Author(s): Manikanth Reddy Yarala, Sowjanya Gummadi

Email(s): statinen@gitam.edu

DOI: 10.52711/0974-360X.2024.00296   

Address: Manikanth Reddy Yarala, Sowjanya Gummadi*
Department of Pharmaceutical Analysis, GITAM School of Pharmacy,
GITAM (Deemed to be University), Visakhapatnam-530045, Andhra Pradesh.
*Corresponding Author

Published In:   Volume - 17,      Issue - 4,     Year - 2024


ABSTRACT:
This study presents a novel, sensitive and highly reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) methodology for the determination of N-Nitroso Safinamide, a genotoxic impurity in Safinamide mesylate. The optimized chromatographic conditions utilized Poroshell HPH-C18 (150 x 4.6 mm, 2.7 µm) and Ghost Buster columns with a flow rate of 0.8 ml/min and a column temperature of 40 °C. The mobile phase consisted of formic acid and methanol. Mass spectrophotometric analysis employed the Agilent Jet Stream Electrospray Ionization (AJS ESI) mode with a capillary voltage of 3500 V and a nitrogen gas flow rate of 12 L/min at 350 °C, while Multiple Reaction Monitoring (MRM) mode was used for scanning. Rigorous validation demonstrated the method's reliability and robustness. Linearity experiments showed a strong correlation coefficient of 0.999 between analyte concentration and peak area response. The method exhibited low limits of detection (LOD) and quantification (LOQ) of 0.00593 ppm and 0.01797 ppm, respectively, enabling accurate detection and quantification of N-Nitroso Safinamide at low concentrations. Precision studies demonstrated good repeatability and reproducibility, with % RSD values falling within acceptable limits. Specificity evaluations confirmed the absence of interferences in blank, standard, sample, and spiked sample solutions. The method's accuracy was established through satisfactory recovery values, ranging between 70 % and 130 % in spiked samples. The developed LC-MS/MS methodology offers a highly reliable and precise approach for quantifying N-Nitroso Safinamide in Safinamide mesylate.


Cite this article:
Manikanth Reddy Yarala, Sowjanya Gummadi. Trace level Quantification of N-Nitroso Safinamide: A Genotoxic Impurity in Safinamide Mesylate Using ESI-MS/MS. Research Journal of Pharmacy and Technology.2024; 17(4):1867-3. doi: 10.52711/0974-360X.2024.00296

Cite(Electronic):
Manikanth Reddy Yarala, Sowjanya Gummadi. Trace level Quantification of N-Nitroso Safinamide: A Genotoxic Impurity in Safinamide Mesylate Using ESI-MS/MS. Research Journal of Pharmacy and Technology.2024; 17(4):1867-3. doi: 10.52711/0974-360X.2024.00296   Available on: https://rjptonline.org/AbstractView.aspx?PID=2024-17-4-70


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Available from: http://www.oecd.org/officialdocuments/publicdisplaydocumentpdf/?cote=env/jm/mono

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