建立了鸡蛋和鸡肉中金刚烷胺和金刚乙胺残留量的分散固相萃取-超高效液相色谱-串联质谱测定方法。鸡蛋和鸡肉样品经氨水-乙腈（2：98，v／v）提取后，提取液经氮气吹干至1 mL后，利用C18和NH2填料进行分散固相萃取净化，过滤膜后分析。采用ZORBAX C18色谱柱分离，用1 mmol／L乙酸铵水溶液（含0.1％（ v／v）甲酸）-甲醇作为流动相进行梯度洗脱，正离子多反应监测模式。结果表明，金刚烷胺和金刚乙胺在0.15~10.0μg／L 范围内具有较好的线性关系，鸡蛋和鸡肉中的检出限均为0.05μg／kg，定量限均为0.20μg／kg。当2种药物在鸡蛋和鸡肉中的加标水平为0.2、1.0和2.0μg／kg时，平均回收率范围为89％~108％，相对标准偏差范围为5.0％~8.6％。该方法能够满足鸡蛋和鸡肉中金刚烷胺和金刚乙胺残留量分析的要求。
A method was developed for the determination of residual amantadine and rimanta-dine in eggs and chickens by dispersive solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry. Egg and chicken samples were extracted with ammonia water-acetonitrile(2:98,v/v). The extraction solution was dried to 1 mL under nitro-gen,and then purified by dispersive solid phase extraction method with C18 and NH 2 sorbents. After purification,the extraction solution was filtered through a filter. The target compounds were analyzed by ultra high performance liquid chromatography-tandem mass spectrometry ( UHPLC-MS/MS)on a ZORBAX C18 column using a mixture of 1 mmol/L ammonium acetate solution( containing 0. 1%( v/v ) formic acid ) and methanol as mobile phases with gradient elution. The mass spectrometer was operated under multiple reaction monitoring( MRM)mode in positive mode. The good linearities were obtained for amantadine and rimantadine at a con-centration range of 0. 15-10. 0 μg/L. The limits of detection for amantadine and rimantadine were all 0. 05 μg/kg,and the limits of quantification were 0. 20 μg/kg. The recoveries of aman-tadine and rimantadine in eggs and chickens at three spiked levels(0. 2,1. 0 and 2. 0 μg/kg) were in the range of 89%-108% with the relative standard deviations of 5. 0%-8. 6%. The results demonstrated that the method is suitable for the determination of amantadine and rimantadine in eggs and chickens.
参考文献
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