柱前衍生气相色谱测定土壤和糙米中的三乙磷酸铝残留  

Quatification of Fosetyl-Al in Soil and Brown Rice by Gas-chromatogrphy Coupled with Pro-column Derivatization

作　　者：万宇[1] 陶静[1] 王军[1] 王华鼎[1] 蒋闳[1] 

机构地区：[1]安徽省化工研究院,安徽合肥230041

出　　处：《安徽化工》2015年第4期83-85,89,共4页Anhui Chemical Industry

基　　金：农业部农药检定所农药残留登记试验(项目编号:2013F260)

摘　　要：建立了土壤和糙米中三乙磷酸铝残留量的检测方法。采用柱前衍生技术，甲酯化后气相色谱-火焰光度检测器（GC—FPD磷模式）测定土壤和糙米中的三乙磷酸铝残留量。在三乙磷酸铝添加水平为0．01、0．1、1．0mg／kg浓度时，土壤中的回收率为72．6％～98．3％，变异系数为3．88％～8．35％；在三乙磷酸铝添加水平为0．05、0.1、1．0mg／kg浓度时，糙米中的回收率为82．1％～97．6％，变异系数为4．79％～6．52％。三乙磷酸铝在土壤中的最小检出量为0．01ng，最低检测浓度为0．01mg／kg；三乙磷酸铝在糙米中的最小检出量为0．05ng，最低检测浓度为0．05mg/kg.该方法简单、灵敏度高、操作性强、重现性好，可满足农药残留试验准则（NY788—2004）的要求。A method based on pro-column derivatization was developed for determining Fosetyl-Al residue in soil and brown rice. Samples were derivatized by using pro-column derivatization, and determined by gas chromatography - Flame Photometric Detector（GC - FPD P model）. The results indicated that average recoveries for soil at three level（0.01, 0.1 and 1.0 mg/kg） ranged from 72.6%-98.3% with relative standard deviations （RSD） 3.88% - 8.35%; for brown rice at three level （0.05, 0.1 and 1.0 mg/kg） ranged from 82.1% - 97.6% with relative standard deviations（RSD） 4.79% - 6.52%. The LOD of Fosetyl-Al in soil is 0.01 ng, LOQ is 0.01 mg/kg; the LOD of Fosetyl-Al in brown rice is 0.01 ng, LOQ is 0.05 mg/kg. The method is simple , high sensitivity, strong operability with good reproducibility, which could fulfill the requirement of Guideline on pesticide residue trials （NY788-2004）.

关 键 词：柱前衍生 气相色谱 三乙磷酸铝 残留 

分 类 号：O657.71[理学—分析化学]