Hildebrandt Alain, Lacorte Sílvia, Barceló Damià
Department of Environmental Chemistry, IIQAB - CSIC, Jordi Girona 18-26, 08034 Barcelona, Spain.
Anal Bioanal Chem. 2007 Feb;387(4):1459-68. doi: 10.1007/s00216-006-1015-z. Epub 2007 Jan 9.
Gas chromatography-mass spectrometry (GC/MS) was employed for the determination of 30 widely used pesticides including various transformation products and alkylphenols in water and agricultural soils with the aim of assessing the impact of these compounds in agricultural soils and the underlying aquifer. The extraction, clean-up, and analytical procedures were optimized for both water and soil samples to provide a highly robust method capable of determining target analytes at the ppb-ppt level with high precision. For water samples, different solid-phase extraction cartridges and conditions were optimized; similarly, pressurized liquid extraction conditions were tested to provide interference-free extracts and high sensitivity. Instrumental LODs of 3-4 pg were obtained. The multi-residue extraction procedures were applied to the analysis of groundwaters and agricultural soils from the Ebro river basin (NE Spain). Most ubiquitous herbicides detected were triazines but some acetanilides and organophosphorus pesticides were also found; the pesticide additive tributylphosphate was found in all water samples. Levels varied between 0.57 and 5.37 microg/L in groundwater, whereas nonylphenol was the sole compound detected in soil. Alkylphenols are used as adjuvants in pesticide formulations and are present in sludges employed as soil fertilizers. Occurrence was found to be similar to other environmental studies.
采用气相色谱 - 质谱联用(GC/MS)法测定水和农业土壤中30种广泛使用的农药,包括各种转化产物和烷基酚,旨在评估这些化合物对农业土壤及下层含水层的影响。针对水和土壤样品,对萃取、净化及分析程序进行了优化,以提供一种高度稳健的方法,能够高精度地测定ppb - ppt水平的目标分析物。对于水样,对不同的固相萃取柱和条件进行了优化;同样,对加压液体萃取条件进行了测试,以提供无干扰的提取物和高灵敏度。获得了3 - 4 pg的仪器检测限。将多残留萃取程序应用于埃布罗河流域(西班牙东北部)地下水和农业土壤的分析。检测到的最普遍的除草剂是三嗪类,但也发现了一些乙酰苯胺类和有机磷农药;在所有水样中均发现了农药添加剂磷酸三丁酯。地下水中的含量在0.57至5.37 μg/L之间变化,而壬基酚是在土壤中检测到的唯一化合物。烷基酚用作农药配方中的助剂,存在于用作土壤肥料的污泥中。其出现情况与其他环境研究相似。