鸡、猪组织中甲砜霉素、氟苯尼考、氟苯尼考胺残留量测定的GC-MS法建立

Determination of Thiamphenicol,Florfenicol and Florfenicol Amine Residues in Chicken and Swine Tissues by Gas Chromatography-Mass Spectrometry

为监控鸡和猪组织中酰胺醇类药物残留,保障畜禽产品质量安全,建立了同时测定鸡和猪组织中甲砜霉素(TAP)、氟苯尼考(FF)及其代谢物氟苯尼考胺(FFA)残留量的气相色谱-质谱法(GC-MS)。样品经2%氨化乙酸乙酯溶液提取,PEP-2固相萃取柱净化,N,O-双三甲基硅烷三氟乙酰胺(BSTFA)衍生,气相色谱-质谱法测定,内标法定量。结果显示,甲砜霉素、氟苯尼考及其代谢物氟苯尼考胺在5~5000μg/L浓度范围内线性关系良好,相关系数r均大于0.999。本方法在鸡、猪肌肉、皮+脂(脂肪)、肝脏和肾脏中的检出限均为5μg/kg,定量限均为10μg/kg,在鸡和猪各空白组织添加10~5000μg/kg浓度水平下,其平均回收率在88.1%~106.4%之间,相对标准偏差在1.5%~10.8%之间。结果表明:本方法准确可靠,普遍适用于鸡和猪各组织中TAP、FF、FFA残留量的检测。

To monitor the residues of amphenicol in chicken and swine tissues and ensure the safety of animal products,method for simultaneously determination of TAP,FF and its metabolite FFA residues in chicken and swine tissues was established by GC-MS.Samples were extracted by 2%ammoniated ethyl acetate,purified by PEP-2 solid phase extraction column,derivated by BSTFA,determined by GC-MS and quantified by internal standard.Results showed that between the concentration of 5~5000μg/L the linearity of TAP,FF,and its metabolite FFA were fine and correlation coefficients were exceeding 0.999.The limit of detection in chicken and swine tissues including muscle,skin plus fat(fat),liver,kidney tissues were 5μg/kg and limit of quantification were 10μg/kg.Average recoveries ranged from 88.1%to 106.4%at the spiked level of 10~5000μg/kg in blank chicken and swine tissues.The relative standard deviations ranged from 1.5%to 10.8%.Results showed that the method was accurate,selective and was universally suitable for the determination of TAP,FF,FFA in chicken and swine tissues.