HPLC/UV法对银鲫肌肉组织中甲苯咪唑及其代谢产物残留的同时测定

Simultaneous Determination of Mebendazole and Its Metabolites in Johnny Carp(Carassius Auratus Gibelio) Muscle by HPLC/UV Method

建立了一种用高效液相色谱同时测定银鲫肌肉组织中甲苯咪唑（MBZ）及其代谢物氨基甲苯眯唑和羟基甲苯咪唑的方法。银鲫肌肉组织用乙酸乙酯提取，萃取物旋转蒸发至干后用1mL二甲基甲酰胺-0．05mol／L磷酸盐缓冲液（体积比3：7）定容。色谱条件：Waters symmetryC18反相色谱柱（250mm×4．6mm，5μm）；流动相：乙腈-0．05mol／L磷酸二氢铵溶液（体积比33：67）；流速：0．8mL／min；检测波长为298nm；检测温度为室温。在10～120μg／kg添加水平，MBZ、MBZ—NH2、MBZ—OH的回收率分别为81％－86％、71％－75％、86％～93％。MBZ的检出限为2μg／kg，MBZ—OH和MBZ—NH2检出限均为3μg／kg。

A simple high-performance liquid chromatographic （HPLC） method was developed for the determination of mebendazole （ MBZ ） and its metabolites hydroxymebendazole （ MBZ - OH）, aminomebendazole（ MBZ -NH2 ） in Johnny carp（ Carassius auratus gibelio） muscle, The sample was extracted with ethyl acetate. The extracts were evaporated to dryness and redissolved in 1 mL dimethylformamide- ammonium phosphate buffer（3 ： 7, by volume）. The analytes were separated on a reversed phase Cls reverse chromatogramphie column（250 mm ×4.6 mm, 5 μm） at room temperature, using acetonitrile- 0. 05 mol/L ammonium phosphate buffer（S3 ： 67, by volume） as mobile phase with a flow rate of 0. 8 mL/min. The detection wavelength was set at 298 nm. The mean recoveries at four fortification levels of 10, 30, 60, 120μg/kg were in the range of 81% -86% for MBZ, 71% - 75% for MBZ - NH2, and 86% -93% for MBZ - OH. The detection limits（3S/N） were found to be 2 μg/kg for MBZ and 3 μg/kg for MBZ - OH and MBZ - NH2. The low detection limit and good accuracy of method make it suitable for the routine determination of MBZ and its metabolites in fish muscle.