超声衍生萃取法对土壤中草灭平的分析  被引量:1

Determination of Chloramben in Soil by Ultrasonic Assisted Extraction and Derivatization Method

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作  者:李科[1] 张莉[1] 赵国兴[1] 

机构地区:[1]中国地质科学院水文地质环境地质研究所,河北正定050803

出  处:《湖北农业科学》2014年第13期3153-3155,共3页Hubei Agricultural Sciences

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(R^2=0.990);利用负化学源技术检测,检出限低于0.4μg/lkg;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.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.

关 键 词:络合反应 超声衍生萃取法 土壤 草灭平 

分 类 号:O657.71[理学—分析化学]

 

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