高效液相色谱-串联质谱法测定辣椒及辣椒制品中金刚烷胺残留  

Determination of Amantadine Residues in Pepper and Pepper Products by High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

作　　者：胡巧茹 周长朋 张玉春 崔嘉 鞠玲燕 杨丽君 

机构地区：[1]威海出入境检验检疫局检验检疫技术中心,山东威海264205

出　　处：《分析测试学报》2014年第10期1184-1188,共5页Journal of Instrumental Analysis

基　　金：国家科技支撑计划项目(2012BAK08B01);质检公益性行业科研专项资助(201310143);国家质检总局科技计划项目(2013IK178)

摘　　要：建立了高效液相色谱-串联质谱（ HPLC-MS/MS）测定辣椒及辣椒制品中金刚烷胺残留的分析方法。样品采用1％三氯乙酸溶液-甲醇（1：1）提取，经Oasis-MCX固相萃取小柱净化后用Atlantis T3 C18柱进行分离，以0.1％甲酸水-乙腈（85：15）作为流动相进行等度洗脱，电喷雾正离子（ ESl＋）扫描方式下多反应监测（ MRM）模式对样品进行检测。实验结果表明，金刚烷胺在1.0-50μg/kg范围内线性关系良好，鲜辣椒样品的定量下限为1.0μg/kg，干辣椒及干辣椒制品为5.0μg/kg。鲜辣椒在1.0，2.0，5.0μg/kg加标水平下的回收率为72.2％-98.2％，相对标准偏差（n=6）为1.2％-4.6％；干辣椒及干辣椒制品在5.0，10.0，25.0μg/kg加标水平的回收率为64.2％-81.6％，相对标准偏差（ n=6）为1.3％-6.3％。该方法操作简单、灵敏度高、重现性好，可用于辣椒及辣椒制品中金刚烷胺残留量的检测。A high performance liquid chromatography tandem mass spectrometric（ HPLC-MS/MS ） method was developed for the determination of amantadine residues in pepper and pepper products. After extracted with 1% trichloroacetic acid solution-methanol（ 1 ： 1 ）and purified by an Oasis-MCX SPE cartridge,the samples were sepatated on an Atlantis T3 C18 column（3. 0 μm,2. 1 mm ＆#215; 150 mm）by gradient elution. The electrospray was operated in positive mode and the samples were monitored under the multiple reaction monitoring（ MRM）mode. The calibration curves showed good linearity in the range of 1. 0-50μg/kg. The quantitation limit was 1. 0μg/kg for fresh pepper,and 5. 0 μg/kg for dried pepper and chili products. The recoveries of amantadine in fresh pepper at spiked levels of 1. 0,2. 0,5. 0 μg/kg were 72. 2% -98. 2% ,with relative standard deviations （ RSDs,n=6）of 1. 2% -4. 6% ,and recoveries in dry pepper and chili products at spiked levels at 5. 0,10. 0,25. 0 μg/kg were 64. 2% -81. 6% ,with RSDs（n=6）of 1. 3% -6. 3% . With ad-vantages of simple operation,high sensitivity,good reproducibility,the method could be used for the detection of amantadine residues in the pepper and pepper products.

关 键 词：高效液相色谱-串联质谱 金刚烷胺 辣椒 辣椒制品 

分 类 号：O657.63[理学—分析化学]