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Development, evaluation of critical method variables and stability assessment using a Box-Behnken design for the determination of organic impurities in a pharmaceutical dosage form of a centrally acting muscle relaxant drug chlorzoxazone.

Santhosh Kumar EttaboinaSatyasree NannapaneniNagalakshmi JeedimallaThirupathi DongalaSiva Krishna MuchakayalaNaresh Kumar Katari
Published in: Biomedical chromatography : BMC (2024)
This study validates a stability-indicating LC method for detecting organic impurities in the chlorzoxazone dosage form. Using a Waters X-Select R HSS T3 analytical column, mobile phase of it was made by mixing of water, methanol, and glacial acetic acid in the ratio of 700:300:10 (v/v/v). The drug product and drug substance were subjected to the stress conditions such as acid, base, oxidation, heat, and photolysis as per the recommendations of the International Conference on Harmonization (Q2) methodology. The study revealed the susceptibility of 4-chloro-2-aminophenol to alkaline environments, emphasizing peak homogeneity and stability. The method verification, per ICH guidelines and USP<1225>, established precision, specificity, linearity, accuracy, and robustness for quality control. The mean impurity recovery ranged from 95.5% to 105.2%, the correlation coefficient (r) was greater than 1.000, and the RSD values (n = 6) ranged from 0.6% to 5.1% across the LOQ-150% ranges. Full-factorial design tested final method conditions, evaluating multiple parameters concurrently. Graphical optimization within the design space defined strong method requirements, ensuring consistent and reliable outcomes. The study develops and validates chlorzoxazone stability-indicating methods, employing advanced statistical approaches like design of experiments and factorial design, with resilient conditions established through graphical optimization of the design space.
Keyphrases
  • quality control
  • skeletal muscle
  • clinical practice
  • magnetic resonance imaging
  • mass spectrometry
  • liquid chromatography
  • solid phase extraction
  • functional connectivity
  • molecularly imprinted
  • stress induced