Add time:08/28/2019         Source:sciencedirect.com

A novel and sensitive derivatization procedure for the determination of 2-cynaoacetamide in pharmaceutical samples using liquid chromatography with the fluorescence detection was discovered. The method is based on derivatization of 2-cynaoacetamide using 2-hydroxyacetophenone as a new derivatization reagent. The product of derivatization reaction was isolated and characterized using spectroscopic techniques namely LC–MS, NMR and IR. The structure of 2-cyanoacetamide derivative was unambiguously assigned as a 2-amino-4-phenylfuran-3-carboxamide.Two derivatization systems were optimized in terms of reaction temperature, reaction time, pH and concentration of 2-hydroxyacetophenone, and a new pre- and post-derivatization HPLC methods were developed. The separations on HPLC with pre-column derivatization were accomplished using stationary phase based on a XBridge C18 column (100 × 4.6, 3.5 μm) and isocratic elution using the mobile phase acetonitrile – 0.1% formic acid (30:70, v/v). The separations on the HPLC with post-column derivatization were performed on stationary phase on a TSKgel Amide-80 column (150 × 4.6 mm, 3 μm). The mobile phase was a mixture of acetonitrile, methanol and 10 mM sodium formate buffer at pH = 4.5 in ratio 3:2:95 (v/v).Both HPLC methods were fully validated in terms of linearity, sensitivity (limit of detection and limit of quantification), accuracy and precision according to ICH guidelines. The pre-column derivatization method was linear in the range 1.1–2000 μg/l with method accuracy ≥ 98.2% and method precision RSD ≤ 4.8%. The post-column derivatization method was linear in the range 12–2000 μg/l. Method accuracy ≥ 96.3% and method precision RSD ≤ 3.5%. Proposed new methods were proved to be highly sensitive, simple and rapid, and were successfully applied to the determinations of 2-cynaoacetamide in pregabalin.

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