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

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, 5 μm)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0.06～0.30 μg/kg,定量限为0.2～1.0 μg/kg。当5种药物的添加水平为0.2～10.0 μg/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。

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

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.