CAJ | 학술논문

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。
건립료고효액상색보-천련질보（ HPLC-MS/MS）측정랄초급랄초제품중금강완알잔류적분석방법。양품채용1％삼록을산용액-갑순（1：1）제취，경Oasis-MCX고상췌취소주정화후용Atlantis T3 C18주진행분리，이0.1％갑산수-을정（85：15）작위류동상진행등도세탈，전분무정리자（ ESl＋）소묘방식하다반응감측（ MRM）모식대양품진행검측。실험결과표명，금강완알재1.0~50μg/kg범위내선성관계량호，선랄초양품적정량하한위1.0μg/kg，간랄초급간랄초제품위5.0μg/kg。선랄초재1.0，2.0，5.0μg/kg가표수평하적회수솔위72.2％~98.2％，상대표준편차（n=6）위1.2％~4.6％；간랄초급간랄초제품재5.0，10.0，25.0μg/kg가표수평적회수솔위64.2％~81.6％，상대표준편차（ n=6）위1.3％~6.3％。해방법조작간단、령민도고、중현성호，가용우랄초급랄초제품중금강완알잔류량적검측。
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.