Drug Impurities may be formed in low concentrations during API manufacturing, formulation, and stability studies. Impurities can originate from degradation, residual intermediates used during synthesis, packaging leachable, unknown contamination, and unwanted by products of reactions. As per ICH Q3A (R2)* guidelines, it is required that impurities are isolated and identified. If the estimation indicates that the given impurity content is greater than 0.1%, it must be identified and characterized according to all regulatory requirements. Axios is fully equipped to support our client in this endeavor. Axios specializes in isolation, structure elucidation and characterization of the unknown impurities. The impurities are isolated using prep HPLC/SFC and then complete structure is elucidated by 2D_NMR, HRMS and IR. In addition, our team has vast experience in chiral separations.
The US Pharmacopeia (USP) defines reference-standard materials as "highly characterized specimens of drug substances, excipients, reportable impurities, degradation products, compendial reagents, and performance calibrators". The appropriate characterization of a reference standard is very important because quality and purity of reference standards are critical for reaching scientifically valid results. The key requirements for a reference standard are:
a) Unambiguous confirmation of the structure.
b) Accurate determination of the purity of the standards.
c) Accurate reporting of “Purity as is basis” or potency.
Each reference standard supplied by Axios undergoes rigorous analysis using NMR (2D-NMR if needed) and Mass spectral analysis (HRMS if required) and IR to confirm the structure and the HPLC analysis and TGA analysis to ascertain the purity and potency. Wherever needed, moisture content by KF is ascertained. Salt forms undergo ICPMS to quantify the counter ion. Characterization protocol of Axios Reference standards is above and beyond the current industry standard.