Structural Identification and Characterization of Potential Impurities of Azelnidipine

Author(s)

Kapavarapu, S., Bhandaru, V.R., Chintala, R.

Author's Affiliation

Abstract

Azelnidipine (AZL) is a pale yellowish white tablet (16mg) with diameter of 9.2mm and thickness of 3.3mm. A reverse phase performance liquid chromatographic method was developed for the determination of AZL in bulk and pharmaceutical dosage form.  During the synthesis of bulk drug of AZL, we observed four impurities. All the impurities were detected by a gradient high performance liquid chromatographic (HPLC) method. LC-MS was performed to identify the mass number of these impurities. A thorough study was carried out to characterize the impurities. These impurities were synthesized, characterized and were co-injected with the sample containing impurities and are found to be matching with the impurities present in the sample. Based on the complete spectral analysis (UV, IR, NMR and MS) these impurities were characterized as 1) Azelnidipine Stage-I para impurity [Impurity 1], whose molecular formula is C₁₄H₁₅NO₅ and molecular weight is 277.27, 2) Azelnidipine Intermediate [Impurity 2], whose molecular formula is C₁₄H₁₅NO₅ and molecular weight is 277.27, 3) 4-Nitro Azelnidipine [Impurity 3], whose molecular formula is C₃₃H₃₄N₄O₆ and molecular weight is 582.65 and, 4) 2-Nitro Azelnidipine [Impurity 4], whose molecular formula is C₃₃H₃₄N₄O₆ and molecular weight is 582.65. The proposed method was validated as per International Conference on Harmonization (ICH) guidelines. The method was accurate, precise, specific and rapid found to be suitable for the quantitative analysis of the drug and dosage form.

Keywords

Azelnidipine, Impurity Profiling, Impurities, Identification, IR, UV, NMR, MS, Isolation, Characterization

Cite This Article

Kapavarapu, S., Bhandaru, V.R., Chintala, R. (2016). Structural Identification and Characterization of Potential Impurities of Azelnidipine, International Journal for Pharmaceutical Research Scholars (IJPRS), 5(2), 202-217.