Determination of two genotoxic impurities in sulconazole nitrate by combining derivatization with LC-MS method
An analytical method was established for the determination of alkyl sulfate esters genotoxic im-purities in sulconazole nitrate,including dimethyl sulfate and diethyl sulfate.The separation was per-formed on an HILIC column(2.1 mm×50 mm,3 μm)utilizing the aqueous phase of 20 mmol·L-1 ammo-nium formate solution-formic acid(1 000∶1)and the organic phase of acetonitrile with isocratic elution(10∶90)at the flow rate of 0.2 mL·min-1.The column temperature was set at 20 ℃.Multiple reaction monitoring(MRM)mode was performed on quantitative determination.Effects of temperature and time for derivatization were investigated.Under the conditions,the linear correlation coefficient of dimethyl sulfate and diethyl sulfate were 0.999 7 and 0.998 9,respectively.And the recovery were 80.3％—102.3％and 90.3％—100.0％,respectively.The operation is simple and meets the requirements of quantitative analysis.
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