SU726471A1 - Method of quantitative determining of phenothiazine derivatives - Google Patents

Description

The invention relates to analytical chemistry, namely to methods for the quantitative determination of phenothiazine derivatives-diprazine, dinazine, aminazine, chloroazisin. A known method for the quantitative determination of aminazine, which consists of the alkaline titration of the analyzed sample 1. The disadvantages of the method are this To nonspecificity, subjectivity, i.e., the physiologically active part of the molecule cannot be determined in this way. method of determination of phenothiazine derivatives, concluded in dissolving the analyzed sample in anhydrous acetic acid with the addition of a solution of acetate acetate Clear mercury followed by titration of the resulting solution with perchloric acid in the presence of an indicator. 2. The disadvantages of this method are low sensitivity and non-specificity of the determination. The aim of the invention is to increase the sensitivity and specificity of op1 chopping. The goal is achieved by a method for the quantitative determination of phenothiazine derivatives, which consists in the sequential processing of an analyzed sample by ammonium rhodium, ferric chloride and dichloroethane in the presence of hydrochloric acid, followed by separation and photocolorimetry of the colored / dichloroethane layer. Example 1. In a separating funnel, with 1.5 ml of a 1-10 M solution of diprazine, 0.5 ml of a 5 M solution of ammonium Rodanide is poured, 1.5 ml of a 0.1 M solution of ferric chloride, 0, 5 ml 0.1 n. hydrochloric acid solution. Then extracted with 5 ml of dichloroethane for G minutes. After separation of the phases, the dichloroethane layer is separated, placed in a cuvette with a layer thickness of 1 cm, and the optical density is measured on a photoelectric bromimeter with a green light filter. This method can be used to quantify the determination of phenothiazine derivatives, in dosage forms. Auxiliary and stabilizing substances. Used for

the preparation of tablets and injection solutions do not interfere with the determination.

EXAMPLE 2: One tablet containing 0.025 g of dipraenin, dissolved in distilled water in a 100 ml volumetric flask. The analysis was carried out as described above.

The quantitative content calculated by the formula

D - and X -,

s

where p is the optical density of the CTrac; ,

a, b are direct comparison factors; .

for aminazine, 06, 39 for chloroazine, 29, 10 for dinesin, G7, 82 for dipraein, 15, 50. The optical density is extracted at different wavelengths on the spectrophotometer SF-16.

As a result of the experiment, it was established that the maximum absorption of the products of the reaction of phenothiamine derivatives with the single-complex iron complex in dichloroethane is in the range 505-510 / nmT /: - ::. .. p -.- - 1. Quantitative determination of aminazine.

Chlorotherapy drug is used in medicine as vice drug, injection solutions and dragees.

726471

Calibration plotting

In a separating funnel is placed 0.5 ml of a 5 M solution of rhodium ammonium 0.5 ml of a 0.1 M solution of ferric chloride, 0.5 ml of 0.1 N. solution of hydrochloric acid and 0.5-3.3 ml of aminazine solution. Volumes are equilibrated by adding the calculated amount of distilled water. The mixture was extracted with 5 ml of dichloroethane for 1 minute. The extractant is separated and the optical density is determined on a photoelectric colorimeter. FZK-M with a green light filter in a ditch with a layer thickness of 1 cm.

determination of aminazine in the preparation of a solution; aminazine is prepared with such

calculated 1 "1 to 1 ml of it. contained 0.3-3.0 mg of aminazine. To a 0.5 ml solution of ammonium rhodanide, 0.5 ml of a solution of ferric chloride, O, 5 ml of hydrochloric acid and 1 ml of the aminazine solution under study are added. Extraction and photometry are carried out as described when plotting a calibration graph.

The quantitative content of aminazine in the solution is determined by the calibration graph or by the formula.

In parallel, quantitative determination of aminazine is carried out by a known method. The determination results are given in .tab. one.

Table 1

 In a known way, the sample is given in

B known method the amount of aminazine found in g (%),

The known method is characterized by low sensitivity; one determination takes 0.25-0.30 g

drug that b is 250 times the amount required for the analysis of the photometric method. Poi

Anhydrous titration of the drug is difficult to establish the color transition indicator.

Determination of aminazine in solution for injection.

According to the HVAC, 1 liter of the solution for injections contains, g: 25.0 aminazine, 1.0 anhydrous sodium sulfite, 1.0 sodium metabisulfite, 2.0 ascorbic acid, 6.0 sodium chloride.

Since the aminazine solution for injection, in addition to the main ingredient, contains other substances that influence and interfere with the determination of the drug by known methods, the interaction of the substances listed above with the rhodanide iron complex has been investigated. Experiments have shown that these substances do not form colored extractable reaction products with the rhodanide iron complex.

