SU717631A1 - Method of quantitative determining of sodium para-aminosalicylate - Google Patents

Description

METHOD OF QUANTITATIVE DETERMINATION

(54) SODIUM PARAAMINOSALICILATE

The invention relates to analytical chemistry, in particular to a method for the determination of sodium para-amino salicylate, and can be used in the analysis of medicinal products in laboratories of pharmacy departments and pharmaceutical pharmaceutical plants, as well as in biochemical laboratories of the public health system and chemical and chemical research. x The known method for the quantitative determination of sodium para-n-bsalicylate by treating a sample of the analyte with concentrated sulfuric acid followed by measuring the fluorescence intensity of the solution obtained 1. The disadvantages of the method are its unequality and low sensitivity. This method allows detection at a concentration of 50 µg / ml on average only 75% of the drug in the urine and 71.5% c. , blood even in artificial mixtures. The goal of the inventor is to increase the selectivity and chupspitol1, post the method. The goal is achieved by the method in which a sample of an analyte is treated with an inorganic Membolr 1 and 1 Yum B after dosing the fluorescence intensity of the resulting solution as an inorganic reagent, chloride and aluminum are processed in an acidic medium in the presence of butyl alcohol. . The concomitant ingredients found in the dosage forms do not interfere with the direct determination. The linear relationship between the fluorescence intensity of the resulting complex compound and the concentration of the para-amino saline / sodium pat is from 0.01 To. 5O µg / ml. The content of sodium para-aminosalicylate, starting with 0.1 µg / ml, is determined by the full (100%) content of biologic samples (urine and blood). Example 1. Quantitative determination of sodium para-amino salicylate in dosage forms. Accurate weighed portion (0.05 g, 0.1 g or 1-2 ml) of the samples under study transfer to a 100 ml volumetric flask, add 50-60 ml of ethyl alcohol and shake vigorously for 3-5 minutes, topping up with alcohol to the mark and mix (solution A). An aliquot portion of solution A is transferred to a volumetric flask to obtain a solution with a content not exceeding 200 µg / ml (solution B). To 1 ml of solution B, 1 ml of a 1% solution of aluminum chloride, 8 ml of butyl alcohol, 3 drops of 2.tt, an alcoholic solution of hydrochloric acid are added and the fluorescence intensity of the resulting solution is measured. The content is calculated according to the calibration schedule, for which O, 1 is measured in a series of tubes; 0.5; 1.0; 1.5; 2 ml of a standard solution in ethyl alcohol with a content of 100 µg / ml, 1 ml of 1% aqueous solution of aluminum chloride is added, all solutions are made up to 1 O ml with butanol, 3 drops of 2N are added, and an alcoholic solution of hydrochloric acid is added. acid. Fluorimeter simultaneously with U solutions of the investigated samples. Based on the results of these measurements, a calibration chart is made. The results of the fluorimetric determination of para-aminosalicylate sodium in Pasomycin are given below (the weight of the powder is 0.9194). The para-aminosalicylate was found by calibration based on 1 schedule, µg powder 9,1500 0,4600 10,0000. 0.50OO 11.0640 0.5532 0.3723 7.4469 8.7234 0.4361 0.4468 8.9361 6.1702 O, ZO85 7.8723 0.3936 0.4150 8, ZOOO Metrological characteristics X 0, 4317 + 0.0714 Е 0.95 ± О, О547 and 0.43Г7 ± 0.0547 Below are the results of fluorometric determination of sodium para-aminosalicylate in a 3% injection solution, Found by sodium vapor-palysalicylate by calibration solution, graph, µg 10, 43470.0344 9.78260.0322 10.21370.0337 9.56520.0315 10.03470.0331 9.13040.033 Metrological characteristics X 0.0325 tf + 0, ОО19V Ео, ± 0.0019 and 0.0325 ± 0.0019 Example 2, Determination of sodium para-amino salicylate in blood, 0.1 ml of blood is diluted to 1 ml with ethyl alcohol, good The mixture is stirred, centrifuged for 3–4 minutes at 3000 rpm, 1 ml of 1% alcohol solution of aluminum chloride, 8 ml of butyl alcohol and 3 drops of 2 N solution of hydrochloric acid are added to 1 ml of centrifugate. The fluorescence intensity is measured. The content is calculated according to a calibration graph, for which 0.1 is measured in a series of tubes; 0.5; 1, O; 2.0; 3.0; 4.0 ml of a standard solution containing 25 µg / ml in ethanol, 1 ml of 1% solution of aluminum chloride is added, the volume of all tubes is reduced to 1 O ml with butyl alcohol, 3 drops of 2I are added. solution of hydrochloric acid, fluorimetricate simultaneously with the solutions of the samples. Example 3: Determination of sodium para-amino salicylate in urine, 1 ml of urine is diluted to 1 O ml with ethyl alcohol, centrifuged for 3–4 minutes at 30,000 rpm, 1 ml of 1% aluminum chloride in ethyl solution is added to 1 ml of this solution. alcohol, 8 ml of butyl alcohol and 3 drops 2 and. alcoholic hydrochloric acid solution measure the fluorescence intensity. The PAS content is calculated according to a calibration graph, for which 0.1 is measured in a series of tubes; 0.5; 1.0; 2.0; 3, O; 4.0 ml of a standard solution in ethyl alcohol with a content of 25 µg / ml, 1 ml of 1% solution of aluminum chloride is added, the volume of all tubes is brought to 10 ml with butyl alcohol, 3 drops of 2i are added, and acids, fluoridate simultaneously3, 457 3.063 0.856 0.210 O, 114 0.061 0.045 0, O35 7.844 44.6 48.5 47.7 40.2

d ± 0.774

0 7,844 i 0,815

When studying the optimal conditions of pro-j40.0 µg / ml, linear from 0.01 to

maintaining a fluorescent reaction on the par., 0 µg / ml. sodium aminosalidylate found that.

direct dependence of the fluorescence intensity - Dependence of the fluorescence intensity on the concentration of para-amino 25 25% from the concentration of para-aminosalicylate

sodium lyzpatat is from 0.01. archives are given in table. one,

The sensitivity of the reaction is quite high (o, 01 µg / ml), which makes it possible to determine the drug in dosage forms (0.01 µg / ml) and biological fluids (0.1 µg / ml) without separation from related components.

The determinations were carried out on an EF-ZMA electron fluorometer.

Concentration of Al71763 chloride solution 5

Table 1

the mini used to process the sample being analyzed ranges from OjOOOOOl to 0.1 g / ml. The optimal values of this range are from 0.01 to 0, 03 g / ml.

Below is the dependence of the fluorescence intensity on the concentration of aluminum chloride 1 but with solutions of the samples under study. The results of the determination are presented. The results of fluorimetric determination of sodium para-amino salicylate in the blood and urine with the appointment of 9.0 g in the form of tablets (5. out of 10 patients) are given below.

review 92 100

The composition of the intracomplex compound of sodium para-aminosalicylate with aluminum chloride by isomolar series

4i: J-j6S 2: -

The composition of the obtained intracomplex compound was studied by the method of iso-molar series (see tab. 2).

T and b and U and

717631

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Claims (1)

1. Senov P.L., Pavlyuchenkova L.P. Fluorimetric determination of sodium para-amino esaliaet. Pharmacy, 1973, No. 5, p. 32-34 (prototype).