SU1748057A1 - Method of determination of 5-nitrofurane derivatives and semi-products - Google Patents

Abstract

SUMMARY OF THE INVENTION: A sample is applied to a chromatographic plate. Chromatography is carried out using ethyl acetate as the mobile phase. After chromatography and removal of the excess ethyl acetate by drying, the plate is chlorinated, dried and treated with a developing agent consisting of an acetic acid solution of a mixture of 4,4-tetramethyldiamino-diphenylmethane, ninhydrin and iodine stone. 2 tab.

Description

The invention relates to chemical methods of determination, derivatives of 5-nitrofuran and their intermediate products using chromatographic separation methods, in particular thin-layer chromatography (TLC), and can be used to determine the content of furadonin, furagin, furacilin, furazolidone, hydantoin and 1-amino-hydantoin in pure form, in mixtures, in dosage forms, in the practice of control and analytical laboratories and pharmacies.

A known method for the determination of 5-nitrofuran derivatives by thin layer chromatography using methylene chloride – methyl alcohol – 10% aqueous ammonia as the mobile phase at a ratio of 80: 20: 3.

The disadvantage of this method is low sensitivity and the use of expensive reagents (methylene chloride).

The closest to the present invention is a method for the determination of 5-nitrofuran derivatives and intermediates for their synthesis, which consists in the fact that solutions of furagin, furacilin, furazolidone in dimethylformamide and dimethylformamide extracts from ointments and suppositories are applied to a chromatographic plate with an unfixed layer of aluminum oxide. The solvents used were a mixture of ethyl alcohol with acetone (1: 1), acetone, a mixture of acetone with ethyl acetate (7: 3), chloroform. The color of the obtained spots was observed under daylight without manifestation, as well as after treatment with 50% sodium hydroxide solution or under UV light. The minimum detectable amount is 5 µg.

The disadvantage of this method is its low sensitivity.

AND

00

about

SP XI

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

The goal is achieved by the fact that a sample containing furadonin, furagin, furazolidone furacillin, as well as their semi-products of synthesis - 1-amino hydantoin and hydo-toin, is applied on

chromatographic plate: Silufol UV- 254 with a thin fixed layer of silica gel. Chromatography is carried out using ethyl acetate as the mobile phase. After chromatography and removal by drying of ethyl acetate, the plate is chlorinated with free chlorine, dried, disposing of excess chlorine and treated with a developing reagent (TDM) consisting of an acetic acid solution of a mixture of 4,4-tetramethyldiaminodiphenylmethane, K1 and ninhydrin .

The method is carried out as follows.

PRI me R 1. Chromatographic determination of 5-nitrofuran derivatives and semi-products of their synthesis.

A series of witness solutions is prepared, 1 ml of which contains 10 µg furadonin, furagin, furacilin, furazolidone, 1-amino hydantoin, or hydantoine.

On the start line of the Sllufol UV-254 plate, 0.01 ml of the indicated aqueous solutions are applied using calibrated capillaries. After drying the zones, the chromatogram is placed in a chromatographic chamber, which was previously placed with ethyl acetate as a mobile phase. After the solvent front reaches 10 cm, the chromatographic plate is removed from the chamber, dried and placed for 15 min. chlorine vapors, which are obtained by the action of 6 ml of co-concentrated hydrochloric acid per 2 g of potassium permanganate. Then excess chlorine is blown off the plate with air and the chromatogram is sprayed with developing reagent (TDM), which is prepared as follows:

Solution, 5 g of 4,4-tetramethyldiaminodiphenylmethane in 10 ml of glacial acetic acid and 50 ml of distilled water. Solution h B: 5% aqueous solution of potassium iodide.

Solution, 3g of ninhydrin in 10 ml of pedal acetic acid and 90 ml of distilled water.

Solution A is mixed with Solution B and the mixture is added with 1.5 ml of Solution B,

Zones of furadonin (Rf 0.83), furagin (Rf - 0.87), furazolidoia (Rf 0 37), furacilin (Rf 0.22), 1-amino nidangoina 0.31), hydantoin (Rf 0.25) are detected on chromatogram in the form of dark blue spots.

PRI me R 2, Chromatographic separation of a mixture of 5-nitrofuran derivatives and intermediates for their synthesis. Prepare the solution by mixing 10 ml of the prepared aqueous solutions, in 1 ml of which 10 µg furadonin, furagin, furacilin, furazolidone, 1-amino-hydantoin, hydantoin are each contained.

On the starting line of the Silufol UV-254 plate, 0.01 ml of the indicated aqueous solutions and the prepared mixture are applied using calibrated capillaries. After drying the zones, the chromatogram is placed in a chromatography chamber, in which ethyl acetate has previously been placed as a mobile phase. After the mileage of the front of the solvent reaches 10 cm, the chromatographic plate is removed from the chamber, dried and placed for 15 minutes in a chamber saturated with chlorine vapor, which is obtained by the action of 6 ml of concentrated hydrochloric acid per 2 g of potassium permanganate. Then excess chlorine is blown off the plate with air and the chromatogram is sprayed with a developing reagent (TDM, the preparation conditions are given above).

Example 3: Chromatographic determination of furagin, furadonin, furacillin, furazolidone in tablets of 0.05 g. The tablet of the test drug is triturated in a porcelain mortar to obtain a homogeneous mass. The resulting powder was dissolved in 10 ml of distilled water and filtered through a red tape filter previously moistened with distilled water. O.OJ ml of the test solution was applied to the Silufol UV-254 starting line using calibrated capillaries. After drying the zones, the chromatogram was placed in a chromatographic chamber into which ethyl acetate was previously placed as the mobile phase. After the solvent front run reaches 10 cm, the chromatographic plate is removed from the chamber, dried, and placed for 15 minutes in a chamber saturated with chlorine vapor, which is obtained by the action of concentrated hydrochloric acid (6 ml) per 2 g of potassium permanganate. Then excess chlorine is blown off the plate with air and the chromatogram is sprayed with a developing reagent (TDM, the preparation conditions are given above),

Rf penta furadonin, furagin, furacillin, furazolidone are compared with the Rf values shown in Table 1.

Comparative characteristics of the proposed and known methods are given in Tables 1 and 2.

Thus, the method makes it possible to more sensitively determine the components of a medicinal mixture of a complex composition, which makes it possible to use it both in the analysis of tablets of individual drugs and in the analysis of complex drugs to confirm the purity and homogeneity of the drugs.

0

five

Claims (1)

Claims The method of determining the derivatives of 5-nitrofuran and their intermediate products by applying the sample to a chromatographic separation plate using a mobile phase, followed by treating the plate with a reagent, characterized in that, in order to increase the detection sensitivity, ethyl acetate is used as the mobile phase, Before the treatment with the reagent, the plate is chlorinated and dried, and acetic acid solution of 4,4-tetramethyldiaminodiphenylmethane iodide is used as a reagent. and ninhydrin. Table 1 The obtained values of Rf and the sensitivity of the determination of derivatives of 5-nitrofuran and semi-products of their synthesis The mobile phase is ethyl acetate. table 2 The Rf values and the stain color for furagin, furazolidone and furatsillin according to the known way;