It was established that sodium sulfite, sodium metabisulfite, ascorbic acid and sodium chloride in concentrations exceeding their content against the known one 10 times do not affect the determination of aminazine in the solution for injection by the extradio-photometric method.

From tab. 2, it can be seen that the proposed method makes it possible to determine chlorpromazine in dragees without preliminary separation of auxiliary substances. The mean value is within the tolerance limits.

2. Quantitative determination of chloracizine.

Chloracizine is used in medicine as a drug.

Build a calibration graph.

In a separating funnel, place 1 ml of a 5 M solution of ammonium rhodanide, 2.5 ml of a 0.1 M solution of ferric chloride and a variable amount (0.5-2.0 ml)

726471

Method for the determination of aminazine in solution for injection.

2 ml of the injection solution is quantitatively transferred to a 50 ml volumetric flask and made up to the mark with distilled water.

In a separating funnel is placed 0.5 ml of a 5M solution of ammonium rohanide, 0.5 ml of a 0.1 M solution of ferric chloride, O, 5 ml of 0.1 and. of a solution of hydrochloric acid and 1 ml of the prepared solution of chlorpromazine. The volume is adjusted to 5 ml with water. Extracted with 5 ml of dichloroethane for 1 min. The extract is separated and the optical density is determined on a FEC-M in a cuvette with a thickness of 1 Cm with a green light filter. The content of chlorpromazine is determined by the formula:

y - 0,006 V X. ,

0

0.39 2 where X is the content of aminazine in 1 ml

injection solution, mg; y is the optical density of extraction: ta, V is the volume of the volumetric flask.

5 The results of quantitative determination of aminazine in solution for injection are given in Table. 2

table 2

1 -10- to a solution of chloroazisin. The mixture was extracted with 5 ml of dichloroethane for 1 minute, the extract was separated and the optical density was measured on FEC-M in a cuvette with a layer thickness of 1 cm with a green light filter.

The solution of chloroazisin is prepared so that 1 ml of it contains 6.2-1.0 mg of chloroazisin. Quantitative determination is carried out according to the procedure described above. The experimental data and their statistical processing are presented in Table. 3.,

In parallel, chlorine reactive chlorine is measured by a known method.

 In the known method, the sample is given in g. In the known method, the amount of chloraciein is found in g (%).

The sensitivity of the photometric method is much higher: one definition is spent 400 times less than the substance being determined than with the titrimetric method.

3 .. Quantitative determination of diprazin. .

Build a calibration graph.

In a separating funnel is placed 0.5 fvui of a 5 M solution of ammonium rhodium, 1.5 ml of 0.1 M solution of iron chloride, 0.7 ml of 0.1 N. solution of hydrochloric acid and 0.5-2.3 ml of 1-10 M solution of diprazina. Extraction reaction product. In a known method, the sample is given in g.

found ug (%).

5 ml of dichloroethane for 1 mi. The dichloroethane extract is separated and the optical density of the FEC-M in a cuvette with a layer thickness of 1 cm is determined at a green light filter.

Determination of diprazine in the preparation

Prepare a solution of diprazine containing in 1 ml of 0.16-0.80 mg of the drug. Quantitative determination is carried out according to the above method.

In parallel, the diprazine content is determined by the non-aqueous titer method. The results of the determination are given in table. 4.

Table 4

4. Quantitative determination of dinszin.

Dinesin is used in medicine ToJtbKO in the form of the drug.

Calibration plotting

To 0.5 ml of a 5 M solution of ammonium rhodanide, 1.5 ml of a 0.1 M solution of ferric chloride, 0, 3 ml of 0.1 N are poured. solution of hydrochloric acid and 0.5-2.5 ml of 1-10 M dinezin solution. The reaction product is extracted with 5 ml of dichloroethane for 1 minute. After separation of the phases, the dichloethane layer is separated and the optical density is measured on a FEC-M in a cell with a layer thickness of 1 cm with a green light filter.

The proposed method has high sensitivity, one definition is spent in the 200-400

times less than the detectable substance

what a known method requires.

The photometric extraction method is characterized by high selectivity. Sodium chloride, sodium metabisulfite, sodium sulfite, ascorbic acid auxiliary substances (talc, starch, white clay) do not interfere with the determination in an amount that exceeds their content by a known method 10 times.

Determination of the drug iropodit according to the physiologically active part of the molecule is different from the known method, where, along with the drug, its decomposition products with basic properties can be titrated.

Claims (2)

1. State formakopa, edition IX, M., Medgiz, -1961, p. 531. 2. The State Pharmacopoeia, edition X, M., Medgiz, 1968, p. 182 (prototype).