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作 者:汤晓艳[1] 陈东宇[1] 周剑[1] 毛雪飞[1] 邱静[1] 王敏[1]
机构地区:[1]中国农业科学院农业质量标准与检测技术研究所农业部农产品质量安全重点实验室,北京100081
出 处:《中国食品学报》2014年第9期190-194,共5页Journal of Chinese Institute Of Food Science and Technology
基 金:2014年国家畜禽产品质量安全风险评估项目(GJFP2014007);“十二五”国家科技支撑计划课题(2012BAD28B03);现代农业产业技术体系专项资金资助(CARS-42)
摘 要:采用液相色谱-串联质谱(LC-MS/MS)法检测鸡蛋中金刚烷胺,比较不同类型色谱柱、提取溶液(甲醇-1%三氯乙酸水溶液与甲醇/氨-氯化铵缓冲液)和净化方式(正己烷分配去脂、正己烷/二氯甲烷反萃取及Oasis MCX固相萃取柱净化)。结果显示,用甲醇-1%三氯乙酸水溶液提取,正己烷分配去脂,经Agilent XDB-C18(150 mm×2.1 mm,3.5 m)色谱柱分离,LC-MS/MS检测效果最好。本方法检出限(LOD)为2μg/kg,线性范围在1~1 000μg/L之间,回收率88.0%~99.6%。方法操作简便,实用性强,精密度好,为禽产品的质量安全检测与监管提供方法依据。An analytical method was developed to determine amantadine in fresh eggs by LC-MS/MS. Different chromatographic column, two extraction systems, which were methanol:l% trichloroacetic acid aqueous solution and methanol / ammonia-ammonium chloride buffer, and three purification systems, which were assigned fat by N-hexane, N-hexane / dichloromethane anti-extraction and Oasis MCX solid phase extraction column purification were considered. The optimum condition was achieved by extracted with a mixed solvent of methanol-l% trichloroacetic acid, removing lipids with N- hexane, and separating by Agilent XDB-C18 (150mm×2.1 mm,3.5 m). The linear range wasl-1 000 μg/kg, and the limit of detection was 2 μg/kg. The recoveries ranged from 88.0%-99.6%. The method provides scientific basis for the supervision of poultry eggs safety with simplified operation, good practicability and higher sensitivity.
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