SU834467A1 - Method of 1,2,5-trimethyl-4-propionyloxi-4-phenylpyperidyn hydrochloride quantitative determination - Google Patents

Description

54) METHOD FOR QUANTITATIVE DETERMINATION OF 1,2,5-TRIMETHYL-4-PROPIONYL-OXY-4PHENYLPIPERIDINE HYDROCHLORIDE

fiku, which is constructed as follows. To 1 ml of a standard aqueous solution of Promedol containing 500 μg / ml, 9 ml of a 1% solution of formaldehyde in concentrated sulfuric acid are added and mixed thoroughly. Then, O, B, O, 7, 0.8, 0.9 and 1.0 ml of the obtained solution are measured and distilled water is added to 10 ml. The obtained solutions are fluorimetric in parallel with the solutions of the studied samples. Based on the results of these measurements, a calibration chart is constructed.

The results of the fluorimetric determination of a 2% aqueous solution of promedol are presented in Table. 1. Table

Example 2. Determination of prome dol in tablets of 0.025 g. 0.1 g (exact batch) of finely divided tablets are transferred into a 50 ml volumetric flask, 30 ml of distilled water are added and vigorously shaken until completely dissolved. Then, add distilled water to the mark and mix thoroughly again. To 1 ml of this solution was added 9 ml of 1% aqueous solution of formaldehyde in concentrated. sulfuric acid, mix. To 1 ml of the solution obtained was added 9 ml of distilled water and measured in0, 1034.8

0.099- 4.5

table 2

0.0240 0.0225

X 0.02325 fluorescence intensity. The content of promedol is determined by the standard solution, for the preparation of which to 1 ml of a standard aqueous solution with a preparation content of 1000 was added 9 ml of a 1% solution of formaldehyde in concentrated sulfuric acid, stirred. And 0.5 ml of this solution added 9.5 ml of distilled water and fluoridated simultaneously with the solutions of the test samples. The results of fluorimetric determination of promedol in tablets of 0.025 g are presented in Table. 2

Example 3. Determination of promedol in serum .. 5 ml of the studied oxalate blood is placed in a centrifuge tube and centrifuged for 30 minutes at 8 kb / min. 10 ml of chloroform was added to a 2 ml centrifugal separatory funnel and stirred for 20 minutes. The chloroform layer was separated into an evaporating dish. Extraction is repeated. Chloroform is evaporated in a water bath at a temperature not exceeding 90 ° C. To the dry residue, 1 ml of 1% formaldehyde solution in concentrated sulfuric acid is poured, mixed thoroughly, 9 ml of distilled water is added and the fluor is transferred to the cuvette.

6.9

7.4 7.9 5.9

6.5 6.7 8.4

7, (T

Continued table. 2

The meter, Fluorimetry simultaneously with the standard samples. The amount of promedol in the test specimen is determined by the calibration

0 schedule for the construction of which to 1 ml of a standard aqueous solution of the drug with a concentration of 1000 µg / ml add 9 ml of 1% aqueous solution of formaldehyde in concentrated

5 sulfuric acid. 9.9, 9.5 and 9.0 ml of distilled water are added to 0.1, 0.5 and 1.0 ml of this solution, respectively. Standard samples. Fluorimeter simultaneously with the investigated solutions.

Data on the determination of promedol in the serum are given in the table.

bloody

Metrological

B ± 3.76

2o ,, 688 The true value of the parameter to be determined: A 35.8 + 2,688

35.0 Example 4, Determination of promidol in urine. 10 ml of chloroform is added to 2 ml of urine in a separatory funnel and stirred for 10 minutes. Extraction is repeated. The chloroform layer is separated into a porcelain dish for evaporation. Evaporated in a water bath at. To the dry residue is poured 1 ml of 1% formaldehyde solution in concentrated sulfuric acid ,. mix thoroughly, add 9 ml of distilled water. The resulting solution is transferred to a fluorometer cuvette and fluorimetric simultaneously.

The determination was made on a domestic electronic fluorometer EF-ZMA with filters and. The spectra were measured on a Hitachi fluorescence spectrophotometer, model MPF-2A, manufactured in Japan.

The concentration of the formaldehyde solution in concentrated sulfuric acid used to process the sample being analyzed is from 0.001 to 0.3 g / ml. Optimum concentrations are from 0.01 to 0.1 g / ml. In fact, the concentration of formaldehyde in concentrated sulfuric acid of 0.01 g / ml was used to determine promedol.

The dependence of the fluorescence intensity on the ratio of the form of dehydrate in sulfuric acid is given in Table. five

Table3

Studying the optimal conditions for the fluorescent reaction of promelole with formaldehyde in sulfuric acid, the influence of the ratio of the volumes of the aqueous phase (standard aqueous solution of promedol) and the phase of concentrated sulfuric acid with formaldehyde on the fluorescence intensity (Table 6), the optimum ratio of volumes 3: 1 (formaldehyde solution in concentrated sulfuric acid: aqueous solution of promedol).

The dependence of the relative fluorescence intensity on the volume ratio of the phases of sulfuric acid and with standard samples. The amount of promedol in the test sample is determined according to a calibration graph, to build which, 9 ml of a 1% formaldehyde solution in concentrated sulfuric acid is added to 1 ml of a standard aqueous solution of a preparation with a concentration of 1000 µg / ml. 9.9, 9.5 and 9.0 4P distilled water are added to 0.1, 0.5 and 1.0 ml of this solution. Standard samples fluoridate simultaneously with the test solutions. Data on the determination of promedol in the urine are reflected in the table. 4. T and l and c and 4

an aqueous solution of Promedol is given in Table. 6

Table 6 When studying the optimal ratios of the volume of a mixture of mixed with an aldehyde in acid, the volume of distilled water and the preparation of a fluorescent solution, it was found that the ratios of volumes are no more than 49: 1 and not less than 9: 1. In tab. Figure 7 shows the dependence of the relative fluorescence intensity on the dilution with water of the sample being analyzed.

Table

Claims (2)

Volume Ratio (Water: Acid) Formula of the Invention The method of quantitative determination of 1,2,5-trimethyl-4-propionyl-hydroxy-4-phenylpiperidine hydrochloride, characterized in that, the sample being analyzed is treated with a solution of formaldehyde in sulfuric acid, followed by adding to the resulting solution of water and fluorimetry the resulting solution. Sources of information taken into account during the examination 1. Instructive and methodical instructions. Issue 1. M., 1976, p. 45. 2. State pharmacology of the USSR. 10th ed. M., 1968, p. 563 (prototype).