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

Determination of amantadine residues in chicken tissue by UPLC-QTOF

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. 8ng·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.