The formation of various sulfonate esters is unavoidable during the synthesis of teneligliptin (TEN), an important drug of type 2 diabetes mellitus. They are essentially to be eliminated from the drug due to their potential genotoxic nature, but there are no effective methods in practice. Hence, we developed an efficient method to get rid of those genotoxic impurities from the drug. The successfully developed method was validated for the trace-level analysis of methyl 1-octanesulfonate (MOS), ethyl 1-octanesulfonate (EOS), and butyl 1-octanesulfonate (BOS) in TEN by gas chromatography-mass spectrometry, in terms of detection limit (LOD), quantification limit (LOQ), precision, accuracy, linearity, robustness, and specificity. The LOD and LOQ values are 0.74, 0.68, and 0.61 ppm and 2.48, 2.25, and 2.03 ppm, respectively, for MOS, EOS, and BOS. The approach was linear in the LOQ of 56 ppm with the correlation coefficient of 0.9979 and above. The average %recovery of residual sulfonate esters from the drug was 94.5 (MOS), 97.5 (EOS), and 97.2 (BOS). The developed method is suitable for even trace-level quantification of MOS, EOS, and BOS content in TEN.
It is clear from the literature that there are only a few methods reported with limitations of sophisticated instruments and poor sensitivity for the assay of Brivaracetam, and, particularly, no report on the simultaneous determination of the assay of Brivaracetam and its enantiomers (En) and diastereomers (DS) in a single method. Hence, it was our goal to build on a robust high-performance liquid chromatography (HPLC) process to the simultaneous assessment of Brivaracetam, and its En and DS, from the Brivaracetam drug. Accordingly, the reverse-phase chiral HPLC method development was established in a constructive way, such as buffer selection, column selection, mobile phase composition, organic modifier compositions, and column temperature variation. As a consequence, the simultaneous assessments were achieved in Daicel CHIRALPAK IG-3 (250 mm x 4.6 mm x 3 µm) with reverse-phase setup conditions consisting of 10 mM (NH 4 )HCO 3 buffer: CH 3 CN (1:1) %v/v in an isocratic elution. High sensitivity was obtained for Brivaracetam and its stereoisomers at Limit of quantitation (LOQ) 0.25 µg/ml and Limit of detection (LOD) 0.08 µg/ml. This method is systematically validated by the International Council for Harmonization procedures. Thus, the method is applicable in quality control, in drug analysis, and in the investigation of counterfeit drugs as well.
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