الرئيسية / الفعاليات العلمية / ابحاث / New approach for determination of sulfadiazine in pharmaceutical preparations using 4(4-sulphophenylazo)pyrogallol: Kinetic spectrophotometric method

New approach for determination of sulfadiazine in pharmaceutical preparations using 4(4-sulphophenylazo)pyrogallol: Kinetic spectrophotometric method

Naser A. Naser a,, Kasim M. Alasedi b, Zainab A. Khan c
a Department of Chemistry, Faculty of Science, University of Kufa, P.O. Box(21), Najaf Governorate, Iraq
b AL-Sheik al-tousi, University College, An-najaf al-ashraf, P.O. Box(9), Iraq
c Department of Chemistry, Faculty of Education for Girls, University of Kufa, P.O. Box(21), Najaf Governorate, Iraq
Abctract
A new trend describes the development and validation of a simple, sensitive and selective kinetic spectrophotometric methods for the determination of sulfadiazine in pharmaceutical formulations has been conducted. In this
paper, sulfadiazine was derivatized as a new organic compound 4(4-sulphophenylazo) pyrogallol, 4-SPAP, by
coupling pyrogallol with diazotized sulfadiazine in medium of controlled pH. 4-SPAP was characterized by techniques of FT-IR, H-NMR, GC-Mass, TG and DSC thermal analysis methods. Solvatochromic behavior in solvents of
various polarities was also investigated.
The determination of sulfadiazine was accomplished by initial rate and
fixed time methods. These methods were
based on the reaction of the compound containing sulfadiazine, 4-SPAP, with Ca(II) to form colored product with
a maximum absorbance at 520 nm. The two methods were adopted for constructing the calibration curves and
examined for their suitability for the quantitation of sulfadiazine in pharmaceuticals. The limit of detection
(LOD) and limit of quanti
fication (LOQ) were found to be, by initial rate method, 0.35 and 1.05 μg·mL1and
that by
fixed time method were found to be 0.69 and 2.07 μg·mL1, respectively. The percent relative standard
deviations (%RSD) for the results ranged from 1.04% to 1.76% and 0.85% to 1.42% for the initial rate and
fixed time
methods of the proposed kinetic spectrophotometric method, respectively. The existence of common excipients
in the pharmaceutical formulation did not produce any signi
ficant interference. Statistical comparison was reported as indicated from the F- and t-test data of the proposed methods with that of reference method showing
excellent agreement and indicating no signi
ficant difference in their accuracy and precision.
© 2018 Elsevier B.V. All rights reserved

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