固相萃取-液相色谱法测定水果中的氨基甲酸酯与有机磷农药  

Determination of carbamates and organophosporus pesticides in vegetables and fruits by solid-phase extraction and high performance liquid chromatography

作　　者：邹力[1] 同帜[1] 董祥芝[1] 

机构地区：[1]西安工程大学环境与化学工程学院,陕西西安710048

出　　处：《纺织高校基础科学学报》2011年第4期563-567,共5页Basic Sciences Journal of Textile Universities

基　　金：陕西省科技厅工业攻关项目(2009K06-27)

摘　　要：建立了固相萃取-高效液相色谱同时测定水果中4种氨基甲酸酯与一种有机磷的方法.对提取溶剂、固相萃取柱种类、洗脱剂类型和用量及检测的色谱条件进行筛选和优化.样品经乙腈超声提取,弗罗里硅土固相萃取柱净化,净化后的样品采用液相色谱柱分离,以甲醇:水(体积比70∶30)为流动相,紫外检测波长为210nm,流速1.0mL/min.结果表明,5种农药在0～20μg/mL内具有良好线性,检出限为0.004～0.29μg/mL,样品的加标平均回收率为62%～91%,相对标准偏差为4.1%～11.3%(n=6).该方法可用于水果中衡量氨基甲酸酯与有机磷农药残留的测定.A solid phase extraction-high performance liquid chromatographic method for the determination of carbamates and organophosphorus pesticides in vegetables is developed in this study.The analysis conditions for the extraction solvent,SPE columns,elution solvent and separation of samples were optimized.The analytical procedure involved in ultrasonic extraction with acetonitrile,purification using a Florisil SPE column.The separation procedure of the cleaned samples depend on a liquid chromatography column.The mobile phase was methanol：water（V：V,70：30） at a total flow rate of 1.0 mL/min and the ultraviolet wavelength was 210 nm.The linear ranges of the five pesticides were 0-20.0 μg/mL with the detecting limit 0.004-0.29 μg/mL.The average recoveries ranged from 62% to 91% with the relative standard.deviations were 4.1%-11.3%（n=6）.The results indicated that the method was suitable for the determination of trace carbamate and organophosporus pesticides in fruits.

关 键 词：固相萃取 高效液相色谱 氨基甲酸酯农药 有机磷农药 

分 类 号：O657.7[理学—分析化学]