摘要
首次建立了蔬菜中常见基质干扰物的净化方法。用GC-MS分析样品提取液、确定了蔬菜农药多残留检测常见的基质干扰物。建立常见吸附剂对基质干扰物的吸附模型，以及吸附剂对农药的吸附模型。据此建立了番茄、油菜和尖椒3种蔬菜中102种农药多残留SPE净化方法和气相色谱-质谱／选择离子存储检测方法（gas chromatography - ion trap mass spectrometry/selective ion storage, GC - MS/SIS）。样品用凝胶渗透色谱（GPC）去除大分子干扰物和部分色素和（或）采用石墨化碳黑（GCB）＋Florisil混合SPE柱去除色素和脂肪酸。在0．02mg／kg和0．10mg／kg两个水平，农药添加回收率为65％-123％（除久效磷、抗蚜威和蝇毒磷），RSD不大于15％。方法检出限在2～30μg/kg范围。对于其它蔬菜，只要确定样品中的基质干扰物，即可选择合适的吸附剂制备专用的SPE柱。该方法适用于含色素、脂肪酸和大分子干扰物蔬菜样品中的农药多残留分析。
The paper reports the development of special solid-phase extraction（SPE） tube for different co-extractions and a rapid multiresidue screen method for pesticides in vegetables based on gas chromatography - ion trap mass spectrometry/selective ion storage （ GC - MS/SIS）. Firstly, the extractions of 10 vegetables were compared, the main co-extractions of vegetables were confirmed. The set up of the SPE method for interferances were graphitized carbon black（GCB） for pigment, Florisil or NH2 for fatty acids and gel permeation chromatography（GPC） for macromolecule interferance. Finally, a multiresidue determination method for multi class pesticide in tomato, cole and capsicum was developed. All compounds were determined by GC - MS/SIS. Samples were spiked at 0. 02 mg/kg and 0. 10 mg/kg, the average recoveries were in the range of 65% - 123% （ except monocrotophos, coumaphos and pirimicarb） with RSD no more than 15% The LODs of this method were between 2 μg/kg and 30 μg/kg for all pesticides. This method is suitable for all vegetables, which contain pigment, fatty acid and co-extraction of macromolecules.
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第8期795-799,共5页
Journal of Instrumental Analysis
基金
“十五”科技攻关重大项目资助(2004BA210A04)
