摘要
建立以SPE与GC-MS联用技术测定大豆中11种二硝基苯胺类除草剂(氟乐灵、乙丁氟灵、乙氟灵、环丙氟、氯乙氟灵、二硝胺、氨基丙氟灵、异乐灵、仲丁灵、二甲戊乐灵和磺乐灵)。目标农药经石油醚饱和的乙腈提取,液-液萃取法除去大豆中大部分油脂,再经Florisil柱净化和富集,用5ml乙酸乙酯-正己烷(2:8,V/V)洗脱目标化合物。目标农药采用GC-MS检测,外标法定量。两个添加水平重复6次,回收率范围分别为80%～100%、71%～110%,变异系数小于13%,检测限为0.25～0.32μg/kg,定量限为0.7～0.96μg/kg。
A method using solid phase extraction-gas chromatography-mass spectrometry （SPE-GC-MS） was presented for the determination of dinotroaniline herbicides （trifluralin, benfluralin, ethalfluralin, profluralin, fluchloralin, dinitramine, prodiamine, isopropalin, butralin, pendimethalin and nitralin） in soybean. The procedure was based on extraction of test portions using acetonitrile saturated with petroleum ether, removal of lipid by liquid-liquid extraction method, clean-up and enrichment using a Florisil column with 5 ml of a mixture composed of ethyl acetate and n-hexane （2：8, V/V） as the eluant. The analytes were quantitatively determined using an external calibration method. The average spike recoveries for six replicate determinations at two levels ranged 80% - 100% and 71%- 110%, respectively, with a relative standard deviation （RSD） of less than 13%. This analytical method exhibited a limit of detection （LOD） ranging 0.25-0.32μg/kg and a limit of quantification （LOQ） ranging 0.7 - 0.96 μg/kg.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2009年第20期299-302,共4页
Food Science
