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柱前衍生-气相色谱法测定柑橘中2,4-D残留量研究初报
Determination of 2,4-Dichlorophenoxyacetic Acid Residue in Orange by GC with Pre-column Derivatization
【摘要】 为了解决柑橘出口中2,4-D残留监测问题,研究了快速测定柑橘中2,4-D残留方法。样品经酸性乙腈提取,用酸性硅藻土净化,经三甲基氢氧化硫(TMSH)衍生后,用带电子捕获检测器的气相色谱仪进行测定。试验结果表明:2,4-D的最低检出量为5×10-13g,最低检出浓度为4×10-4mg/kg,在0.001、0.01、0.1mg/kg三种添加水平下,添加回收率范围为77.16%~97.72%,变异系数范围为3.30%~8.65%。该分析方法快速、准确、灵敏,重现性好,适用于柑橘中2,4-D残留量的检测。
【Abstract】 For effective detecting of 2,4-Dichlorophenoxyacetic Acid (2,4-D) residue in orange fruit,a quick analytical method was developed.After extracted by acidic acetonitrile,the filtrate was purified by acid diatomite.The target compound in sample was derivatised by Trimethylsulfonium Hydroxide (TMSH),and then determined by GC-ECD.The results suggested that the lowest detection limit for 2,4-D was 5×10-13g,and the limit of quantification was 4×10-4mg/kg.The recoveries of 2,4-D from orange spiked with 0.001,0.01,0.1mg/kg ranged from 77.16 to 92.72%,with the coefficient of variation of 3.30% to 8.65%.This method is fast,accurate,sensitive,and with good reproducibility.It can be used to determinate 2,4-D in orange fruit.
【Key words】 2; 4-D; Orange fruit; Acid diatomite; Pre-column derivatization; Residue analysis;
- 【文献出处】 中国农学通报 ,Chinese Agricultural Science Bulletin , 编辑部邮箱 ,2006年10期
- 【分类号】TS255.7
- 【被引频次】23
- 【下载频次】182