摘要
建立了一种同时检测烟叶中92种农药残留的加速溶剂萃取-液相色谱-串联质谱方法.通过在加速溶剂萃取池底部放置净化剂,将烟叶样品的提取、净化一步完成,之后采用液相色谱-串联质谱（LC-MS/MS）的多反应监测模式（MRM）进行分析.结果表明：①最优实验条件为：提取溶剂乙腈,净化剂4 9弗罗里硅土（florisil）和40 mg石墨化炭黑（GCB）,提取温度120 ℃,提取压力10 MPa（1500 psi）,静态提取时间6 min,冲洗体积50％,静态循环2次.②目标物基质匹配标准曲线线性良好（r2＞0.99）,0.1,0.5和1 mg/kg 3种加标水平的回收率在70％～124％之间,相对标准偏差（RSD）不大于20％.该方法准确度和精密度好,适合用于烟草样品中92种农药残留的检测.
A method combining accelerated solvent extraction （ASE） with liquid chromatography-tandem mass spectrometry （LC-MS/MS） was developed for simultaneously determining 92 pesticide residues in tobacco, which integrated the extraction and purification of tobacco samples into one step by putting adsorbents at the bottom of extraction cell. The extract was analyzed by LC-MS/MS under multi-reaction monitoring （MRM） mode. The results showed that： 1） The optimized extraction conditions were： acetonitrile as extraction solvent, 4 g florisil and 40 mg graphitized carbon black （GCB） as adsorbents, extraction temperature 120 ~C, extraction pressure 10 MPa, static extraction time 6 minutes, flush volume 50% of extraction cell volume, static circulation twice. 2） All matrix-matched calibration curves displayed good linearity （r2 〉 0.99）. The recoveries of standard addition at three levels of 0.1, 0.5, and 1 mg/kg ranged from 70% to 124% with the relative standard deviations （RSDs） no more than 20%. The developed method is accurate, precise, and suitable for the determination of 92 oesticide residues in tobacco.
出处
《烟草科技》
EI
CAS
北大核心
2014年第4期79-87,共9页
Tobacco Science & Technology
