关键词: 高效液相色谱- 串联质谱, 内标法, 水产品, 磺胺类药物, 多残留, 同时测定

Abstract:

The method for simultaneous determination of 18 sulfonamide residues (SAs) in aquatic was developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Deuterium substituted reagents were used as internal standards and added to the sample before extraction. The sample was extracted with acidified acetonitrile, cleaned up with hexane, and concentrated with a rotary evaporator．The mass spectrometer was operated in the positive ion mode using select reaction monitoring for qualitative and quantitative analysis of 18 SAs at the same time. The limits of detection for SAs were 0.5μg/kg (RSN =3) except for sulfaguanidine and sulfaphenazole，which were 1.0 μg/kg, and the limits of quantitation were 1.0 μg/kg, except sulfaguanidine and sulfaphenazole，which were 2.0 μg/kg. The correlation coeficient of linear calibration curve was over 0.99 within the SAs concentration range 5.0 － 200 μg/ml except for sulfaguanidine and sulfaphenazole．The average recoveries for 18 SAs were 70% to 120%. The method are simple operation, and it make fast analysis come true.

Key words: high performance liquid chromatography-tandem mass spectrometry, internal standard method, aquatic products, sulfonamide, multi-residue, simultaneous determination