SU1231442A1 - Method of determining camphor - Google Patents

Abstract

The invention relates to analytical chemistry, in particular, to methods for the qualitative and quantitative determination of camphor (1,7,7-trimethylbicyclo-2,2,1-heptanone-2) - a medicinal preparation with an analeptic effect. In order to improve the accuracy and sensitivity of the determination, reduce its duration and reduce the toxicity of the determination, the method is carried out by treating the analyzed sample with 2-dinitrophenshidrazin perchlorate 2 in ethanol at a molar ratio of the analyzed sample and 2,4-dinitrophenylhydrazine 1: 1.5 perchlorate , heating in a boiling water bath for 6–10 min, adding sodium hydroxide to the resulting solution, followed by photometric measurement of the product obtained. The determination error is 2.05-2.72%. Sensitivity 0,002-0,01%. The time is significantly reduced and the detection toxicity decreases. 3 tab. C IAD I th

Description

one

The invention relates to the chemical and pharmaceutical industry, as well as to the analysis of medicinal substances, and in particular to methods for the qualitative and quantitative determination of camphor (1,7,7-trimethylbicyclo -2,2,1-heptanone-2) - a drug that has - kim action.

The purpose of the invention is to improve the accuracy and sensitivity of the determination, reduce its duration and reduce toxicity in determining

Example 1, qualitative definition. ,

0.001 g of camphor is dissolved in 1 ml of ethanol, 5 drops of a 0.005 M solution of 2,4-dinitrophenylhydrazine perchlorate are added. The mixture is heated on a spirit lamp for 1 min, cooled, 1 drop of 2.5 M hydroxy sodium solution is added, a dark cherry color is formed, which should not disappear with the addition of 3 ml of distilled water.

Example 2. Quantitative determination of camphor.

About 0.025 g (exact weight) of camphor is placed in a flask or test tube, dissolved in 5 ml of ethanol, 4 ml of a 0.005 M solution of 2,4-dinitrophenylhydrazine perchlorate is added, the reaction mass is heated on a boiling water bath for 10 minutes, cooled and transferred into a 100 ml volumetric flask, made up to the mark with ethanol, 2 ml of the reaction mass are taken, 4 ml of ethanol and 2 drops of 2.5 M sodium hydroxide solution are added, a dark cherry coloration is formed, incubated for 5-7 minutes.

The optical density of the solution was measured on a photoelectric bromide meter with a transmission maximum of 490 nm and a layer thickness of 1 cm. The measurement was carried out against a control sample.

The content of camphor (x) in the preparation (according to 2,4-dinitrophenylhydrazone) in percent is calculated by the formula

a-V.100 „X -%; where a

quantity

mg of 2,4-dinitrophenylhydrazone in 1 ml, found from the calibration graph b - the actual amount of camphor in solution, mg; V - solution volume, ml. Preparation of the control sample.

31442i

4 kp of a 0.005 M solution of 2,4-dinitro-phenylhydrase are placed in a 100 ml flask, made up to the mark with ethanol, the mixture is stirred, 2 ml of plant solution are taken and 4 ml of ethanol are added and

2 drops of a 10% sodium hydroxide solution form a dark cherry stain. After 5-7 minutes, absorbance is measured in parallel with

10 trial breakdown.

Preparation of standard solutions.

To construct a calibration graph, 0.5 g (0.003 M) of camphor is placed in a 50 ml flask, dissolved in 5 ml of ethanol, and 0.99 g (0 (005 M) of 2,4-dinitrophenylhydrazine perchlorate) is added. The reaction mass is heated in boiling water

20 bath for 10 minutes, cool,

The precipitate of camphor 2,4-dinitrophenylhydrogen is filtered off and dried.

0.05 g (exact weight) of camphor 2,4-di25 nitrophenyl hydrazone is placed in a 50 ml volumetric flask, dissolved in ethanol, and brought to the mark. Take 2: ml; 1 ml; 0.75 ml; 0.5 ml; 0.3 ml of volume is made up to 10 ml each, from JQ 2 ml are taken here, 4 ml of ethanol and 2 drops of 10% sodium hydroxide solution are added, and a dark cherry color is formed.

