鸡肉和鸡蛋中金刚烷胺与金刚乙胺残留检测UPLC-MS/MS法研究

Determination of Amantadine and Rimantadine Residuein Chicken Muscle and Egg by UPLC-MS/MS

关键词:  金刚烷胺  金刚乙胺  鸡肉  鸡蛋  超高效液相色谱-串联质谱

Key words:  Amantadine  Rimantadine  chicken muscle  egg  UPLC-MS/MS

摘要:

建立了鸡肉和鸡蛋中金刚烷胺与金刚乙胺残留检测的超高效液相色谱-串联质谱方法(UPLC-MS/MS)。样品在酸性条件下用乙腈提取后,用正己烷去除脂肪,高速离心去除蛋白质等杂质,上机测试。液相色谱条件：色谱柱为BEH C18(50×2.1mm,1.7μm),流动相为0.1%甲酸乙腈溶液 0.1%甲酸水溶液,流速为0.3 mL/min,柱温为30 ℃,进样量为10 μL。质谱条件：电喷雾离子源(ESI ),多反应监测(MRM)方式进行采集。结果表明：金刚烷胺与金刚乙胺在2~100 ng/mL浓度范围内均呈现良好的线性关系,相关系数(R2)分别为=0.9977和0.9988；鸡蛋和鸡肉中金刚烷胺与金刚乙胺残留检测方法检测限均为1ng/g,定量限均为2ng/g。鸡肉组织在2、5和10 ng/g三个添加浓度检测结果可以看出,金刚烷胺与金刚乙胺的平均回收率分别为79.6％~107.5％和78.4％~101.2％,批内和批间RSD均小于15%鸡蛋在2、5和10 ng/g三个添加浓度检测结果可以看出,金刚烷胺与金刚乙胺的平均回收率分别为96.3％~111.1％和78.1％~87.4％,批内和批间RSD均小于15%。该方法具有简便快捷、灵敏度高、定性准确等特点。

Abstract:

A UPLC-MS/MS method was established for the determination of Amantadine and Rimantadine residue in chicken muscle and egg. The samples were extracted by acetonitrile in acid conditon, then the fat was removed by hexane, and the protein was deposited by high speed centrifugation. LC conditions were as follows: the chromatography column is BEH C18 column of 50×2.1 mm, 1.7 μm；mobile phase is acetonitrile(0.1% formic acid) and water(0.1% formic acid); column temperature is 30 ℃; flow rate is 0.3 mL/min; injection volume is 10 μL. Mass spectrometry conditions were ESI and MRM mode. The calibration curve of Amantadine and Rimantadine were good linear from 2 to 100 ng/mL with the correlation coefficient R2 of 0.9977 and 0.9988, respectively. The limit of detection of the method was 1ng/g, and the limit of quantification was 2ng/g. The average recoveries of Amantadine and Rimantadine from spiked egg at three concentrations of 2, 5 and 10ng/g were 96.3％~111.1％,78.1％ to 87.4％, and intra- and inter-batch RSD were <15%. The average recoveries of Amantadine and Rimantadine from spiked chicken muscle at three concentrations of 2, 5 and 10ng/g were 79.6％~107.5％,78.4％~101.2％,and intra- and inter-batch RSD were <15%.