4 table 2 13 1719972 14 Continued t bl. 3 15 Furadonn 1 Resorcin Pyrogallol A 0.5 ml of a 10% aqueous solution of resorcinol and 18.0 ml of concentrated sulfuric acid were added to 5.0 ml of the sample, cooled, and the total volume was adjusted to 25.0 ml; . water, photometrically against control 478,783.32 20066.96 To 5.0 ml of the sample in a 25.0 ml volumetric flask was added 4.0 ml of a 0.2% aqueous solution of pyrogallol L and 12.0 mp of concentrated sulfuric acid, the volume was made up to the mark with water, stirred, cooled and Reconfigured to the mark with water, photometered against the control 468 925, -01 23696.91 Pirokate-K 5.0 ml of sample added Quin 2.0 ml of a 5% aqueous solution of pyrocatechin and 18.0 ml of concentrated sulfuric acid, cooled and photo. . met against control 468 694.49 17791.55 Floroglu - To a 5.0 ml sample in a 25 ml volumetric qing flask is added 1.0 ml of a 1% aqueous solution of phloroglucinol and 18.0 ml concentrated chamois acid, cool and total the volume in the flask is adjusted to water marks, photometry against control 455 593.9 14448.30 1719972 16, Table 6 Table 7 Phenol Thymol Hydroquinone 8 1-Naftol Pikrinova to-that To 5 ml of the sample was added 2.0 ml of 1% aqueous solution of phenol and 18.0 ml of concentrated sulfuric acid, cooled and photometrically against the control 468,768.01 19674.88 To 5.0 ml of the sample in a 25.0 ml volumetric flask was added 0.5 ml of 1% aqueous solution of thymol in 96% ethanol and 18.0 ml of concentrated sulfuric acid, cooled and made up to labels total volume with 96% ethanol, photometrized after .15 min versus control 468 496.10 12709.19 1.0 ml of a 5% aqueous hydroquinone solution and 18.0 ml of concentrated sulfuric acid were added to 5.0 ml of the sample in a 25.0 ml volumetric flask, cooled, and the total volume in the flask was made up to the mark with water, photometered against control 495 414.82 10599.45 To 5.0 ml of the sample in a 25.0 ml volumetric flask was added 0.25 ml of a 0.1% solution of 1-naphthol in 96% ethanol, 5.0 ml of 96% ethanol and 14.0 ml of concentrated sulfuric acid, cool and bring the total volume to the mark with 96% ethanol, photometrically against control 512; 145.13 3717.94 The reaction does not go Note. In all cases, the control is the blank solution. Continued table. 7 Table 8 Table 9  The numerical values of optical density are given as the average of three independent variables. Continued table. 9 I Table 10 23 171997224 Continued table. ten Note, the density hereinafter of three independent The numerical values of the optical in the text are given as mean variables.