基质分散萃取-高效液相色谱分析大豆植株、籽粒及豆田土壤中咪唑乙烟酸残留  

Residue Analysis Method of Imazethapyr in Soybean Plants,Seed and Soybean Field by QuEChERS-HPLC

作　　者：李广领[1] 董丽红[1] 刘博[1] 郭文举[1] 陈锡岭[1] 

机构地区：[1]河南科技学院,河南新乡453003

出　　处：《大豆科学》2015年第3期480-484,共5页Soybean Science

基　　金：公益性行业(农业)科研专项(201203098);国家级大学生创新训练计划项目(20121046701703);河南省教育厅科学技术研究重点项目(13B210003)

摘　　要：对确立的以甲醇为分散萃取溶剂,乙二胺-N-丙基硅烷（PSA）、十八烷基硅烷键合相（C18）和石墨化碳黑（GCB）为基质分散材料的大豆植株、籽粒及豆田土壤咪唑乙烟酸残留基质分散萃取前处理方法,进行了乙腈等度洗脱的高效液相色谱（HPLC）残留样品外标定量方法条件的优化。结果表明：优化色谱条件下,咪唑乙烟酸的色谱保留时间为6.97 min,在0.01~10.0 mg·L-1质量分数范围内与对应色谱峰积分面积线性响应良好,回归方程为y=4.003 8 x-0.275 6（R2=0.999 5）,回收率均在85%以上,相对标准偏差均小于9%;该色谱条件下仪器检出限为0.104 ng,方法的最低检测浓度分别为0.024（植株）,0.033（籽粒）和0.026 mg·kg-1（豆田土壤）,表明该残留样本前处理方法和样品检测方法简便、高效、经济、可靠,可满足咪唑乙烟在大豆植株、大豆籽粒及豆田土壤中残留定量检测要求。A method based on dispersive solid phase extraction determining Imazethapyr residue in soybean plants,seed and soybean field by HPLC-UVD was developed. The target analysis was quantified by external standard method and matrixmatched standard solution used to compensate for matrix effect. The sample was extracted by methanol and cleaned up by dispersive solid phase extraction using primary secondary amine（ PSA） and C18-bonded silica dispersant sorbent. Under the optimal conditions,the retention time of Imazethapyr was 6. 97 min,the calibration curves showed good linearity（ y = 4. 003 8 x-0. 275 6,R2= 0. 999 5） from 0. 01 to 10. 0 mg·L- 1concentration of Imazethapyr,the average recoveries were determined in soybean plants,soybean and soybean field blank spiked at 0. 05,0. 1 and 0. 5 mg·kg- 1and the overall recovery rates were over 85%,with the relative standard deviations（ RSD） less than 9%. The detection limit of Imazethapyr was 0. 104 ng,and the limit of quantification was 0. 024,0. 033 and 0. 026 mg·kg- 1in soybean plants,seed and soybean field respectively. The results indicated that the sample pretreatment method and the residue sample detection method were simple,good effect,low operation cost,and stable reliability.

关 键 词：咪唑乙烟酸 大豆植株 大豆籽粒 豆田土壤 分散固相萃取 残留分析 

分 类 号：S565.1[农业科学—作物学] S481.8