萘乙酸残留的高效液相色谱法测定.docVIP

第29卷第4期2010年4月　　　　　　　　　分析测试学报FENX I CESH I XUEBAO (Journal of I nstrumental Analysis 　　　　　　　　　Vol 129No 14382~385 收稿日期:2009-11-13;修回日期:2010-03-09 基金项目:国家水体污染控制与治理科技重大专项资助项目(2008ZX07101-006-05;环保公益资助项目(200809102 第一作者:孔德洋(1977-,男,山东滕州人,助理研究员,博士研究生,Tel:025-********,E -mail:kongdeyang@hot m ail 1com 萘乙酸残留的高效液相色谱法测定 孔德洋1,石利利1,单正军1,葛　峰1,高士祥 2(1.环境保护部南京环境科学研究所,江苏　南京　210042;2.南京大学　环境学院　 污染控制与资源化国家重点实验室,江苏　南京　210093 摘　要:建立了水稻植株及环境样品中萘乙酸的快速分析方法。以二氯甲烷为提取溶剂,对试样进行加速溶 剂萃取,自动凝胶渗透色谱仪净化,高效液相色谱分离,二极管阵列(P DA 检测器测定,外标法定量。萘乙 酸的质量浓度在0105~20100mg/L 范围内与色谱峰面积呈良好的线性关系。萘乙酸在土壤及水稻样品中的检 出限为0105mg/kg,土壤中的添加水平为0105、1100mg/kg 时,回收率为92%、86%,相对标准偏差为 119%、313%;植株中添加水平为0110、1100mg/kg 时,回收率为76%、83%,相对标准偏差为215%、219%。该方法的灵敏度及重复性均符合农药残留分析的要求。关键词:萘乙酸;加速溶剂萃取;凝胶色谱法;农药残留;高效液相色谱 中图分类号:O65717;O6251512　　文献标识码:A 　　文章编号:1004-4957(201004-0382-04 doi:1013969/j 1issn 11004-4957120101041014 Deter m inati on of α2Naphthylacetic Acid by ASE -GPC Coup led with HP LC K ONG De 2yang 1,SH IL i 2li 1,SHAN Zheng 2jun 1,GE Feng 1,G AO Shi 2xiang 2 (1.Nanjing I nstitute of Envir on mental Science,M inistry of Envir on mental Pr otecti on of the Peop le πs Republic of China,Nanjing 　210042,China;2.State Key Laborat ory of Polluti on Contr ol and Res ource Reuse,School of the Envir on ment,Nanjing University,Nanjing 　210093,China Ab s trac t:A rap id detecti on method has been established t o deter m ine the residues of α2naphthylace 2tic acid in rice p lants and the envir onmental sa mp les by high perfor mance liquid chr o mat ography (HP LC in combinati on with accelerated s olvent extracti on (ASE and aut o gel per meati on chr oma 2 t ography (GPC .The sa mp le was extracted by ASE with dichl or omethane as extracti on reagent and cleaning up by aut o GPC .The extract was analyzed by HP LC with phot odi ode array (P DA detect or . The results showed that the calibrati on curve was linear over the concentrati on of α2naphthylacetic acid in the range of 0105-20100mg/L.The li m its of detecti on (LOD s of α2naphthylacetic acid