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 × 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.
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