高效液相色谱-串联质谱法测定水产品中硝基咪唑类药物残留量

Determination of nitroimidazole drug residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS)

为建立高效液相色谱-串联质谱测定水产品中10种硝基咪唑类药物残留量的检测方法,样品经乙酸乙酯提取、正己烷除脂净化,采用高效液相色谱-串联质谱法在正离子模式下进行检测,外标法定量。结果表明,在优化的前处理方法和仪器条件下,10种硝基咪唑类药物在5.00~200 ng/mL的浓度范围内具有良好的线性关系,线性相关系数均大于0.9950;在不同水产样品中分别添加1.00、2.00和5.00μg/kg三个浓度水平时,加标回收率在70.2%~119%之间,相对标准偏差为1.46%~13.5%。该方法准确度和精密度均满足兽药残留检测的要求,而且操作简单、快速,可适用于水产品中硝基咪唑类药物的大批量样品检测。

A highly sensitive detection of 10 nitroimidazole drug residues in aquatic products has been achieved by optimizing the sample pretreatment methods combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS).The nitroimidazole drug residues in samples were extracted with ethyl acetate and removed fat by n-hexane,then quantified by the external standard method after detected in the positive ion mode by high performance liquid chromatography-tandem mass spectrometry.Under the optimized pretreatment methods and instrument conditions,the calibration curves were linear in a concentrations range of 5.00~200μg/mL with R>0.9950.The average recovery was 70.2%~119%and the relative standard deviation was in the range of 1.46%~13.5%for spiked aquatic sample with 1.00μg/kg,2.00μg/kg and 5.00μg/kg of nitroimidazoles.The accuracy and precision of the method was in accordance with the requirements of veterinary drug residue detection,and the operation was simple and fast.It showed that the method was suitable for the nitroimidazole drug residues detection of large quantities of samples.