摘要: |
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0.05 μg/kg,定量限为0.15 μg/kg,在0.3 μg/L~150 μg/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。 |
关键词: 高效液相色谱-串联质谱 金刚烷胺 熟制鸡肉制品 |
DOI: |
投稿时间:2016-02-14修订日期:2016-03-18 |
基金项目: |
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Determination of amantadine in cooked chicken products by high performance liquid chromatography coupled to tandem mass spectrometry |
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(Inspection and Quarantine Technique Centre,Qinhuangdao Entry-Exit Inspection and Quarantine Bureau) |
Abstract: |
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. |
Key words: High performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) Amantadine Cooked chicken products |