液相色谱-串联质谱法测定猪肉中13种磺胺类药物残留

利用液相色谱-电喷雾串联质谱建立猪肉中13种磺胺类药物残留的同时、快速分析方法.猪肉样品中的残留药物用1%乙酸-乙腈均质提取,浓缩后用0.1%甲酸-乙腈定容,并用正己烷液-液分配除脂后,用Kinetex C18色谱柱(100mm×2.1mm,2.6μm)分离,以0.1%甲酸-乙腈作为流动相梯度洗脱,采用电喷雾正离子电离,多反应监测模式检测,基质匹配外标法定量.13种磺胺类药物在1~300μg/kg范围内线性关系良好,定量限均小于10μg/kg.在1、2μg/kg和10μg/kg这3个添加水平下,回收率在60.0%~78.1%之间,相对标准偏差(RSD)在0.24%~8.88%之间.此方法操作简便,灵敏度、准确度、精密度均满足残留分析的要求.

Simultaneous Determination of Thirteen Sulfonamides in Pork by HPLC-MS/MS

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,filtered through a 0.22 μm filter 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 quantification 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.