Development of a procedure for the determination of magnesium and calcium in pharmaceutical preparations by atomic absorption spectrometry (AAS)

Tóm tắt

   Objective: To establish and validate an F-AAS procedure for the simultaneous quantification of Mg and Ca in oral solutions.
   Subjects and Methods: An oral solution containing calcium glycerophosphate and magnesium gluconate was used. Sample treatment (mineralization) was optimized using Response Surface Methodology (RSM) with a Box-Behnken Design (BBD), surveying HNO₃ concentration (1–3 M), digestion time (10–30 min), and temperature (50–70°C) for maximum recovery Method validation was performed in accordance with the ICH Q2 (R1) guidelines and Ministry of Health standards.
   Results: Optimal sample treatment conditions were 1.7 M HNO₃, 11 minutes, and 54°C. F-AAS showed high specificity and was unaffected by excipients. The linearity range had r ≥ 0.998. Accuracy (recovery) was 99.64%–103.76% for Mg and 97.04%–106.22% for Ca. Precision (RSD) was ≤ 2%. F-AAS demonstrated higher precision and fewer errors than complexometric titration.
   Conclusion: This study successfully established a high-precision F-AAS protocol for the simultaneous quantification of Ca and Mg in complex oral solutions. The primary novelty lies in the application of a Box-Behnken Design (BBD) to rigorously optimize the wet digestion process, ensuring total analyte release from organic matrices with minimal acid consumption and time. By addressing the specific challenges of complex organic matrices and simultaneous determination, this method provides a superior and more efficient alternative to traditional pharmaceutical analysis, significantly enhancing quality control standards for such liquid formulations.

DOI: 10.59715/pntjmp.5.2.13