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建立了同时测定鱼、虾生物体中甲苯咪唑及代谢物-氨基甲苯咪唑和羟基甲苯咪唑残留的分析方法。样品以水和乙酸乙酯提取,正己烷去脂、MCX固相萃取柱净化,高效液相色谱-紫外检测器测定。重点研究了样品前处理方法,并对各种不同的固相萃取柱的净化效果和准确度进行了研究。甲苯咪唑及代谢物在5~200μg/kg的添加水平下回收率为81.4%~95.3%,相对标准偏差为1.9%~8.6%,方法线性范围为10~2000ng/mL。方法检测限为甲苯咪唑:5μg/kg,羟基甲苯咪唑:5μg/kg,氨基甲苯咪唑:10μg/kg。
An analytical method was established for the simultaneous determination of mebendazole and its metabolites, aminobenzimidazole and hydroxybenzimidazole, in fish and shrimp organisms. Samples were extracted with water and ethyl acetate, n-hexane defatted, cleaned up with MCX SPE, and detected by HPLC-UV detector. Focus on the sample preparation methods, and a variety of solid-phase extraction column purification effect and accuracy were studied. The recoveries of mebendazole and metabolites ranged from 81.4% to 95.3% at 5-200 μg / kg with the relative standard deviations of 1.9% -8.6%. The linear range was 10-2000 ng / mL. The detection limits of the method were mebendazole: 5μg / kg, hydroxybenzimidazole: 5μg / kg, aminomebezole: 10μg / kg.