SU968714A1 - Khellin determining method - Google Patents

Description

(54) METHOD FOR DETERMINING KELLIN

one

The invention relates to analytical chemistry, in particular to methods for determining the drug drug-2-methyl-5, 8-dimethoxyfuro-4,5:: 6,73 chromone-kellin and can be used to analyze this compound in various materials required for clinical research and dosage forms.

A known method for the determination of kellin, based on the use of the LO polygraph.

The disadvantage of this method is low sensitivity, 25 µg / ml.

Closest to the proposed technical essence and the achieved results is a method for determining kellin by dissolving the analyte in ethanol, followed by measuring the optical density of the resulting solution t 2.

The disadvantage of this method is its low sensitivity (6 μg / ml) and non-selectivity.

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

This goal is achieved in that according to the method of determining 10 kellin by dissolving the analyte in chloroform, followed by measuring the fluorescence intensity of the resulting solution, chloroform is used as an organic solvent and, after dissolving, the fluorescence intensity of the resulting solution is measured.

The proposed method allows, without separation from related ingredients, quantitative determination of kellin in complex dosage forms, and high sensitivity (0.1 µg / ml) and selectivity allows it to be used for quantitative determination of kellin in biological fluids.

at

It was found that Kellin fluorescence intensity in chloroform does not change for 2 hours. Kellin fluorescence intensity dependence in chloroform (µg / ml on pH remains constant in the interval. Fluorescence excitation spectrum lies in the range of 350 nm , and the fluorescence emission spectrum is from 375 to 520 nm with a maximum of 460 nm. The linear relationship between the fluorescence intensity and kellin concentration corresponds to 0.1-70 µg / ml kellin.

Example 1. Quantitative determination of kellin.

PRI mme R 2. The definition of kellin tablets kellatrine tablets of the following composition:

Kellin0.02

Papaverine hydrochloride Oh, 02 Atropine sulfate 0.00025

A dark portion of the finely divided tablet (0.03 g) is placed in a 100 ml volumetric flask. Add 8 mL of chloroform and shake vigorously.

5-10 minutes, chloroform is added and stirred. 7 ml of chloroform was added to 3 ml of this solution, shaken, and the fluorescence intensity was measured. The kellin content is calculated from a calibration curve, for which 1.0 is measured in a series of tubes; 3.0; 5.0; 7.0 and 10 ml of the standard solution of kellin in chloroform with a content of 100 µg / ml, bring all

solutions up to 10 ml of chloroform, shaken and fluorimetric simultaneously with the solution of the samples under study. According to the results of these measurements, a calibration graph is constructed. The results of the quantitative fluorimetric determination of kellin in tablets of 0.02 g are presented in Table 1.

Table 1

A fine sample (0.05 g) of a finely divided tablet is placed in a volumetric flask of 10O ml, 3050 ml of chloroform is added, shaken vigorously for 5 minutes, chloroform is added to the mark, and mixed. To 3 ml of this solution was added 7 ml of chloro-596871 "

shape and measure the fluorescence intensity of the quantitative fluorescence. The kellin content is calculated by the calibration graph in kellatrine tablets (see example 1.c in table 2. Example 3. Kellin determination in vikalin tablets of the following composition: Basic bismuth magnesium carbonate basic sodium carbonate calamus powder and buckthorn bark Rutin and kellin. An exact weight (0.1 g of finely divided tablet is placed in measures

12 11

0.1219 0.1173

table 2

.0,0049

0.0047 0.0046 50 ml flask, add 30 ml of chloroform and shake vigorously for 5 minutes, add chloroform to the mark, mix. 10 ml of this solution is transferred to a cuvette and the fluorescence intensity is measured. Kellin content is calculated according to a calibration graph (see example C) The results of quantitative fluorimetric determination of kellin in vikalin tablets are presented in Table 3. Table 3

eight

e (Continuation of table. 3

Claims (1)

Claim The method of determining kellin by dissolving the analyte 35 in an organic solvent, characterized in that, in order to increase the sensitivity and selectivity of the method, 40 chloroform is used as an organic solvent, and after dissolution with modified kellin solutions with a content of 1.0; 3.0; 5.0; 7.0 and 10.0 μg / ml in chloroform. The proposed method is 60 times _{4 more} sensitive than the known one, which makes it possible to effectively use it in biopharmaceutical and other biochemical studies to develop the optimal Compose.