SU1627939A1 - A method for quantifying oxymethylamine carboxylic acid - Google Patents

Abstract

This invention relates to knowledge chemistry, in particular to methods for the determination of pyridine-3-carboxylic acid oxymethylamide (the drug is nicodine). The purpose of the invention is to increase the sensitivity and accuracy of determination. For this purpose, solutions of ammonium rhodanide and chloramine B in an acidic medium are added to the analyzed sample, then a solution of sulfophenylmethylpyrazolone in an alkaline medium (pH 8.2-8.6) and the resulting colored solution is photometricized at 530 nm. 1 tab. (I

Description

This invention relates to analytical chemistry, and specifically to methods for the determination of pyridine-3-carboxylic acid oximethylamide (drug nicodine).

The purpose of the invention is to increase the sensitivity and accuracy of determination.

The method is carried out as follows.

The analyzed sample is treated with a 1% solution of ammonium rodanide and a 1% solution of chloramine B in an acidic medium created by 0.1 n. solution of hydrochloric acid, 0.38 / 4-nym solution of sulfophenylmethylpyrazolone (0.03-0.05 mg) in the presence of universal buffer solutions pH 8.2

8.6; colored reaction products photometrically at 530 nm "

The detection limit is 0.05 µg / ml. Submission to the law of faith in the range of 0.05-0.5 mg of nicodine in 25 ml of solution.

Example. I ml of a standard nicodine standard sample solution (0.0005 g / ml) is introduced into a 25 ml volumetric flask, and 1 ml of the test solution is added to another one. 1 ml of 0.1 N is added to both flasks. hydrochloric acid solution, 1 ml of a 1% ammonium rhodanide solution, 8 ml of a 1% solution of chloramine B and leave for 10-15 minutes. Further, 1.8 ml of 0.1 N are added. pacfBOpa sodium hydroxide, 0.8 ml 0.38% solution

about

1C

NJ

with

WITH

with

sulfophenylmethyl pyrazolone and volume in flasks with buffer solution pH 8.4 to the markers. After 30-40 minutes, measure the optical density of the colored solutions on FEC-56M in cuvettes with a layer thickness of 10 mm with a green light filter. The comparison solution is a solution containing all the above reagents, except for the test solution

The content of the drug is calculated by the formula

Mr. -) SЈ,

cx ,

where DQ is the optical density of the standard sample solution;

C0 is the concentration of the solution of the dart sample, g;

)% is the optical density of the test solution;

Su is the concentration of nicodine in the test solution, g. Agates for determining the content in the sample are given in the table.

NIKO1

Tse,

F o h

1 v l and

inventing

n and

1: CQ of quantitative determination of pyridine-3 carboxylic acid oimothylamide, including the treatment of the ai and 1 sample with solutions

of ammonium robanide and chloramine B in an acidic medium, adding glutaco derivative to the solution | A new aldehyde solution of the color-reagent, measuring the optical density of the resulting colored solution, by which the concentration of the substance being determined is judged, characterized in that, in order to increase the sensitivity and accuracy of the determination, the solution of the glutaconic aldehyde derivative is alkalized to pH 8.2-8 , 6 and a 0.38% solution of the color reagent — sulfophenylmethylpyrazolone — is added, and the optical density of the colored solution is measured at 530 nm

Metrological characteristics

25 0, jOGU 100.00 99.40% - average

0, 98.96 arithmetic out of 5

definitions

О 497 99.42 0.17 - average quad, 0, 99.14, ratification deviation

0.497з 99.50 ± 0.47 - relative error

Claims (1)

<claim-text> <table border = "1"> <tbody> <tr> <td colspan = "3"> 20 ——————— </ td> <td rowspan = "2"> Metrological characteristics </ td> </ tr> <tr> <td> </ td> <td> Caideo ΞΖ1 </ td> <td> % </ td> </ tr> <tr> <td> 25 </ td> <td> OOOOOO </ td> <td> 100.00 </ td> <td> 99.40% - average </ td> </ tr> <tr> <td> </ td> <td> 0.494Y </ td> <td> 98.96 </ td> <td> arithmetic of 5 definitions </ td> </ tr> <tr> <td> </ td> <td> 0.437 '</ td> <td> 99.42 </ td> <td> 0.17 - quadratic mean - </ td> </ tr> <tr> <td> </ td> <td> 0.49 l </ td> <td> 99.14 </ td> <td> ratification rejection - </ td> </ tr> <tr> <td> 30 </ td> <td> </ td> <td> </ td> <td> </ td> </ tr> <tr> <td> </ td> <td> 0.49 / 3 </ td> <td> 99.50 </ td> <td> ± 0.47 - relative </ td> </ tr> </ tbody> </ table> <claim-text> error </ claim-text> <claim-text> A.Dolinich Redakyur </ claim-text>