多壁碳纳米管分散固相萃取结合LC-MS-MS测定鸡肉中金刚烷胺

建立了采用多壁碳纳米管为吸附剂的分散固相萃取净化、液相色谱串联质谱测定鸡肉中金刚烷胺残留量的方法。鸡肉样品经乙酸乙腈提取后,调节pH值至11,加入75 mg多壁碳纳米管进行分散固相萃取,被吸附的药物经5.0%甲酸溶液:甲醇(5∶5,V/V)洗脱,洗脱液过滤膜后直接进样分析。采用Acquity UPLC BEH C18色谱柱分离,以0.1%甲酸水溶液和甲醇作为流动相作梯度洗脱,电喷雾正电子(ESI+)模式电离,多反应监测模式检测,内标法校准进行定量。金刚烷胺在0.05~5.0μg/L质量浓度范围内呈良好的线性,线性相关系数均大于0.99,鸡肉样品中最低定量限为0.50μg/kg。鸡肉样品中添加0.5~1.0μg/kg金刚烷胺的回收率在97.8%~103.6%之间,相对标准偏差均小于10%。

Determination of Amantadine in Chicken Muscle by Liquid Chromatography with Tandem Mass Spectrometry Coupled with Dispersive Solid Phase Extraction Using Multiwalled Carbon Nanotubes as Adsorbent

A simple, sensitive and reliable analytical method was developed for amantadine in chicken muscle by ultra high performance liquid chromatography-positive electrospray ionisation tandem mass spectrometry （UHPLC-ESI-MS/MS） using dispersive solid phase extraction （dSPE） with multi-walled carbon nanotubes （MWCNTs）. Chicken muscle was extracted using 1.0% acetic acid in acetonitrile. After adjusting pH value to 11, 75 mg of MWCNTs were added to absorpt amantadine and 5.0% formic acid solution：methanol （5：5, V/V） was used to elute the compound from the MWCNTs. The eluate was directly analyzed by LC-MS-MS on an Acquity UPLC BEH C18 column with a mixture of methanol and 0.1% formic acid solution as the mobile phase. The samples were quantified with the internal standard calibration curve method. Good linearities were obtained for amantadine in the concentration range of 0.05-5.0 μg/L with correlation coefficient more than 0.999. The recoveries for amantadine in chicken muscle were 97.8%-103.6% at three fortified levels （0.5, 0.75 and 1.0 μg/kg） with relative standard deviations less than 10.0% （n = 3）. The limit of quantitation was 0.5 μg/kg.