液相色谱-串联质谱法高通量定性筛查畜禽肉中221种兽药残留

High-throughput Qualitative Screening of 221 Veterinary Drug Residues in Livestock and Poultry Meat by Liquid Chromatography-tandem Mass Spectrometry

该文建立了一种基于液相色谱-串联质谱的畜禽肉中221种兽药残留的高通量定性筛查方法。畜禽肉样品经1%甲酸(V/V)-乙腈提取,提取液于40℃水浴下氮气吹干,30%甲醇(V/V)-0.1%甲酸(V/V)水溶液复溶后测定。以甲醇和5 mmol/L乙酸铵(含0.1%甲酸,V/V)为流动相梯度洗脱,流速为0.3 mL/min,进样体积为2μL,柱温保持40℃,采用C18色谱柱分离,ESI离子源正负离子模式同时进行多反应监测(MRM),以化合物保留时间及离子丰度比定性。各兽药化合物峰型尖锐对称,该方法在猪肉、牛肉、羊肉、鸡肉、鸭肉基质中的筛查检出限分布在0.1μg/kg和20μg/kg之间,均能满足筛查基本要求。该方法简便快捷,专属性强、无明显干扰,能在短时间内实现大批量样品的处理和筛查定性,已应用于实际样品的检测,检出率高,定性能力强,并且可以扩展至其他动物源性食用农产品基质的定性筛查检测。

A high-throughput qualitative screening method for 221 veterinary drug residues in livestock and poultry meat based on liquid chromatography-tandem mass spectrometry was established.Livestock and poultry meat samples were extracted with 1%formic acid-acetonitrile,and the extract was dried under nitrogen in a water bath at 40℃and reconstituted in 30%methanol-0.1%formic acid aqueous solution for determination.Gradient elution was carried out with methanol and 5 mmol/L ammonium acetate(containing 0.1%formic acid)as the mobile phase,with the flow rate being 0.3 mL/min,the injection volume being 2μL,the column temperature being kept at 40℃,and C18 chromatographic column being used for separation.Multiple reaction monitoring(MRM)was performed simultaneously in positive and negative ion mode,and the compound was qualitatively analyzed based on retention time and ion abundance ratio.The peak shape of veterinary drug compounds was sharp and symmetrical.The detection limit of this method for pork,beef,mutton,chicken and duck matrices was between 0.1μg/kg and 20μg/kg,which can meet the basic requirements for screening.This method is simple and rapid,with high specificity no obvious interference.The method can realize the processing and screening of large quantities of samples in a short time period.It has been applied to the detection of actual samples with high detection rate and strong qualitative ability,and can be extended the application to the qualitative screening and detection for other animal-derived edible agricultural product matrices.