ABSTRACT The study aimed to develop and validate a sensitive and robust LC‐MS/MS method for the quantification of N ‐nitroso‐desmethyl‐zolmitriptan in pharmaceutical samples, ensuring method specificity, accuracy, and regulatory compliance. Mass spectrometric parameters were optimized using an electrospray ionization (ESI) source in positive ion mode with multiple reaction monitoring (MRM). The precursor‐to‐product ion transitions were identified as Q1 m / z 303.10 with fragment ions at m / z 273.10, 230.0, and 144.0. Chromatographic separation was optimized using a Poroshell HPH C18 column (150 × 4.6 mm, 2.7 µm) with a mobile phase comprising 0.77 g of ammonium acetate in 1000 mL water with 0.3 mL formic acid (Mobile Phase A) and acetonitrile (Mobile Phase B). The method was validated in accordance with ICH guidelines, assessing system suitability, linearity, accuracy, precision, and sensitivity. System suitability parameters confirmed method consistency, with %RSD values of 1.0% for peak area and 1.9%–2.3% for bracketing standard injections. The method exhibited excellent linearity over a concentration range of 0.032–3.95 ppm with an R 2 value of 0.9975. Sensitivity assessment established the limit of detection (LOD) at 0.010 ppm and the limit of quantification (LOQ) at 0.032 ppm, with corresponding signal‐to‐noise ratios exceeding acceptance criteria. Accuracy studies demonstrated recovery rates of 92.4%–96.5% at the LOQ level and 96.1%–98.4% at 100% concentration. Precision at the LOQ level yielded a %RSD of 3.5%, confirming method reproducibility. The developed LC‐MS/MS method provides a reliable, specific, and sensitive approach for the quantification of N ‐nitroso‐desmethyl‐zolmitriptan in pharmaceutical matrices. The optimized chromatographic and mass spectrometric conditions ensured high recovery, precision, and linearity, making the method suitable for routine quality control and regulatory compliance in pharmaceutical analysis.
Patha et al. (Mon,) studied this question.