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
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%。...
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| Published in | 分析化学 Vol. 39; no. 8; pp. 1238 - 1242 |
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| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
中国地质科学院水文地质环境地质研究所,正定,050803%河北科技大学,石家庄,050018
2011
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| Subjects | |
| Online Access | Get full text |
| ISSN | 0253-3820 |
| DOI | 10.3724/SP.J.1096.2011.01238 |
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| Summary: | 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%。 |
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| Bibliography: | Complexing extraction； In-situ derivatization； Soil； Herbicide； Negative ion chemical ionization 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%. 22-1125/O6 ZHANG Li,GUI Jian-Ye,QI Ji-Xiang,CHEN Zong-Yu,ZHANG Yong-Tao, ZUO Hai-Ying,LI Xiao-Ya,WEI Fu-Xiang,WANG Hao-Ran 1（Institute of Hydro |
| ISSN: | 0253-3820 |
| DOI: | 10.3724/SP.J.1096.2011.01238 |