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

作　　者：仲伶俐[1] 郭灵安[1] 付成平[1] 李曦[1] 雷欣宇[1] 赵姗 李华仙[1] ZHONG Ling-Li;GUO Ling-An;FU Cheng-Ping;LI Xi;LEI Xin-Yu;ZHAO Shan;LI Hua-Xian(Analysis and Testing Center of Sichuan Academy of Agricultural Sciences, Chengdu 610066, China)

机构地区：[1]四川省农业科学院分析测试中心,成都610066

出　　处：《食品安全质量检测学报》2018年第6期1321-1325,共5页Journal of Food Safety and Quality

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1.0~50.0μg/L范围内线性关系良好(r^2=0.9994)。在添加水平为1.0,5.0和20.0μg/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0.2μg/kg,定量限(limit of quantification,LOQ)为1.0μg/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。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 1.0-50.0μg/L, with correlation coefficients （r^2） more than 0.9994. The recoveries of amantadine were 76.3%-93.5% at the spiked levels of 1.0, 5.0 and 20.0μg/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.

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 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]