高效液相色谱-串联质谱法检测猪肝中苯并咪唑类药物及其代谢物的残留量  

Simultaneous Determination of Benzimidazoles and Their Metabolites Residues in Pig Liver by HPLC-MS/MS

作　　者：刘琪[1] 朱馨乐[1] 孙雷[1] 王树槐[1] 汪霞[1] 

机构地区：[1]中国兽医药品监察所,北京100081

出　　处：《中国兽药杂志》2010年第2期1-6,共6页Chinese Journal of Veterinary Drug

基　　金：国家科技支撑计划课题项目(2006BAD31B09)

摘　　要：建立了猪肝中阿苯哒唑及其代谢物阿苯哒唑砜、阿苯哒唑亚砜、2-氨基阿苯哒唑砜，噻苯哒唑及其代谢物5-羟基噻苯哒唑，甲苯哒唑及其代谢物氨基甲苯哒唑、5-羟基甲苯哒唑，芬苯哒唑及其代谢物芬苯哒唑砜、等效物奥芬哒唑，氟苯哒唑及其代谢物2-氨基-氟苯哒唑共14种苯并咪唑类药物及其代谢物残留检测的高效液相色谱-串联质谱方法。样品用乙酸乙酯提取，MCX固相萃取柱净化。WatersXterraC18色谱柱（2．1mm×150mm，5μm）分离，流动相A相为0．1％甲酸乙腈溶液；B相为0．1％甲酸水溶液，梯度洗脱，外标法定量。结果表明，14种苯并咪唑类药物及其代谢物标准溶液在10～1000ng／mL的浓度范围内呈现良好的线性关系，尺。均大于0．99，方法检测限为5斗g／kg，定量限为10μg／kg，14种苯并咪唑类药物及其代谢物在10—200μg／kg添加浓度范围内回收率均70％～120％之间。批内、批间相对标准偏差均小于20％。本方法灵敏、准确，满足食品安全检测法规的要求。A high performance liquid chromatography -tandem mass spectrometry （HPLC -MS/MS） method was established for the simultaneous determination of benzimidazoles and metabolites： albendazole, albendazole sulfone, albendazole sulfoxide, albendazole - 2 - aminosulfone, thiabendazole, thiabendazole - 5 - hydroxy, mebendazole, mebendazole- amine, 5 -hydroxymebendazole, fenbendazole, fenbendazole sulfone, oxfendazole, flubendazole, flubendazole -2 -aminosulfone residues in pig liver. The samples were extracted by ethyl acetate, cleaned up with Waters Oasis MCX solid phase extraction （SPE） column. The separation of benzimidazoles and metabolites was performed on Waters 2695 - Quattro micro system with a Xterra Cls column, （2.1 mm × 150 mm, 5 μm） and the gradient elution solvent of acetonitrile （containing 0. 1% formic acid） and water （containing 0.1% formic acid） at a flow rate of 0.2 mL/min. The method was quantified by external standard method. The calibration curves were good linear between the peak areas and the concentrations of 10 - 1 000 ng/mL with the correlation coefficient R2 〉 0.99. and the limit of quantification was 10 μg/kg. The average recoveries from spiked animal tissues at four concentrations of 10 -200 μg/kg ranged 70% - 120%. The relative standard deviations of intra - and inter - batch were both less than 20%.

关 键 词：高效液相色谱-串联质谱 肝 苯并咪唑 代谢物 残留 

分 类 号：S859.84[农业科学—临床兽医学]