高效液相色谱-串联质谱法测定熟制鸡肉制品中金刚烷胺

Determination of Amantadine in Cooked Chicken Products by High Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱（HPLC-MS/MS）测定熟制鸡肉制品中金刚烷胺的分析方法。样品用乙腈提取,PXC小柱净化,经C18色谱柱分离,以电喷雾离子源（ESI）在正离子多反应监测（MRM）模式下进行测定,内标法定量。金刚烷胺的检出限为0.05μg/kg,定量限为0.15μg/kg,在0.3～150μg/L范围内线性关系良好,相关系数r2为0.9992。对于4种不同的熟制鸡肉制品,在4个加标水平下的平均回收率范围为87.2%～94.8%,批内精密度（n=6）为6.7%～10.0%,批间精密度（n=3）为8.5%～13.6%。该方法灵敏度高,准确性好,适用于熟制鸡肉制品中金刚烷胺残留量的测定。

A method for the determination of amantadine in cooked chicken products has been developed by high performance liquid chromatography coupled to tandem mass spectrometry（ HPLC- MS / MS）. The sample was extracted by acetonitrile,then cleaned up by PXC solid phase extraction cartridge,and then separated on a C18 column and finally analyzed by HPLC- MS / MS under multiple reaction monitoring（ MRM） mode via positive electrospray ionization,and an internal standard calibration method was used. The limit of determination for amantadine was 0. 05 μg / kg,and the limit of quantitation was 0. 15 μg / kg. The calibration curves showed good linearity in the range of 0. 3 ～ 150 μg / L with the correlation coefficient of 0. 9992. The average recoveries of amantadine at 4 spiked levels,in 4 kinds of cooked chicken products,were in the range of 87. 2% ～ 94. 8% with intra- assay precision of 6. 7% ～ 10. 0%（ n = 6）,and inter- assay precision of 8. 5% ～ 13. 6%（ n = 3）. The method is accurate and sensitive,which is suitable for the determination of amantadine in cooked chicken products.