柱前衍生-固相萃取／气相色谱法测定油菜、土壤中二氯吡啶酸  

Determination of clopyralid in rape and soil using gas chromatography coupled with pre-column derivatization and solid phase extraction

作　　者：吴祥为[1,2] 花日茂[1] 黄强[1] 唐俊[1] 李学德[1] 汤锋[1] 操海群[1] 

机构地区：[1]安徽农业大学资源与环境学院,安徽省“农产品安全”重点实验室,合肥230036 [2]浙江大学农药环境毒理研究所,杭州310029

出　　处：《分析试验室》2009年第12期35-38,共4页Chinese Journal of Analysis Laboratory

基　　金：国家十一五科技支撑计划(2006BAK02A0403和2007BAD87B06);安徽省十一五科技攻关(08010302166);安徽省教育厅自然科学研究(2006KJ209B)项目资助

摘　　要：采用柱前衍生化法,建立了二氯吡啶酸在油菜植株、菜籽和土壤中的固相萃取-气相色谱测定方法。样品经NaOH溶液提取,乙酸乙酯萃取,甲醇浓硫酸衍生化后,Florsil固相萃取小柱净化,GC-ECD测定。空白油菜植株的平均添加回收率为82.8%～99.1%,RSD为1.0%～11%;菜籽的平均添加回收率为85.0%～94.9%,RSD为2.8%～8.5%;土壤的平均添加回收率为102.3%～109.7%,RSD为3.5%～9.8%。方法的检出限(LOD)为1.87μg/kg,定量限(LOQ)为4.0μg/kg。方法可完全满足农药残留分析要求。A method was developed for pre-column derivatization, solid phase extraction and gas chromatographic determination of clopyralid in rape and soil. Residues of Clopyralid were extracted with 5 g/L solution of soditma hydroxide. The solution was extracted with ethyl acetate. The extract was esterified with methanol in the presence of sulfuric acid. The derivatives were cleaned up with florsil SPE column and analyzed by gas chromatography with electron capture detection. The recoveries of this method in soil, rape, rapeseed were 82.8% -99.1%, 85.0% -94.9% and 102.3%- 109.7%, respectively. The limit of detection （LOD） of elopyralid was 1.87 μg/kg. The limit of quantification of this method was 4.0μg/kg.

关 键 词：二氯吡啶酸 油菜 土壤 固相萃取 残留 

分 类 号：O557.7[理学—热学与物质分子运动论]