采用高效液相色谱分离,荧光检测器检测,建立了固相萃取分析牛组织中埃普利诺菌素、阿维菌素、多拉菌素和伊维菌素残留的方法.样品用乙腈提取,碱性氧化铝和C18SPE柱净化,用乙酸酐和1-甲基咪唑的乙腈溶液作衍生化试剂,在96℃条件下,完全衍生化需要100min.4种药物的平均回收率为70.02%~88.75%,日内变异系数小于8.52%,日间变异系数小于7.13%.埃普利诺菌素、阿维菌素、多拉菌素和伊维菌素的检出限为0.4~0.5μg/kg,定量限为2ug/kg.该方法可靠、灵敏,可用于常规残留分析.
A method using high performance liquid chromatography (HPLC) with fluorescence detection was presented for the simultaneous measurement of the eprinomectin, avermectin, doramectin and ivermectin in liver. Samples were extracted with acetonitrile and cleaned up using solid phase extraction on alumina B and C18 column, and followed by derivatization with acetic an hydride and 1-methylimidazole in acetonitrile. The optimum time required for the completion of derivation reaction of the 4 drugs was 100 min at 96℃. Mean recoveries of the 4 drugs in bovine liver ranged from 70.02% to 88.75%. The intra-and inter-day variations were less than 8.52%and 7.13% respectively. The limit of detection was 0.4-0.5μg/kg, and the limit of quantitation of the method was 2 μg/kg for all of the 4 drugs. The procedure provides a reliable and sensitive method for routine residual analysis.