建立了大黄鱼肌肉、肝脏、鳃和血液中阿维菌素的高效液相色谱-荧光检测(HPlC-fld)法.样品用乙腈提取,正己烷脱脂,经碱性氧化铝固相萃取(SPE)柱过滤,1-甲基咪唑和三氟乙酸酐的乙腈溶液在室温下避光衍生化,再经甲醇水解,进行HPlC-fld测定.结果表明,阿维菌素在0.5~50.0μg/l范围内线性良好,检测限为肌肉0.5μg/kg,其他组织1.0μg/kg.添加5.0~50.0μg/kg时,平均回收率为:肌肉81.2%~87.1%,肝脏68.9%~74.4%,鳃67.6%~80.7%,血液52.4%~60.3%,日内精密度和日间精密度分别为:肌肉4.6%~5.5%、6.1%~6.8%;肝脏5.5%~6.2%、7.6%~8.7%;鳃5.1%~6.3%、6.9%~7.5%;血液7.6%~8.9%、9.7%~11.6%,该方法能满足现行兽药残留分析要求.In order to understand the avermectin residues in the tissues of Pseudosciaena crocea,a method for the quantitative determination of this drug in fish muscle,liver,gill and blood sample was established using high performance liquid chromatography with fluorescence detection(HPLC-FLD).The procedures for sample treatment included extraction by acetonitrile,delipidation by n-hexane,clean-up by Basic Alumina solid phase extraction cartridge and derivation by 1-methylinidazole and trifluoroacetic anhydride inacetonitrile at room temperature away from light and hydrolysis by methanol.Samples were analyzed by HPLC coupled to a fluorescence detector.The results indicated that the calibration curves were linear within the working range from 0.5 to 50.0 μg/L.The limit of detection of the method for avermectin in muscle was 0.5 μg/kg,and 1.0 μg/kg for the other three tissues.When 5.0-50.0 μg/kg samples were added,the overall recoveries of avermectin in Pseudosciaena crocea muscle,liver,gill and blood sample were respectively 81.2%-87.1%,68.9%-74.4%,67.6%-80.7%,52.4%-60.3%.The intra-day and inter-day coefficient variations for muscle,liver,gill and blood sample detection were 4.6%-5.5% and 6.1%-6.8%,5.5%-6.2% and 7.6%-8.7%,5.1%-6.3% and 6.9%-7.5%,7.6%-8.9% and 9.7%-11.6%,which meet the current requirements for drug residue analysis.This research provides a reference for the detection of avermectin for the tissues of P.crocea.国家公益性(农业)行业专项(200903029
