Objetivos: Los estudios cinéticos de substancia y medicamento Famotidina (FMT) han sido realizados en las soluciones amortiguadoras en las condiciones de reacción del segundo orden a temperatura de 293 K. Nuevos métodos titrimétricos están descritos para determinar FMT. Materiales y métodos: La substancia y los comprimidos FMT han sido usados en la reacción analítica con KHSO5. El comportamiento cinético ha sido estudiado por el método de yodometría en diferentes ambientes de pH. Resultados: La reacción de oxidación de FMT se estudiaba para el producto del óxido S con pH = 2,0-5,0 y de la sulfona con pH = 7,0-8,4. La reacción a estudiar corresponde al segundo orden general. Las constantes de velocidad de la reacción de la formación de sulfona del óxido S FMT se encuentra en el intervalo de 14,49 a 32 l mol-1 min-1. La FMT fue determinada mediante la medición del exceso de solución estándar del caroata de potasio en la solución amortiguadora con pH 7 dentro de 20 minutos desde el inicio de la reacción, luego el oxidante restante fue determinado por el método de titulación yodométrica. El método titrimétrico se aplica en el diapasón de 1-10 mg, la reacción corresponde a la estequiometría 1: 2 (FMT: KHSO5). El método ha sido validado a la precisión, reproducción, linealidad, robustez y LOQ. El contenido del principio activo es del 99,2 al 100,5%, RSD del 1,09 al 1,70%, LOQ = 0,03 mg / ml para substancia. RSD para comprimidos se encuentra dentro del 1,17 al 2,87%. Conclusión: Han sido optimizadas las condiciones de formación del óxido S de FMT y sulfona. Los métodos elaborados son rápidos, sencillos y baratos y podrán aplicarse para determinar el fármaco de preparación farmacética.
Objective: The electrochemical behavior of peracetic acid (PAA) in disinfectant "Delakson" has been studied. Materials and Methods: "Delakson" disinfectant is a sample preparation, which was used for the analysis. A new voltammetric method for the quantitative determination of PAA in "Delakson" disinfectant at the carbositall rotating electrode (CE) in the interval of potential +1.0…-1.0 V (the reference electrode Ag, AgCl/KСl [sat]) (E p = +0.15 V) was proposed. Results: It has been experimentally proved that height of PAA reduction peak decreases and the reduction peak potential is shifted toward more electronegative values with the background electrolyte pH increasing from 2.15 to 4.78. The optimum pH for analysis is approximately 3.6. The linear relationship has been observed in the PAA concentration range 3.12-12.50 × 10-5 mol/L, the calibration curve equation was I р = (3.78 ± 0.46) × 10 3 с (r = 0.995). Determining PAA in the work solution with the relative standard deviation (RSDs) were 0.035-0.022 (δ = +0.30... +0.90%); limit of detection = 1.19 × 10-6 mol/L, and limit of quantification = 3.97 × 10-5 mol/L. Determining PAA in the test solution of "Delakson" disinfectant with the concentrations of 0.1% the RSD was 0.024 (δ = +0.9%). Conclusions: Thus, new voltammetric method of PAA determination in "Delakson" disinfectant at CE has been developed and the possibility of its quantitative determination has been shown.
The search for new analytical reactions and finding out the optimal conditions for their course, which can be used as the basis for quantitative analytical determinations of penicillins, is a very urgent task.Aim. To develop methods for the quantitative determination of Oxacillin.Materials and methods. The study object was Oxacillin sodium salt powder in vials for preparing a solution for injections(0.5 g). Peroxomonosulfate acid as triple potassium salt 2КНSO5∙КНSO4∙K2SO4 (Oxone®) of “extra pure” grade was used as an oxidant. The methods of kinetic spectriphotometry and redox titration were used.Results and discussion. A simple procedure for the quantitative determination of the Oxacillin pure substance by the kinetic spectrophotometry and redox titration methods using potassium hydrogen peroxomonosulfate (KHSO5) has been developed. The results of the drug analysis obtained by newly developed and current methods are in good agreement with each other; δ (correctness) = (0.45 – 0.86) %.Conclusions. Using the methods of kinetic spectrophotometric and redox titration, two independent procedures for thequantitative determination of oxacillin in the substance and the drug product have been developed using potassium hydrogen peroxomonosulfate as an analytical reagent (KHSO5). A relative standard deviation RSD = (1.24 – 2.17) %.
Objective: Kinetics and stoichiometry S-oxidation reaction of sodium Azlocillin (Azl) by means of potassium hydrogenperoxomonosulfate in aqueous solutions using iodometric titration were studied. Materials and Methods: Securopen ®-powder Azl sodium in flacons for preparation of solution for injections (Azl 1.0 g; 5.0 g) was used for analysis. A new iodometric method for quantitative determination of sodium Azl in Securopen ® preparation using potassium hydrogenperoxomonosulfate (KHSO 5) as analytical reagent was proposed. Peroxomonosulfate acid as triple potassium salt 2КНSO 5 •КНSO 4 •K 2 SO 4 (Oxone ®) of "extra pure" qualification was used as oxidant. Results: At pH 2-4 for 1 mole of penicillin, 1 mole of KHSO 5 is consumed; the quantitative interaction is achieved within a time of more than 1 minute (observation time). The results were obtained by the recommended procedure for seven replicate titrations of mixtures containing the three species at various concentrations. Relative standard deviation = (0.8 −2.8) %, δ = (+0.2 …−0.31) %. It can be seen that Azl can be determined successively with good accuracy and reproducibility. Conclusion: The new procedure was developed and ability of quantitative determination of penicillin in pharmaceutical preparation Securopen ® by iodometric method using potassium hydrogenperoxomonosulfate (KHSO 5) as analytical reagent was shown.
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