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@article{207182,
        author = {Anil Jagannath Pawar and Babla Vinayak Pendam},
        title = {Evaluation of N-Nitrosodibutylamine a Genotoxic Impurity in Labetalol Drug Substance by GC-MS Technique},
        journal = {International Journal of Innovative Research in Technology},
        year = {2026},
        volume = {13},
        number = {2},
        pages = {4507-4520},
        issn = {2349-6002},
        url = {https://ijirt.org/article?manuscript=207182},
        abstract = {During the analysis of the pharmaceutical drug Labetalol, an unidentified impurity was detected in the final active pharmaceutical ingredient (API). The impurity was suspected to originate from the presence of a secondary amine or from intermediates formed during different stages of the synthetic process used for Labetalol production. The unknown impurity was successfully isolated and comprehensively characterized using advanced analytical techniques, including Fourier Transform Infrared Spectroscopy (FTIR), Nuclear Magnetic Resonance (NMR), Liquid Chromatography–Mass Spectrometry (LC–MS), and Gas Chromatography (GC). Structural characterization confirmed the impurity as N-Nitrosodibutylamine (NDBA). Consequently, a sensitive, reliable, and accurate Gas Chromatography–Mass Spectrometry (GC–MS) method employing Electron Ionization (EI) and Flame Ionization Detection (FID) was developed and validated for the quantitative determination of NDBA in Labetalol bulk drug. NDBA, with a molecular mass of 159 Da, generated characteristic fragment ions at m/z 99, 84, and 56 during EI fragmentation. The ion at m/z 56 exhibited the highest response and was selected as the quantifier ion, while m/z 84 served as the qualifier ion. Chromatographic separation was achieved using an HI-225-MS capillary column (30 m × 0.32 mm × 3 µm) with argon as the carrier gas, an injector temperature of 220 °C, and a programmed oven temperature profile. The method demonstrated excellent resolution, LOD and LOQ values of 0.0012 and 0.0024 ppm, respectively, recoveries ranging from 93.71% to 113.72%, and was successfully validated according to ICH guidelines for specificity, precision, linearity, accuracy, ruggedness, LOD, and LOQ.},
        keywords = {Limit of Detection (LOD), Limit of Quantitation (LOQ), Precision, Linearity, Accuracy and Ruggedness.},
        month = {July},
        }