超高效液相-飞行时间质谱法测定鸡肉组织中金刚烷胺残留

目的：建立超高效液相-飞行时间质谱法（UPLC-QTOF）测定鸡肉组织中的金刚烷胺。 方法：样品用1%三氯乙酸溶液-乙腈（1：1）溶液超声提取，经固相萃取柱净化浓缩，用Acquity UPLC^® BEH C₁₈柱分离，以乙腈和0.1%甲酸作为流动相进行梯度洗脱，采用电喷雾离子源（ESI）正离子模式将样品离子化，TOF MSMS模式进行检测，提取m/z 135.12的碎片离子进行监测，以色谱保留时间和质谱碎片离子丰度比定性，外标法定量。 结果：金刚烷胺在5.91~147.75 ng·mL^-1浓度范围内，线性关系良好，检出限（LOD）为4.9 ng·g^-1，定量限（LOQ）为9.8 ng·g^-1。回收率在81.8%~96.3%范围内，精密度<6.4%。 结论：本文建立的方法经方法学验证，适合鸡肉组织中金刚烷胺残留的检测。

Objectives: To establish a UPLC/TOF-MS method for determination of amantadine residues in chicken tissue.Methods: The samples were extracted with acetonitrile-1.0% trichloroacetie acid(50:50) solution in ultrasonic bath.Sample purification and concentration were performed by SPE.The liquid chromatography separation was achieved on an ACQUITY UPLC^® BEH C₁₈ column,the mobile phase consisted of acetonitrile-0.1% formic acid with gradient elution.The analyses were operated in the positive electrospray ionization(ESI) source and detected in TOF MSMS mode to extract the product ion of m/z 135.12 as the monitoring ion.The chromatographic retention time and mass fragment ion abundance ratio were taken for qualitative confirmation and the external standard method was employed for quantification.Results: The method was linear in the concentration range of 5.91-147.75 ng·mL^-1.The limit of detection(LOD) was 4.9 ng·g^-1,and the limit of quantification(LOQ) was 9.8 ng·g^-1.Recoveries were in the range of 81.8%-96.3%,and the RSD was less than 6.4%.Conclusions: The methodological validation showed that the method established in this paper could be used for determination of the amantadine residues in chicken tissue.

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