Determination of methanesulfonates impurities in pefloxacin mesilate by GC-MS method
Pages: 521-525
Year: 2017 Issue: 6
Journal: Chinese Journal of Antibiotics
Abstract: Objective To establish the determination method for methyl methanesulfonate (MMS),ethyl methanesulfonate (EMS) and isopropyl methanesulfonate (IMS) in pefloxacin mesilate by GC-MS.Methods The three kinds of methanesulfonates were derived to methyl iodide (MeI),ethyl iodide (EtI) and isopropyl iodide (iPrI) by the iodonation agent as pre-column derivation,DB-WAX (30m×0.25mm,0.25μm) capillary column was used to separate and mass spectrometer for quantitative decermination.Results The calibration curves for MMS,EMS and IMS were good linear in the ranges of 34～549,31～499 and 26～411ng/mL,respectively (r≥0.999).The average recoveries were 101.8％,102.9％ and 100.6％.Quantitative limits were not below 2.6ng/mL.Conclusion The method is simple,accurate and rapid,and it's suitable for the determination of the genotoxic impurities in pefloxacin mesilate.
Year: 2017 Issue: 6
Journal: Chinese Journal of Antibiotics
Abstract: Objective To establish the determination method for methyl methanesulfonate (MMS),ethyl methanesulfonate (EMS) and isopropyl methanesulfonate (IMS) in pefloxacin mesilate by GC-MS.Methods The three kinds of methanesulfonates were derived to methyl iodide (MeI),ethyl iodide (EtI) and isopropyl iodide (iPrI) by the iodonation agent as pre-column derivation,DB-WAX (30m×0.25mm,0.25μm) capillary column was used to separate and mass spectrometer for quantitative decermination.Results The calibration curves for MMS,EMS and IMS were good linear in the ranges of 34～549,31～499 and 26～411ng/mL,respectively (r≥0.999).The average recoveries were 101.8％,102.9％ and 100.6％.Quantitative limits were not below 2.6ng/mL.Conclusion The method is simple,accurate and rapid,and it's suitable for the determination of the genotoxic impurities in pefloxacin mesilate.
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