气相色谱-电子捕获检测器同时测定瓜果类蔬菜中15种除草剂残留  

Simultaneous determination of fifteen herbicides in cucurbitaceous and solanaceous vegetables by gas chromatography with electron caption detector

作　　者：田宏哲[1] 白雪松[1] 苑馨方[1] 杜芳[1] 徐静[2] 

机构地区：[1]沈阳农业大学植物保护学院,沈阳110161 [2]辽宁出入境检验检疫局,辽宁大连116001

出　　处：《农药学学报》2016年第5期625-632,共8页Chinese Journal of Pesticide Science

基　　金：质检公益性行业科研专项(201110207)

摘　　要：采用气相色谱-电子捕获检测器（GC-ECD）法建立了同时测定瓜果类蔬菜中15种除草剂（氟嘧磺隆、草毒死、敌草隆、氯草定、氟乐灵、炔苯酰草胺、乙草胺、甲草胺、异丙甲草胺、吡唑草胺、硝草胺、丁草胺、丙草胺、齅草酮、吡氟酰草胺）残留量的方法。供试番茄、黄瓜、青椒、茄子、西葫芦、马铃薯、芸豆及萝卜8种样品经乙酸乙酯与二氯甲烷混合溶剂提取,Florisil PR固相萃取柱净化,DM-1毛细管气相色谱柱（30 m×0.32 mm,0.25μm）分离,GC-ECD测定,外标法定量。结果表明：在0.002-0.5 mg/kg的3个添加水平下,15种除草剂在8种蔬菜中的平均添加回收率为77%-113%,相对标准偏差（RSD）为3.5%-10.8%,定量限为0.001-0.1 mg/kg。采用所建立的方法对市售蔬菜样品进行测定,结果表明,15种除草剂的残留量均小于最大允许残留限量。该方法简单、快速,灵敏度高,适用于同时测定瓜果类蔬菜样品中15种除草剂的残留量。A gas chromatography-electron caption detector（GC-ECD） method was developed for simultaneous determination of 15 herbcides（primisulfuron,allidochlor,diuron,nitrapyrin,trifluralin,propyzamide,acetochlor,alachlor,metolachlor,metazachlor,pendimethalin,butachlor,pretilachlor,oxadiazon,diflufenican） in cucurbitaceous and solanaceous vegetable samples.The target herbicides were extracted from the test vegetables（tomato,cucumber,pepper,eggplant,courgette,potato,red bean or radish） with ethyl acetate and dichloromethane,purified by Florisil PR solid-phase extraction,separated on a DM-1 capillary column（30 m × 0.32 mm,0.25 μm）,determined by GC-ECD,and quantified by the external standard method.Recoveries of the target herbicides at three spiked concentrations（0.002 mg/kg-0.5 mg/kg） in the tested samples ranged from 77% to 113% with RSDs inthe range of 3.5%-10.8%.The limits of quantitation（LOQ） for the studied herbicides ranged from 0.001 to 0.1 mg/kg.The proposed method was applied in the determination of the selected herbicides residues in samples collected from the local market.The found levels of the target herbicides in vegetable samples were lower than maximum residue levels（MRL）.The method is very simple,fast and highly sensitive.Thus it can be used for the simultaneous determination of the selected herbicides in cucurbitaceous and solanaceous vegetables.

关 键 词：气相色谱-电子捕获检测器 瓜果类蔬菜 除草剂 残留 

分 类 号：S482.4[农业科学—农药学]