固相萃取-高效液相色谱法同时测定大豆和大米中的磺酰脲类和二苯醚类除草剂残留  

Simultaneous Determination of Sulfonylurea and Diphenylether Herbicide Residues in Soybean and Rice by High Performance Liquid Chromatography

作　　者：王和兴[1] 黎源倩[1] 雍莉[1] 谷素英[1] 杨小琪[1] 李磊[1] 

机构地区：[1]四川大学华西公共卫生学院卫生检验学教研室,四川成都610041

出　　处：《色谱》2007年第4期536-540,共5页Chinese Journal of Chromatography

基　　金：卫生部卫生监督司基金课题

摘　　要：建立了大豆和大米中磺酰脲类和二苯醚类除草剂多残留同时检测的高效液相色谱分析方法。样品经乙腈提取,正己烷液-液分配,C18固相萃取小柱净化后,采用高效液相色谱方法分离,以乙腈-三乙胺盐酸溶液作流动相,梯度洗脱,紫外检测器检测。对样品前处理和色谱分析条件进行了优化,8种除草剂（甲磺隆、氯磺隆、苄嘧磺隆、吡嘧磺隆、三氟羧草醚、精恶唑禾草灵、乙氧氟草醚、乙羧氟草醚）在0.05-2.0mg/L范围内线性关系良好。方法的定量限（S/N=10）为0.01-0.02mg/kg,能达到国家有关上述除草剂残留限量的要求。大豆和大米样品的平均加标回收率分别为91.6%-116.1%和76.6%-110.8%,相对标准偏差（RSD）为1.0%-12.2%。所建立的方法在30min内可完成一次检测,具有简便快速、灵敏可靠的特点,适用于大豆和大米中除草剂多残留的测定。A high performance liquid chromatographic （HPLC） method for the simultaneous determination of sulfonylurea herbicide and diphenylether herbicide residues in soybean and rice samples was developed and evaluated. The analytes in soybean and rice samples were extracted with acetonitrile. The extract was cleaned up using an SPE-C18 cartridge, separated and quantitatively determined by reversed-phase HPLC with an ultraviolet detector. The conditions of the pretreatment for soybean and rice samples as well as the parameters of chromatographic separation were optimized. The method had a good linearity in the range of 0.05 - 2.0 mg/L. The quantitative limits （LOQ） of the 8 herbicide residues were 0.01 -0.02 mg/kg. The spiked recoveries were in the range of 91.6% - 116.1% for soybean samples and 76.6% - 110.8% for rice samples with the relative standard deviations of 1.0% - 12.2%. It is concluded that the proposed method is rapid, eight herbicide residues accurate and sensitive and can be used for the determination of the in soybean and rice

关 键 词：高效液相色谱法 固相萃取 除草剂残留 磺酰脲类除草剂 二苯醚类除草剂 大豆 大米 

分 类 号：O658[理学—分析化学]