Development and validation of a microwave-assisted digestion technique as a rapid sample preparation method for the estimation of selenium in pharmaceutical dosage forms by ICP-OES

Document Type : Original Articles

Authors

GITAM Institute of Pharmacy GITAM (Deemed to be University) Gandhi Nagar, Rushikonda, Visakhapatnam-530 045 Andhra Pradesh, India

10.32592/ARI.2024.79.1.68

Abstract

Selenium is a class 2B element according to ICH Q3D guidelines. Selenium sulfide is an anti￾infective agent with antifungal and antibacterial properties used to treat dandruff and seborrheic
dermatitis. The literature survey revealed that most of the analytical techniques to estimate
selenium were found to be time-consuming and/or required high skill. The process involved
identifying the isotopes, selecting the measuring approach, and optimizing a typical
microwave-aided digesting procedure. To the samples, ammonium hydrogen difluoride, water,
and concentrated nitric acid were added. The confirmed microwave digestion program was a
two-step program where in the initial step, the samples were ramped at 200°C for 20 minutes
and held for 5 minutes. Later, samples were cooled and neutralized by boric acid, then ramped
for 20 minutes to a temperature of 180°C and held for 10 minutes. Selenium was estimated at
196.090 nm by ICP-OES. System suitability was run before initiating analysis to ensure that
system performance was consistent. Analytical validation parameters like the specificity of the
method were demonstrated at 196.090nm, linearity was proven from 10 ppm to 150 ppm of
selenium concentration, the detection limit was 1.28 ppm and the limit of quantification was
3.89 ppm. Robustness was confirmed for small changes to ICP-OES operating conditions. The
method's precision was demonstrated by analyzing the percentage relative standard deviation
for six injections was found to be less than 2.0%. Accuracy was confirmed from 10 ppm to 150
ppm, and all the samples were found to be within the range of 95-105%. A common
microwave-assisted digestion technique was developed and the same was validated. The
preciseness, specificity, linearity, accuracy, and robustness of the method for estimating
selenium in selenium sulfide drug substances and various pharmaceutical dosage forms were
demonstrated. This newly developed microwave-assisted digestion technique has optimum
sensitivity, highly reproducible and time saving than the existing methods. This method can be
applied to numerous matrices for a finished dosage of selenium sulfide formulations.

Keywords


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