Determination Of Genotoxic Impurity Methyl P-Toluene Sulfonate in Pharmaceutical Drug by Chromatographic Technique
Keywords:
Genotoxic Impurities, Methyl p-Toluene Sulfonate, Doxofylline, GC-MS, Method Validation, Limit of Detection (LOD), Limit of Quantification (LOQ), Recovery Precision, Pharmaceutical SafetyAbstract
The determination of genotoxic impurities (GIs) in pharmaceutical drug is critical to ensure drug safety and compliance with regulatory standards. It has identified and quantified GIs in Methyl p-Toluene Sulfonate and Doxofylline with use of Gas Chromatography-Mass Spectrometry (GC-MS). The method was developed and validated in accordance with ICH guidelines focusing on specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). It has analysed GC-MS analysis was performed using a DB-5 capillary column, with an electron ionization source and selective ion monitoring (SIM) mode to ensure high sensitivity for trace-level detection. The developed method demonstrated excellent specificity with well-resolved chromatographic peaks and minimal interference from the drug matrix. It has added on calibration curves for both drugs showed good linearity (R2>0.999) over a concentration range of 0.1 ppm to 10 ppm. The accuracy was confirmed by recovery studies with yield results within the acceptable range of 95-105%. The precision studies revealed that intra-day and inter-day relative standard deviations (RSD) below 2% and 3% respectively. The LOD and LOQ for methyl p-toluene sulfonate were 0.05 ppm and 0.1 ppm respectively while for Doxofylline have 0.07 ppm and 0.15 ppm. The method showcases the robustness under slight variation with analytical conditions. It can be concluded that the routine monitoring of genotoxic impurities in pharmaceutical formulations ensuring compliance with regulatory safety limits and contribution to the safety and efficacy of pharmaceutical products.
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