Determination of Sulfonate Genotoxic Impurity Residues in Celecoxib Based on Gas Chromatography-mass Spectrometry Method
A gas chromatography-mass spectrometry(GC-MS)method was developed for the determination of methyl celecoxib sulfonate and ethyl celecoxib sulfonate residues in celecoxib APIs and their formulations.The two impurities were derivatised into iodomethane and iodoethane by sodium iodide derivatisation with headspace injection,and separated on a DB-624 capillary col-umn(60 m×0.25 mm,1.4 μm),with helium as the carrier gas and detected by mass spectrometry detector.Both methyl celecox-ib sulfonate and ethyl celecoxib sulfonate showed good linearity in the concentration range of 10～500 ng·mL-1;the recoveries were in the range of 80.87%～106.52%with the RSDs less than 10%;and the limits of quantification(LOQs)were both 10 ng·mL-1.Methyl celecoxib sulfonate and ethyl celecoxib sulfonate impurities were not detected in any of the celecoxib samples.The meth-od is simple and accurate,which can be used for the detection of genotoxic impurities of two sulfonate esters,methyl celecoxib sulfonate and ethyl celecoxib sulfonate,in celecoxib.
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