烟草科技2017，Vol.50Issue(10)：62-68,7.
同位素内标-UPLC-MS/MS法测定烟草中的9种常见农药残留
Simultaneous determination of nine pesticide residues in tobacco by UPLC-MS/MS with isotope-labeled internal standard
杨飞 1邓惠敏 1边照阳 1李中皓 1王颖 1刘珊珊 1范子彦 1唐纲岭1
作者信息
- 1. 国家烟草质量监督检验中心,郑州高新技术产业开发区枫杨街2号450001
- 折叠
摘要
Abstract
A rapid method combining ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)with isotope dilution technique was developed for determining nine pesticide residues in tobacco. The analytes were extracted from tobacco samples by acetonitrile and purified by dispersion solid phase extraction with N-propyldiaminoethane as the sorbent, then qualitatively and quantitatively analyzed by a tandem mass spectrometer in multiple reaction monitoring(MRM)mode after being separated on BEH C18 column. The pesticide residues were quantitatively analyzed with the corresponding deuteriums as the internal standards separately. The results showed that: 1)Good linear relation was obtained in the range of 12.5-500 ng/mL for nine pesticides with r >0.998. 2)The limits of qualification and limits of quantification for nine pesticides were 0.003-0.009 and 0.011-0.030 mg/kg. The average standard recoveries obtained for control samples ranged from 85.5% to 110.1% with the relative standard deviations less than 6.0%. 3)After determining 30 real samples by this method, it was found that the results of the isotope internal standard method were in good agreement with that of the blank matrix matching standard calibration method, but the operation is simpler. This method has been applied for the analysis of nine pesticides in flue-cured tobacco, burley tobacco, oriental tobacco and tobacco products and found to be suitable.关键词
烟草/同位素内标/超高效液相色谱-串联质谱(UPLC-MS/MS)/农药残留Key words
Tobacco/Isotope-labeled internal standard/Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)/Pesticide residue分类
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杨飞,邓惠敏,边照阳,李中皓,王颖,刘珊珊,范子彦,唐纲岭..同位素内标-UPLC-MS/MS法测定烟草中的9种常见农药残留[J].烟草科技,2017,50(10):62-68,7.
