基质固相分散萃取-分散液相微萃取-气相色谱质谱法测定土壤中拟除虫菊酯类农药

建立了基质固相分散萃取-分散液相微萃取-气相色谱质谱法测定土壤中3种拟除虫菊酯农药（胺菊酯、氯菊酯、溴氰菊酯）的分析方法。最佳前处理条件为：0.5 g样品与1.5 g C18固相萃取粉末研磨5 min,混合物以10 mL丙酮洗脱并浓缩至0.4 mL,加入20μL四氯化碳和5 mL超纯水形成乳化,离心破乳后吸取1μL沉积相进GC-MS分析。3种拟除虫菊酯类农药在5～200μg/kg范围内有良好的线性关系（r^2≥0.9989）,平均加标回收率为86.5%～108.0%,相对标准偏差小于7.8%（n=3）,检出限为1.00～1.48μg/kg,可满足土壤中微量拟除虫菊酯类农药的分析。...

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Published in分析化学 Vol. 43; no. 1; pp. 137 - 140
Main Author 成昊 张丽君 张磊 张占恩
Format Journal Article
LanguageChinese
Published 苏州科技学院环境科学与工程学院,苏州,215009%江苏省环境科学与工程重点实验室,苏州,215009%苏州科技学院环境科学与工程学院，苏州215009 2015
江苏省环境科学与工程重点实验室，苏州215009
Subjects
分散液相微萃取
土壤
基质固相分散萃取
拟除虫菊酯
气相色谱质谱
气相色谱质谱
Dispersive liquid_1 iquid microextraction
拟除虫菊酯
Matrix solid phase dispersion extraction
基质固相分散萃取
Pyrethroids
Soil
分散液相微萃取
Gas chromatography_mass spectrometry
土壤
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Summary:建立了基质固相分散萃取-分散液相微萃取-气相色谱质谱法测定土壤中3种拟除虫菊酯农药（胺菊酯、氯菊酯、溴氰菊酯）的分析方法。最佳前处理条件为：0.5 g样品与1.5 g C18固相萃取粉末研磨5 min,混合物以10 mL丙酮洗脱并浓缩至0.4 mL,加入20μL四氯化碳和5 mL超纯水形成乳化,离心破乳后吸取1μL沉积相进GC-MS分析。3种拟除虫菊酯类农药在5～200μg/kg范围内有良好的线性关系（r^2≥0.9989）,平均加标回收率为86.5%～108.0%,相对标准偏差小于7.8%（n=3）,检出限为1.00～1.48μg/kg,可满足土壤中微量拟除虫菊酯类农药的分析。
Bibliography:CHENG Hao, ZHANG Li-Jun , ZHANG Lei, ZHANG Zhan-En （1School of Environmental Science and Engineering, Suzhou University of Science and Technology, Suzhou 215009, China; 2 Key Laboratory of Environmental Science and Engineering of Jiangsu Province, Suzhou 215009, China）
A matrix solid phase dispersion extraction-dispersed liquid phase microextraction-gas chromatography-mass spectrometric method has been developed for the determination of three pyrethroids （tetramethrin, permethrin and deltamethrin） in soil. The optimal conditions for the analysis were as follows. About 0.5 g soil and 1.5 g C18 solid phase extraction powder were grinding for 5 min. The mixture was eluted with 10 mL of acetone. The eluent was concentrated to 0. 4 mL, and then mixed with 20 μL of tetrachloromethane and 5.0 mL of ultrapure water to form a homogeneous cloudy solution. The emulsion was broken by centrifugation. About 1 μL of sediment was injected and analyzed direetly by GC-MS. Good linearities for three pyrethroids were ranged from
ISSN:0253-3820
DOI:10.11895/j.issn.0253_3820.140549