Simultaneous analysis of daclatasvir with its three organic impurities: Application in stability studies, pharmaceuticals and serum samples

Publication date: June 2019Source: Microchemical Journal, Volume 147Author(s): Asia Naz, Nawab Sher, Farhan Ahmed Siddiqui, Muhammad Kashif, Aurangzeb AnsariAbstractThis work describes quantification of daclatasvir in simultaneous with its three impurities. The chromatography was developed using gradient elution, where mobile phase A is composed of mixture of acetonitrile and phosphate buffer while mobile phase B is pure acetonitrile. Impurities were resolved on a C18 analytical column (4.6 × 100 mm, 5 μm) and quantified after detection at 304 nm. After successful systematic development of chromatographic method, a comprehensive validation study was conducted. Linearity was conducted in the range of 50–50,000 ng/mL for daclatasvir and 25–25,000 ng/mL for the three impurities and in all the cases the correlation coefficient was greater than 0.995. Accuracy for daclatasvir in serum samples was 97–103% with 0.5–2.5% precision, while for related substances the absolute accuracy was 94.2% minimum with 5.6% precision maximum. Statistical analysis was conducted which proved that the newly developed method was highly precise, accurate and specific for the quantitative analysis of Daclatasvir and its three main impurities. The projected method resolves and separates daclatasvir peak from impurities, therefore, the proposed method possesses stability indicating properties and is well applied in stress testing of daclatasvir.
Source: Microchemical Journal - Category: Chemistry Source Type: research