超高效液相色谱-串联质谱法测定动物源性食品中的金刚烷胺

Determination of amantadine in animal derived food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  金刚烷胺  动物源性食品

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  amantadine  animal derived food

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定动物源性食品(鸡肉、鸡肝、鸡蛋和牛奶)中金刚烷胺的分析方法。方法 样品用0.2%(V:V)甲酸乙腈溶液提取, 经Oasis PRiME HLB小柱净化后用Capcell Pak C18 MGIII-H色谱柱分离, 以甲醇和0.1%甲酸水溶液(V:V)作为流动相进行梯度洗脱, 在多反应监测(multiple reaction monitoring, MRM)模式下进行液相色谱-串联质谱法测定, 基质匹配标准溶液外标法定量。结果 金刚烷胺在1.0~50.0 μg/L范围内线性关系良好(r2=0.9994)。在添加水平为1.0, 5.0和20.0 μg/kg时的回收率为76.3%~93.5%, 相对标准偏差(relative standard deviation, RSD)在3.4%~8.6%之间, 方法的检测限(limit of detection, LOD)为0.2 μg/kg, 定量限(limit of quantification, LOQ)为1.0 μg/kg。结论 该法简便、灵敏、准确, 适合于动物源性食品中金刚烷胺的快速分析测定。

英文摘要:

      Objective To establish a method for determination of amantadine in animal derived food (chichen, chicken liver, egg and milk) by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 0.2% formic acid-acetonitrile (V:V), and purified by Oasis PRiME HLB cartridges, then they were seperated on an Capcell Pak C18 MGIII-H column with methanol and 0.1% formic acid (V:V) as the mobile phases in gradient program. The analytes were determined by MS/MS under multiple reaction monitoring (MRM) mode, and quantified by matrix-matched external standard method. Results There were good linearities between the peak areas and the concentrations in the range of 1.0-50.0 μg/L, with correlation coefficients (r2) more than 0.9994. The recoveries of amantadine were 76.3%-93.5% at the spiked levels of 1.0, 5.0 and 20.0 μg/kg, and the relative standard deviations (RSDs) were 3.4%-8.6%. The limit of detection (LOD) for the established method was 0.2 μg/kg, and the limit of quantity (LOQ) was 1.0 μg/kg. Conclusion The method is simple, sensitive and accurate, which is suitable for determination of amantadine in animal derived food.