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Simultaneous Determination of Residues of Four Typical Categories of Veterinary Antibiotics in Organic Fertilizers
Author(s): 
Pages: 587-594
Year: Issue:  5
Journal: Rural Eco-Environment

Keyword:  SPE-UPLC-MS/MS 有机肥 兽药残留;
Abstract: 建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)法同时测定有机肥中7种磺胺类、4种氟喹诺酮类、4种四环素类和3种大环内酯类抗生素残留的方法。采用乙腈和磷酸盐缓冲液(pH=3)的混合液作为有机肥样品的提取溶液,用强阴离子交换柱(SAX)-亲水亲脂平衡萃取柱(HLB)串联进行提取液的富集和纯化。以甲醇-φ=0.1%的甲酸溶液作为流动相,进行液相质谱分析。18种抗生素在5~500μg·kg-1的浓度范围内线性关系良好,决定系数(r2)≥0.99。以3倍信噪比估算磺胺类、氟喹诺酮类、四环素类和大环内酯类的检测限分别为0.37~4.65、0.43~2.42、0.94~2.78和0.83~4.20μg·kg-1,这4类抗生素50和500μg·kg-12个添加水平的样品平均加标回收率分别为71.6%~94.3%、72.3%~86.7%、71.0%~102.2%和70.7%~93.3%,相对标准偏差在2.1%~11.4%之间。采用所建方法对南京地区市售8种有机肥中18种抗生素含量的测定结果显示,除磺胺类外,其他抗生素均有不同程度的检出。
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