高效液相色谱—串联质谱法测定鲍鱼中硝基呋喃类代谢物残留量

本文用高效液相色谱-串联质谱法测定鲍鱼中3-氨基-2-噁唑烷基酮(AOZ)、5-甲基吗啉-3-氨基-2-噁唑烷基酮(AMOZ)、氨基脲(SEM)、1-氨基-2-内酰脲(AHD)4种硝基呋喃类代谢物残留量的方法。0.2mol/L盐酸溶液水解鲍鱼组织中与蛋白结合的硝基呋喃类代谢物,用0.05mol/L的2-硝基苯甲醛溶液(2-NBA)37℃衍生16小时。用1.0mol/L磷酸氢二钾溶液调节pH至7.0~7.5,乙酸乙酯萃取。采用电喷雾电离,正离子扫描,选择反应监测模式(SRM)监测,内标法定量。本方法对4种硝基呋喃类代谢物标准曲线的线性回归系数均在0.99以上,线性范围为0.5μg/kg~20μg/kg。方法定量限为0.5μg/kg。在添加浓度0.5μg/kg~5μg/kg,回收率在75.2%~102.1%之间,相对标准偏差为3.56%~12.6%。说明本方法简单、灵敏,结果可靠,可满足实验室大量、快速分析的需求。

Determination of nitrofuran metabolites in abalone by high performance Liquid Chromatography-Tandem Mass Spectrometry

A method has been developed for four metabolites of nitrofuran antibiotics such as 3-amino-2-oxazolidinone（AOZ）,5-morpholino-methyl-3-anmino-2-oxazolidinone（AMOZ）,semicarbazid（SEM） and 1-aminohydantoin（AHD） by high performance Liquid Chromatography-Tandem Mass Spectrometry.Abalone tissues samples were hydrolyzed with 0.2mol/L HCl,and derivatived at 37℃ for sixteen hours with 2-nitrobenzaldenhyde.The derivatived solutions were adjusted to pH 7.0~7.5,and extracted with ethyl acetate.Analyte identification and quantification were performed using selected reaction monitoring（SRM） with one precursor ion and two product ions as identifiers and electrospray ionization in positive mode.There are good linear correlations between the peak areas and concentrations of the four metabolites of nitrofuran antibiotics（the calibration coefficients are above 0.99）,the dynamic linear range is 0.5~20μg/kg.The limit of detection is 0.5μg/kg for AOZ,AMOZ,SEM,AHD.The average recoveries ranged from 75.2% to 102.1% and their relative standard deviations are between 3.56 % and 12.6 % The method can be used to identify and quantify the metabolites of nitrofuran antibiotics in aquatic products with satisfactory sensitivity,accurcy and precision.