After 5-7 minutes, the optical

.., the density of each solution at 490 nm and a layer thickness of 1 cm. Ethanol is used as a control for standard solutions.

The calibration graph is made by ordinary use, setting off on the abscissa axis the concentration of the standard solution of 2,4-dinitrophenylhydrazone camphor in mg per 1 ml, on the ordinate axis the density A,

PRI and MER 3. About 0.025 g (weighing powder) of a powder containing 0.02 g camphor and 0.005 g papaverine hydrochloride are placed in a flask, dissolved in 5 ml of ethanol, 4 ml of 0.005 M perchlorate 2 solution is added. , 4-dinitrophenylhydrazine, the reaction mass is heated in a boiling water bath for 10 minutes, cooled, transferred to a 5–50 ml volumetric flask, and made up to the mark with ethanol. Then they proceed in the same way as in Example 2. The measurement is carried out according to the principle of identi- ty, i.e. in control rast30

31

0.005 g of papaverine hydrochloride is added to the thief.

Preparation of 2,4-dinitrophenylhydrazine perchlorate solution.

1 g of 2,4-dinitrophenylhydrazine is placed in a 0 ml volumetric flask, 20 ml of a 4% aqueous solution of perchloric acid is added, then brought to the mark with ethanol and filtered.

PRI me R 4. About 0.025 g (precise weighting) of camphor was placed in a flask, a solution of 1 ppm in 5 ml of ethanol, 3 ml of a 0.005 M solution of 2,4-dinitrophenyl hydrazine perchlorate was added (analyte: reagent ratio 1: 1, 2) the reaction mass of heat314424

 water bath for

10 min, then proceed as in example 2.

EXAMPLE 5 About 0.025 g of a camfor 5 (exact sample) was placed in a flask, dissolved in 5 ml of ethanol, 5 ml of a 0.005 M solution of 2,4-dinitrophenyl hydrazine perchlorate was added (the ratio being analyzed sample: re- 10 agent 1: 1.7), the reaction mass is heated in a water bath for 10 minutes, then proceeds as in example 2.

Table 1 shows the metrological characteristics of the proposed method.

Table 1

$ 1231442

Table 2 shows the metrological characteristics of known results. The known method is poorly reproducible to quantify camphor, the error has a high percentage of ± 4.90-5.39% in comparison with the results of the proposed method, the error of which lies within 2.05 -2.72%.

The sensitivity of camphor determination by a known method is in the range of 0.005-0.01%, while the proposed method has a higher sensitivity of 0.002-0.01%.

Table 3 shows the dependence of the optical density of camphor 2,4-dinitrophenyl-hydrazone in ethanol on the heating time.

Editor A.Dolinich

Compiled by V.Shkilkov Tehred I.Gaidosh

Order 2559/49 Circulation 778 Subscription

VNIIPI USSR State Committee

for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab, 4/5

Production and printing company, Uzhgorod, st. Project, 4

Table 3

five

processing the analyzed sample with 2,4-β-dinitrophenylhydrazine in an alcohol medium, heating in a boiling water bath followed by photometry of the obtained product, characterized in that, in order to increase the accuracy and sensitivity of the determination, reduce its duration and reduce toxicity in determining ethanol is used as an alcohol; 2,4-dinitrophenylhydrazine is used as perchlorate with a molar ratio of the sample being analyzed and 2,4-dinitrophenylhydrazine perchlorate 1: 1.5, heating is carried out for 6–10 min. otometrirovaniem added to the resulting sodium hydroxide solution.

Corrector T, Kolb

Claims (1)

Claim The method for determining camphor by processing the analyzed sample with 2,4-dinitrophenylhydrazine in an alcohol medium, heating in a boiling water bath, followed by photometry of the obtained product, characterized in that, in order to increase the accuracy and sensitivity of the determination, reduce its duration and reduce toxicity when determining, in ethanol is used as alcohol, 2,4-dinitrophenylhydrazine is used in the form of perchlorate at a molar ratio of the analyzed sample and 2,4-dinitrophenylhydrazine perchlorate 1: 1.5, heating of 6-10 minutes and is performed before photometric added to the resulting solution of sodium hydroxide.