摘要
建立一种超高效液相色谱-串联质谱法测定畜禽肉中恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、沙拉沙星、双氟沙星、司帕沙星、氟罗沙星和达氟沙星共11种喹诺酮类兽药残留的检测方法。畜禽肉样品经2%甲酸-乙腈均质提取,离心沉淀后上清液经QuEChERS净化剂净化后,经快速溶剂蒸发系统浓缩,采用Waters BEH C18色谱柱(2.1 mm×50 mm,1.7?μm)分离,以0.1%甲酸-水和0.1%甲酸-乙腈为流动相进行梯度洗脱,电喷雾离子源电离,多反应监测模式采集信号,内标法定量。结果表明:11种喹诺酮类兽药在2～80 ng/mL质量浓度范围内线性关系良好(R^2>0.99),方法的检出限和定量限分别为0.5～2.0?μg/kg和1.5～6.0?μg/kg;空白样品加标量为10、25、50?μg/kg 3个水平时,11种喹诺酮类兽药的平均加标回收率为74.52%～106.83%,相对标准偏差为1.8%～8.7%(n=6)。该方法检测过程简单快捷、准确度好、灵敏度高,适用于畜禽肉中喹诺酮类兽药残留的检测。
A method for simultaneous determination of enrofloxacin,ciprofloxacin,ofloxacin,pefloxacin,norfloxacin,lomefloxacin,sarafloxacin,difloxacin,sparfloxacin,flerofloxacin and danofloxacin residues in livestock and poultry meat by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Samples were homogenized and extracted with 2%formic acid-acetonitrile.After centrifugation,the supernatant was purified by the QuEChERS procedure,concentrated by a rapid solvent evaporation system,separated on a Waters BEH C18 column(2.1 mm×50 mm,1.7μm)with a mobile phase consisting of 0.1%formic acid-water and 0.1%formic acid-acetonitrile by gradient elution,detected in the multiple reaction monitoring(MRM)mode using an electrospray ionization source(ESI+)and quantified by an internal standard method.The results showed that good linearity was observed for all analytes in the concentration range of 2.0–80.0 ng/mL with correlation coefficients greater than 0.99 and the detection and quantitation limits were respectively 0.5–2.0 and 1.5–6.0μg/kg.The average recoveries of blank samples spiked at 10,25 and 50μg/kg were 74.52%–106.83%,with relative standard deviation(RSD)values of 1.8%–8.7%(n=6).This method proved to be simple,accurate,highly sensitive and suitable for the simultaneous determination of quinolone residues in livestock and poultry meat.
作者
黄坤
吴婉琴
罗彤
付文雯
范小龙
马弋
王会霞
HUANG Kun;WU Wanqin;LUO Tong;FU Wenwen;FAN Xiaolong;MA Yi;WANG Huixia(Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075,China)
出处
《肉类研究》
北大核心
2019年第3期40-45,共6页
Meat Research
基金
"十三五"国家重点研发计划重点专项(2018YFC1604000)
