| Popis: |
Abstract Background This study reports a new, cost-effective and validated method for the determination of ceftriaxone (CFR). The method involved charge transfer (CT) complexation reaction of ceftriaxone (as n-electron donor) and N-(2,4-dinitro-1-naphthyl)-p-toluenesulphonamide {N-(2,4-DN1NL) PTS} as π-electron acceptor to form a complex. Ultraviolet, infrared and 1H NMR spectra of CFR, N-(2,4-DN1NL) PTS and adduct were then studied to predict the site of interaction between the donor and acceptor. Result The complex formed had deep golden-yellow colour, having a new absorption band at 440 nm. Molar absorptivity of 1.667 × 105 L M−1 cm−1 was obtained. The complexation reaction was completed at 30 °C optimal temperature within 10 min. Acetonitrile was found to be the best diluting solvent for optimal detector response and the complex was stable (absorbance unchanged) at room temperature for hours. At concentration of 1.708–11.956 µg mL−1, with low limits of detection of 0.143 µg mL−1, Beer’s law was observed. Between-day recovery statistics of CFR from quality control samples were 102.15 ± 0.062 (% RSD = 0.61, n = 12) over three days. The site of interaction of donor and acceptor molecules, as revealed through infrared (IR) and proton nuclear magnetic resonance studies (1H NMR) and the formation of charge transfer complex is through intermolecular hydrogen bonding between the amino group of the donor and the acidic proton of the acceptor. Common tablet excipients, as observed, did not interfere with the analytical method and no significant difference existed between the results of this new method and the high performance liquid chromatographic procedures (p > 0.05) documented in the USP. The new CT procedure described in this paper is not only simple but also fast, accurate and precise. Also, the reactions were carried out at room temperature compared to previously described procedures. Conclusions This novel method could therefore be adopted as a fast but cost-effective alternative for the qualitative and quantitative assessment of CFR in its pure and dosage form. It could find usefulness in on-the-spot detection of counterfeit drugs and in field inspections with reliable accurate results that compares with established methods. |
