分散固相萃取结合LC-MS/MS快速测定鸡蛋中的金刚烷胺

Rapid Determination of Amantadine in Eggs by LC-MS/MS and Dispersive Solid-phase Extraction

研究建立了鸡蛋中金刚烷胺的分散固相萃取结合液相色谱一串联质谱测定法。鸡蛋样品经乙腈提取并沉淀蛋白后，提取液用无水硫酸镁脱水、C18和PSA吸附剂吸附脂溶性组分并浓缩后以液相色谱串联四板杆质谱测定，稳定同位素内标法定量。鸡蛋中的金刚烷胺在0．2～10μg／kg范围内呈良好的线性关系，批内、批间精密度小于15％，回收率大于80％，定量限0．2μg／kg。经实际样品的测试，本方法简捷、灵敏、实用。

A dispersive solid-phase extraction combined with liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was established for determination of amantadine in eggs. The egg samples were extracted by acetonitrile, and at the same time, the protein in samples was precipitated by acetonitrile. The extraction was dehydrated by MgSO4, and cleaned up by C18 and PSA adsorbents to remove lipophilic components. After concentrated,the analyte was determined by LC-MS/MS and quantified with stable isotope internal standard. A good linearity was shown between 0.2 μg/kg and 10 μg/kg for amantadine in eggs. The intra- and inter-precision were lower than 15% by calculated the relative standard deviation. The recovery was larger than 80%. The LOQ was 0.2 μg/kg. The method was simple,rapid, sensitive and effective with the practice of real samples.