超声衍生萃取法对土壤中草灭平的分析.docVIP

超声衍生萃取法对土壤中草灭平的分析 　　摘要：以双官能团化合物草灭平为研究对象，采用络合剂Na4-EDTA与其羧基上的氢发生络合反应，络合物极性的降低使得萃取变得简单。再以五氟苄基溴为衍生试剂，利用超声技术在土壤原位上进行动态萃取和衍生。研究证实，Na4-EDTA在水的作用下表现出较强的络合能力，其络合物有较好的稳定性。超声萃取对衍生反应有促进作用，络合反应和衍生反应也存在相互作用。在较宽的范围内（2.5～200.0 μg/kg），响应峰面积与其相应浓度呈现较好的线性关系（R2=0.990）；利用负化学源技术检测，检出限低于0.4 μg/kg；不同浓度的加标回收率为86%～103%；相对标准偏差为5%～10%。方法适用于土壤样品或植物样品中草灭平的检测。 　　关键词：络合反应；超声衍生萃取法；土壤；草灭平 　　中图分类号： O657.7+1 文献标识码：A 文章编号：0439-8114（2014）13-3153-03 　　Determination of Chloramben in Soil by Ultrasonic Assisted Extraction 　　and Derivatization Method 　　LI Ke， ZHANG Li， ZHAO Guo-xing 　　（Institute of Hydrogeology and Environmental Geology， Chinese Academy of Geological Sciences， Zhengding 050803， Hebei， China） 　　Abstract： Chloramben as a bifunctional compound was studied. The carboxyl group reacted with basic complexing agent Na4-EDTA to form a complex compound， so that polar was reduced and extraction was simplified. Derivatization and extraction was acted under ultrasound with pentafluorbenzyl bromide（PFBBr） as derivatization reagent. In the complexation reaction， it was confirmed that Na4-EDTA had good complexing capacity when water was introduced. The complex had good stablity. Ultrasonic assisted extraction promoted the derivatization. Complexation and derivatization interacted each other. Calibration curve showed a good linearity in a the range of 2.5～200.0 μg/kg with correlation coefficients of 0.990.The detection limit was lower than 0.4 μg/kg when negative ion chemical ionization（NCI-MS） was used. The spiked recoveries of different concentrations were 86%～103% with relative standard deviations of 5%～10%. The method proposed could meet the determination of chloramben in samples of soil and plant. 　　Key words： complexation； ultrasonic assisted extraction-derivatization； soil； chloramben 　　草灭平是选择性芽前除草剂，使用较为广泛，由于其移动性较大，容易对水、土造成污染。在草灭平分子结构中，同时含有-COOH和-NH2，其强极性的特点使萃取难度增大，物理萃取方法难以取得好的效果。络合反应后化合物极性的降低可使萃取简单化[1]。目前，多数报道[2， 3]所采用的络合剂多是中性含磷络合剂和酸性含磷络合剂（含有P=O键），如针对羧基或羟基使用的磷酸三丁酯（TBP）、三辛基氧膦（TOPO）和针对氨基