GCMS研究茶叶中拟除虫菊酯类农药残留的提取方法.docVIP

收稿日期:2007208227; 修回日期:2007211220 作者简介:王　翔(1983～ , 男(汉族 , 江苏泰兴人, 硕士研究生。E 2mail :062037001@fudan. edu. cn 通信作者:胡耀铭(1965～ , 男(汉族 , 上海人, 高级工程师, 从事色谱质谱分析研究。E 2mail :ymhu @fudan. edu. cn 第29卷第2期 2008年3月 质谱学报 Journal of Chinese Mass Spectrometry Society Vol. 29　No. 2Mar. 2008 G C/MS 王　翔, (, 摘要:, 比较了加水浸泡对农残提取的影响。结果表明, , 通过对样品净化淋洗剂种类和体积的优化选择, 总结出一套简。, 直接用50mL V (丙酮 ∶V (正己烷 =1∶1的溶液超声提取, 提取液过活性炭柱, 浓缩后再过Florisil 柱, 用15mL V (正己烷 ∶V (乙酸乙酯 =2∶1的溶液淋洗, 浓缩后用 GC/MS 法测定。回收率为81%～120%,RSD 为2. 2%～7. 8%, 检测限为0. 002～0. 01mg ?kg -1。 关键词:拟除虫菊酯; 农药残留; 茶叶; 提取方法; GC/MS 中图分类号:O657. 63　　文献标识码:A　　文章编号:100422997(2008Study on Extraction of Pyrethroid Pesticide Multi 2R esidues in T ea by G C/MS WAN G Xiang , SON G Guo 2xin , HU Yao 2ming (T he Research Center of A nal ysis and Measurement , Fudan Universit y , S hanghai 200433, China Abstract :The factors of ext racting pyret hroid pesticide multi 2residues f rom tea were st ud 2ied , especially for t he influence of adding water into samples before organic solvent s ext rac 2tion. Result s show t hat higher ext racting efficiency is acquired wit hout adding water. A simple and accurate pret reat ment for pyret hroids in tea is reached by optimizing t he choices and volumes of eluting solvent s. The samples wit hout water immersing were ext racted by 50mL of V (hexane ∶V (acetone =1∶1, followed by cleaning up wit h columns of activa 2ted carbon and Florisil respectively. 15mL of V (hexane ∶V (et hyl acetate =2∶1was employed to elute t he Florisil column , t hen was determined by GC/MS. The recoveries range f rom 81%to 120%, RSDs are 2. 2%27. 8%, and t he limit s of detection are 0. 00220. 01mg ?kg -1. K ey w ords :pyret hroid ; pesticide residue ; tea ; extraction met hod ; GC/MS 　　拟除虫菊酯类农药因具有广谱、高效、低毒的优点, 被广泛用于茶叶生产中的害虫防治, 但如果使用不当造成茶产品中的农药高残留会严 重威胁人类健康, 并直接影响我国茶产品的出口, 对此已引起相关方面的高度重视。特别是2006年5月, 日本实施的“肯定列表制度”将茶 叶的农残限量指标从83项增加到276项, 因此 茶叶中的农残检测是当前的一个研究热点。 正确的样品前处理是进行茶叶中农残检测的关键, 而样品提取率的高低直接影响到检测方法的准确性。楼国柱等[123]比较了单一和混合溶剂对茶叶农残提取的影响, 认为用V (丙酮 ∶V