固相萃取-气相色谱-质谱联用检测蔬菜中苄草隆残留及其断裂机理研究

建立了固相萃取-气相色谱-质谱法检测蔬菜中的苄草隆残留的分析方法。样品用乙腈提取,经液液分配,Carb/NH2双层柱净化后过滤膜上机。采用选择离子扫描方式,外标法定量。本方法简便、快速,通过优化前处理和上机条件,在最优条件下进行测试,苄草隆的定量检出限为0.008mg/kg,在加标水平0.01~0.5mg/kg范围内,回收率为98%~122%;相对标准偏差为6.9%~14.2%。对苄草隆的质谱检测断裂机理进行了研究。

Determination of Residual Cumyluron in Vegetable by Solid Phase Extraction with Gas Chromatography/Mass Spectrometry and its Fragmentation Mechanism Study

A method was developed for the determination of residual cumyluron in vegetable by gas chromatography/mass spectrometry(GC/MS).The sample was extracted with acetonitrile,separated with liquid-liquid pa rtition and purified by solid phase extraction(SPE).After investigating the c onditions of pretreatment and determination,the method was convenient and rapid.Under the optimal conditions,the detection limits of cumyluron was 0.008 mg/k g,the recoveries for adding level in the ranges of 0.01-0.5 mg/kg were 98%-12 2%,the relative standard deviations were 6.9%-14.2%.The fragmentation mechani sm of cumyluron was also studied.