液相色谱-电喷雾串联质谱法同时检测鸡组织中5种抗病毒类药物的残留量

Multi-residue determination of five antiviral drugs in chicken tissues by liquid chromatography-electrospray ionization tandem mass spectrometry

建立了鸡组织中抗病毒类药物多残留检测的液相色谱-电喷雾串联质谱法(LC-ESI-MS/MS)。采用三氯乙酸-乙腈溶液提取鸡组织中的金刚烷胺、金刚乙胺、美金刚、咪喹莫特和吗啉胍,离心过滤后经强阳离子交换柱(SCX)净化,色谱柱Xamide(100 mm×2.1 mm,5μm)分离,多反应监测(MRM)正离子扫描方式进行质谱检测。结果表明,鸡组织与鸡肝中5种药物的检出限为0.06～0.30μg/kg,定量限为0.2～1.0μg/kg。当5种药物的添加水平为0.2～10.0μg/kg时,在鸡肉中的平均回收率为72.3%～94.2%,相对标准偏差(RSD)(n=6)为3.5%～11.3%;在鸡肝中的平均回收率为70.8%～92.7%,RSD(n=6)为5.3%～12.6%。该方法选择性好,抗干扰能力强,可作为鸡肉和鸡肝中抗病毒药物残留检测的确证方法。

A method of liquid chromatography-electrospray ionization tandem mass spectrometry（LC-ESI-MS/MS） for the simultaneous determination of five antiviral drug residues,amantadine,rimantadine,memantine,moroxydine and imiquimod in chicken tissues was developed.The compounds were extracted from the samples with trichloroacetic acid solution and acetonitrile,and then cleaned-up by strong cation exchange（SCX） solid phase extraction cartridges.The analytes were separated on a Xamide column（100 mm×2.1 mm,5 μm） and determined qualitatively and quantitatively with tandem mass spectrometry using positive polarity mode under multi-reaction monitoring（MRM） scan type.The limits of detection and the limits of quantification were 0.06-0.30 μg/kg and 0.2-1.0 μg/kg,respectively.The average recoveries of the five drugs were 72.3%-94.2% in chicken muscle and 70.8%-92.7% in chicken livers.The relative standard deviations（RSDs） in chicken muscle and livers were 3.5%-11.3% and 5.3%-12.6%,respectively.The method is selective without interference and suitable for the determination and confirmation of the five antiviral drugs in chicken muscle and livers.