络合萃取-在线衍生气相色谱-质谱法检测土壤中酸性除草剂  

Determination of Acidic Herbicide in Soil by Complexing Extraction-In Situ Derivatization

作　　者：张莉[1] 桂建业[1] 齐继祥[1] 陈宗宇[1] 张永涛[1] 左海英[1] 李晓亚[1] 魏福祥[2] 王浩然[2] 

机构地区：[1]中国地质科学院水文地质环境地质研究所,正定050803 [2]河北科技大学,石家庄050018

出　　处：《分析化学》2011年第8期1238-1242,共5页Chinese Journal of Analytical Chemistry

基　　金：中国地质科学院基本科研业务费(No.Q201017);中国地质科学院水文地质环境地质研究所基本科研业务费(No.SK2010008)资助

摘　　要：以Na4-EDTA为络合剂、五氟苄基溴为衍生试剂,对土壤中酸性除草剂进行在线衍生络合萃取,采用负化学源质谱技术对衍生产物实现了快速、高灵敏检测。将10.0g土壤样品、1.5mL蒸馏水、0.50g Na4-EDTA充分混合,加入过量衍生试剂,采用加速溶剂萃取仪,样品在100℃,10.3MPa压力下,10min完成衍生及萃取过程,萃取液脱水并净化后进行检测。本方法在10～500μg/kg范围内线性关系较好,相关系数r2>0.990。方法的检出限为0.8～7.7μg/kg;回收率为70%～130%;精密度2.0%～8.0%。A rapid and sensitive method for the detection of acidic herbicides in soil was developed by in-situ derivatization complexing extraction with Na4-EDTA as complexing reagent and pentafluorobenzyl bromide（PFBBr） as derivatization reagent combining with GC-negative ion chemical ionization（NCI）-MS.On the basis of sufficient mixture of 10.0 g soil,1.5 mL H2O,and 0.5 g Na4-EDTA,the derivatization and extraction was completed in 10 min,with elevated temperature（100 ℃） and pressure（10.3 MPa） by accelerated solvent extractor（ASE） with excessive PFBBr in the extraction cell.The extract was detected after drying and clean-up.The correlation coefficient（r2） 〉 0.990 in the samples concentration of 10-500 μg/kg,the MDL was 0.8-7.7 μg/kg,the recovery was 70%-130%,and the RSD was 2.0%-8.0%.

关 键 词：络合萃取 在线衍生 土壤 除草剂 负化学源质谱 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]