SU1377688A1 - Method of determining aceclidene - Google Patents

Abstract

The invention relates to analytical chemistry, in particular to the determination of aceclidine used as a pharmaceutical in medicine. To reduce the analysis time and increase its accuracy in processing the water solution of the sample with a color reagent, a mixture of 1 M CoSO solution and NEfNCS solution (volume ratio (0.8–1.8): (0.8–15) is used as the latter. Then the solution is extracted with other the solvent is dichloroethane and the photometry of the colored extract is carried out. The dosage forms are analyzed in 5-10 minutes with a relative error of ± 0.88 versus 1.7% in the known method. Table 7 i (L

Description

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but

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The invention relates to analytical chemistry, and specifically to methods for the extraction-photometric determination of aceclidine (3-acetoxyquinuclidine salicylate) „

The purpose of the invention is to improve the accuracy of the determination and reduce the analysis time.

the volume ratios of 1 M cobalt sulfate and 5 M ammonium radium are given in the proposed method to maintain a quantitative determination of between 2.4 and 24–24 Sensitivity of method 1 At a wavelength of 630 nm

Example 1. Exact mass (approx. 1.3-10)

0.05 g) of aceclidine is placed in a 25 ml measuring coil, the contents of the flask are dissolved in water and the water is made up to the mark in a separating funnel

Example 2 Determination of clidine in solution for in. 3 ml of a 0.2% solution of a are introduced into a separator

whether

e13776882

volume ratios of 1 M solution of cobalt sulfate and 5 M solution of ammonium rhodanide are given in Table 1-6. The proposed method allows a quantitative determination of aceclidine in the range of 2.4-24 mg / 5 ml. "Method sensitivity 1.20 µg / ml 630 nm wavelength molar coefficient Q = 1.3-10

Example 2: Determination of aceclidine in the injection solution, 3 ml of a 0.2% aceclidine solution are added to a separatory funnel and then

3 ml of the obtained solution are introduced, 1 ml of 5 is carried out as in Example 1.

1m cobalt sulfate solution, 1 ml of 5 M ammonium rhodanide solution. The mixture is extracted with dichloroethane for 2 minutes. The extract was separated and after 1 min the optical density was measured using a FEK-56M photoelectrocolorimeter with a red light filter in a cell with a layer thickness of 1 cm см

In parallel, the measurement of the optical density of a dichloroethane extract of a standard solution of aceclidine

The content of aceclidine in percent (x) is calculated by the formula

DJL OiOlOO -100% V,

- optical density of the studied extract; - optical density of extract-35 ta using a standard solution;

- the sample of the analyte, g;

40

40

breeding capacity;

aceclidine content

1 ml of a standard solution (a standard solution of aceclidine is prepared by dissolving a drug that meets the requirements of the State Pharmacopoeia, X ed). The results of a quantitative definition are 50%, as an organic dilution of aceclidine for various

20

25

thirty

five

0

X -

The content of aceclidine in grams (x) is determined by the formula

D ,, 0100

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Results of quantitative determination of aceclidine in. injection solution c.

The proposed method of quantitative determination of aceclidia in the preparation and dosage forms is simple to perform, has sufficient accuracy, sensitivity, the reagents used are stable, the analysis takes 5-10 minutes.

The relative error of the proposed method is ± 0.88%, while the known value is ± 1.57%

Claims (1)

Invention Formula The method of determining aceclidine by dissolving the sample being analyzed in water, treating the resulting solution with a color reagent, extracting the colored compound with an organic solvent, followed by photometry of the extract, is different from that with the aim of reducing the analysis time, As a color reagent, a mixture of ω cobalt sulfate solution and a 5M ammonium rhodanide solution, taken in a volume ratio of 0.8-1.8: 0.8-1.5, is used, respectively, dichloroethane is used. The results of quantitative determination of aceclidine at volume ratios of cobalt sulfate and ammonium rhodanide 0.8: 0.8 table 2 The results of the quantitative determination of aceclidine with volume ratios of cobalt sulfate and ammonium rhodanide 1.8: 1.5 Table 1 513776886 Table3 The results of the quantitative determination of aceclidine at volume ratios of cobalt sulfate and ammonium rhodanide 1.0: 1.2 ... Found Statistical T „processing of results 0.0500100.00X 100.00 p 6 0.0560101.20 S 0.78 0.049398.60S 0.88 0.049899, 36 0.0500100.0.88 0.0503100, 0.88% T a b l and c a 4 Tats of quantitative determination of aceclidine cobalt sulphate and roammonium sulfate ratios 0.7: 0.8 .-Statistical analysis of results 0.0340 68.00 Statistical processing .0.0417 83.33 results are not held since 0.0399 79.60 method is not reproducible 0.0378 75.50 0.0387 .77.30 0.0376 75.30 7 37.76888 Table 5 The results of the quantitative determination of aceclidine at volume ratios of cobalt sulfate and ammonium rhodanide 0.8: 0.7 Found Statistical 1 „result processing 0.0403 80.60 Statistical processing of results 0.0388 77.50 not held, so as a method not repro, 0398 79.60 we exhaust 0.0387 77.30 0.0395 79.00 0.0400 80.00 Table 6 You can quantify aceclidine with cobalt sulfate and ammonium rhodanide: 1.9: 1.6 Found Statistical 1 „result processing 0.0418 0.0398 0.0446 0.0425 0.0407 0.0403 83.60 79.60 89.10 85.05 81.50 80.60 Statistical processing of the results was not carried out, because the method is not reproducible. 1377688 Table 7 The results of quantitative determination of aceclidine in the solution for injection of 0.2% Look, then Found, g (Permissible deviations 0.0018 0.0020 0.0022 0.0020 0.0018 0.0022 ten 0,0018-0,0022