液相色谱_串联质谱法测定猪肉中13种磺胺类药物残留_张志刚.pdf

2013, Vol. 27, No. 02 13 CHINA MEAT RESEARCH CENTER MEAT RESEARCH -13 ( 361100) -13 1%-0.1%--Kinetex C18 (100mm2.1mm2.6μm)0.1%- μ μ 131300 g/kg10 g/kg1 μ μ 2 g/kg10 g/kg 360.0%78.1%(RSD)0.24%8.88% Simultaneous Determination of Thirteen Sulfonamides in Pork by HPLC-MS/MS ZHANG Zhi-gang (State Key Laboratory of Food Safety Technology for Meat Products, Xiamen Yinxiang Group Co. Ltd., Xiamen 361100, China) Abstract An HPLC-MS/MS method was developed for the simultaneous and rapid determination of thirteen sulfonamides in pork. Sulfonamide residues in samples were extracted with acidic acetonitrile. The extract was concentrated, defatted with hexane, fi ltered through a 0.22 μm fi lter membrane and transferred to a sample vial prior to HPLC-MS/MS analysis. Chromatographic separation was performed on a Kinetex C18 (100 mm 2.1 mm, 2.6 μm) column using a gradient elution with water (0.1% formic acid) and acetonitrile as mobile phases. The mass spectrometer was operated using multiple reaction monitoring in positive ionization mode. All thirteen sulfonamides showed good linearity in the concentration range of 1 to 300 μg/kg, and the limit of quantifi cation for each of the sulfonamides was below 10 μg/kg. The average recoveries from samples spiked at levels of 1, 2 and 10 μg/kg ranged from 60.1% to 78.1% with relative standard deviations of 0.24%8.88%. The HPLC-MS/MS method is simple, sensitive, selective, and applicable for the routine simultaneous determination of sulfonamides in meat. Key words meat sulfonamides liquid chromatography mass spectrometry