摘要
建立了动物源性食品中噻酰菌胺残留量的检测方法。样品用乙酸乙酯匀浆提取，上清液采用冷冻过滤和凝胶渗透色谱除杂后，用氨基柱进一步净化，45℃氮吹至近干，用甲醇和去离子水定容。经电喷雾电离，负离子扫描，多反应离子监测模式检测，外标法定量。该方法对噻酰菌胺的定量下限为10μg/kg，线性范围为10．0～100．0μg/L，选用鸡肉、罗非鱼、牛肉、羊肝4种样品进行10、20、50μg/kg3个水平的添加回收实验，回收率为68％～110％，RSD为3．2％～15．2％。该方法可满足动物源性食品中噻酰菌胺残留检测的需要。
A high performance liquid chromatography -tandem mass spectrometric （HPLC -MS/MS） method was established to analyse tiadinil residues in foodstuffs of animal origin. Samples were extrac- ted with ethyl acetate using homogenate extraction technology. The supernatant was cleaned up by freezing lipid filtration and gel permeation chromatography （GPC）, respectively. Then the extract was further cleaned up on a NH2 （aminopropyl） solid phase extraction （SPE） cartridge, condensed to nearly dryness at 45 ℃ water bath, and redissolved with methanol and deionized water. The identification of tiadinil were carried out by MS/MS equipped with electrospray ionization （ESI） in negative scan and multiple reaction monitoring（MRM） mode. The quantification of tiadinil was performed by external standard method. The result indicated that limit of quantification（LOQ） was 10 μg/kg, and a good linearity between the peak area and concentration was obtained in the range of 10. 0 - 100. 0 μg/L. The recoveries of tiadinil from chicken, tilapia, beef and sheep liver sample at three spiked concentration levels of 10, 20, 50 μg/kg were in the range of 68% - 110% with RSDs of 3.2% - 15.2% . The method could meet the requirement for determination of tiadinil residues in foodstuffs of animal origin.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第2期207-210,共4页
Journal of Instrumental Analysis
基金
国家认证认可监督管理委员会资助项目(2007B950)
