SU1416900A1 - Method of quantitative analysis of phencarol - Google Patents

Abstract

The invention relates to analytical chemistry, in particular, to the method of photometric determination of fencarol in the preparation and dosage forms, which can be used in pharmacy. The goal is to increase the specificity, selectivity and sensitivity of the method. The determination of phencarol is carried out by treating the sample being analyzed with a mixture of 5 M solution of ammonium rhodide and O, 1 M solution of iron nitrate in a volume ratio of 0.7-1.4: 1.0-1.6. The resulting colored compound is extracted with chloroform and then photometric. The method allows to reduce the detectable minimum from 30 mg / ml to 1.1 µg / / ml, determine the hydrolysis products of phencarol using this method, and also carry out the analysis in the presence of talc, starch, glucose, sugar, white clay, barbital, phenobarbital, caffeine, theophylline, theobromine and morpholine. 5 tab. i SL

Description

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This invention relates to analytical chemistry, in particular to a method for the photometric determination of phencarol (quinuclidyl-3-diphenylcarbinol hydrochloride) in a preparation and medicinal forms.

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

Calibration plotting

In a separating funnel, 1 ml of a 5 M solution of ammonium rohanide, a 0.1 M solution of iron nitrate, 0.1 and a solution of hydrochloric acid and a variable amount (0.5-4.0 ml) of a 0.004 M solution of phencarol are placed. In each case, the total volume of the mixture is adjusted to 10 ml with water. Extract 1.0 ml of chloroform for 2 minutes and measure the optical density of the extract on FEC-56 M in a cuvette with a layer thickness of 1 cm with a green light filter. Straw calibration graph of the dependence of optical density on concentration.

Example 1. Determination of phencarol in the preparation.

Exact sample of phencarol (0.12 g): dissolved in a 100 ml volumetric flask. CZ ml of the prepared solution of the drug is poured a mixture of 5 M solution of ammonium rhodium and 0.1 M solution of iron nitrate in a volume ratio of 0.7-1.4: 1.0-1.6 ml 0.1 n. hydrochloric acid solution and volume is adjusted to 10 ml with water. Next, do as described when constructing a calibration graph.

The content of phencarol is determined from a calibration graph.

In parallel, phencarol was determined by non-aqueous titration by a known method. The data presented in Table. one.

PRI and M e p 2. Definition of fenkarola tablets.

A portion of the powder rubbed tablets (0.1 g) equal to the average weight of one tablet is placed in a 25 ml volumetric flask and dissolved in water.

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de, bring to the mark with water, filter. For the study, take 1 ml of the prepared solution and carry out the determination according to the described method.

In tab. 2 shows the volume ratio of reagents used in the analysis.

In tab. 3 shows the results of the analysis using different ratios of reagents.

In tab. 4 shows the specificity of the reagent in the presence of the hydrolysis products of fencarol, which is important in determining the goodness of the preparation.

Talcum, starch, glucose, sugar, white clay, barbital, phenobarbital, coffee-in in, theophylline, theobromine, morpholine (Table 5) do not interfere with the determination of phencarol, which confirms the selectivity of the method.

The proposed method has a high sensitivity. The molar rejection ratio is 3121. The detectable minimum of phencarol for this method is 1.1 µg / ml.

Thus, the proposed method has a high sensitivity, rapid, reproducible, objective assessment of results, eliminates the use of toxic, volatile compounds (acetic and perchloric acids, mercury acetate). The method is easy to perform, the hardware is available.

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Claims (1)

Invention Formula The method of quantitative determination of phencarol by treating the sample being analyzed with a chemical reagent, characterized in that, in order to increase specificity, selectivity, sensitivity and sensitivity, a mixture of 5 M ammonium rhodanide solution and 0.1 M iron nitrate solution is used as a chemical reagent 0.7-1.4: 1.0-1.6, the resulting colored compound is extracted with chloroform, followed by photometric measurement. 314169004 Table 1 Comparative evaluation of quantitative methods table 2 The volume ratio of a mixture of solutions of ammonium rhodanide and iron nitrate Maximum Table The results of the quantitative determination of fenkarol at the maximum and minimum ratio of reagents 3.67 98.1, 9. 3.75100.0 3.75100.0. ta,, 271 3.75100.0, 95 3.75100.0, 13% 3,80101,5 102,, 1 100, 100.0ta ,, 271 98, 95 100, 09% 100.0 5U16900 T a b i c a 4. The effect of the hydrolysis products of fencarol on the results of quantitative definitions Table3 Comparative characteristics of the proposed and known methods Characteristic The proposed method Analysis time, min Consumption of the drug Toxicity Specificity 3-5 mg ten 0.3 g The reagents used are perchloric acid, ammonium rhodanide acetate and nitro mercury (II) are very toxic. Iron is not toxic and requires special precautions. The hydrolysis products of the op. The hydrolysis products are jointly determined by this method; the drug is titrated with chlorochloric acid. minimum Talc, starch, glucose, sugar, white clay, barbital, phenobarbital, caffeine, theophylline, theobromine, morpholine do not interfere with the determination. 1.1 µg / ml VNIIPI Order 4060/42 Random polygons pr-tie, Uzhgorod, st. Project, 4 Known method ten 0.3 g Interfere with the determination of talc, starch, glucose, white clay, caffeine, morpholine 30 mg / ml Circulation 847 Subscription