高效液相色谱-串联质谱法检测动物源性食品中9种抗病毒药物残留

Determination of Nine Antiviral Drug Residues in Animal Origin Foods by High Performance Liquid Chromatography-tandem Mass Spectrometry

本研究建立了一种高效液相色谱-串联质谱测定肉、蛋、奶等动物源性食品中奈韦拉平、泛昔洛韦、阿比多、阿昔洛韦、咪喹莫德、美金刚、金刚烷胺、奥司他韦和吗啉胍9种抗病毒药物残留的方法。样品前处理采用1%乙酸-乙腈提取,经PRiME HLB小柱净化后检测。采用乙腈-10 mmol/L乙酸铵溶液(含0.1%甲酸)流动相体系,在梯度洗脱的模式下,经Sielc Obelisc R柱分离,电喷雾离子源模式电离、多反应监测(MRM)模式进行检测,可以实现9种目标物的分离。结果表明9种抗病毒药物组分在一定浓度范围内线性关系良好,决定系数R 2为0.9991~0.9998,检出限范围为0.1~0.5μg/kg,定量限范围为0.3~1.5μg/kg,加标回收率达到82.3%~95.7%,相对标准偏差为3.2%~5.9%(n=5)。利用本方法对10份样品进行检测,并与标准方法进行对比。本方法准确度和灵敏度均较高,可以满足动物源性食品中9种抗病毒药物残留的检测需求。

A method for detecting nine antiviral drug residues of nevirapine,famciclovir,abidox,acyclovir,imiquimod,memantine,amantadine,oseltamivir and morpholinoguanidine in animal origin foods such as meat,egg and milk was established by high performance liquid chromatography-tandem mass spectrometry.The samples were first extracted by 1%acetic acid-acetonitrile solution,then purified by PRiME HLB column.The nine components were separated by Sielc obelisc R column and gradiently eluted using acetonitrile-10 mmol/L ammonium acetate solution(containing 0.1%formic acid)as mobile phase.The detection of antiviral drugs was performed by tandem mass spectrometry in electrospray ionization under multiple reactions monitoring(MRM)mode.The calibration curves for the nine antiviral drugs were linear over the range,and the determination coefficients R 2 was 0.9991~0.9998.The detection limit of the nine antiviral drugs ranged from 0.1~0.5μg/kg,and quantitative limit ranged from 0.3~1.5μg/kg.The recoveries of the nine antiviral drugs were between 82.3%and 95.7%with the relative standard deviations of 3.2%~5.9%(n=5).This method was used to detect 10 samples and compared with the standard method.The method has high accuracy and sensitivity,and can meet the detection needs of antiviral drug residues in animal origin foods.