PDF(Pubmed)
Abstract：
Pesticides can enter the atmosphere during spraying or after application, resulting in environmental or human exposure. The study describes the optimisation and validation of analytical methods for the determination of more than 300 pesticides in the particulate and gaseous phases of the air. Pesticides were sampled with high-volume air samplers on glass-fibre filters (GFFs) and glass columns filled with polyurethane foam (PUF) and XAD-2 resin. Comparing different extraction methods, a QuEChERS extraction with acetonitrile was selected for the GFFs. For the PUF/XAD-2 columns, a cold-column extraction with dichloromethane was used. Instrumental determination was performed using liquid chromatography/electrospray ionisation-time-of-flight mass spectrometry (LC/ESI-QTOF) and gas chromatography/electron impact ionisation-tandem mass spectrometry (GC/EI-MS/MS). Recovery experiments showed recovery rates between 70 and 120% for 263 compounds on the GFFs and 75 compounds on the PUF/XAD-2 columns. Semi-quantitative determination was performed for 39 compounds on the GFFs and 110 compounds on the PUF/XAD-2 columns. Finally, 27 compounds on the GFFs and 138 compounds on the PUF/XAD-2 columns could be determined only qualitatively. For the determination of the PUF/XAD-2 samples, signal suppression (LC) or signal enhancement (GC) due to matrix effects were determined. Method quantification limits of the optimised methods ranged from 30 to 240 pg/m3 for the target compounds on the GFFs, and from 8 to 60 pg/m3 on the PUF/XAD-2 columns. The applicability of the method was demonstrated by means of environmental air samples from an agricultural area in the Netherlands.
摘要：
农药可以在喷洒过程中或施用后进入大气，导致环境或人类暴露。该研究描述了用于测定空气中颗粒和气相中300多种农药的分析方法的优化和验证。在玻璃纤维过滤器（GRFs）和填充有聚氨酯泡沫（PUF）和XAD-2树脂的玻璃柱上使用大容量空气采样器对农药进行采样。比较不同的提取方法，选择用乙腈进行的QuEChERS萃取用于GFF。对于PUF/XAD-2列，使用二氯甲烷冷柱萃取。使用液相色谱/电喷雾电离-飞行时间质谱(LC/ESI-QTOF)和气相色谱/电子碰撞电离-串联质谱(GC/EI-MS/MS)进行仪器测定。回收实验表明，对于GFF上的263种化合物和PUF/XAD-2柱上的75种化合物，回收率在70％至120％之间。对GFF上的39种化合物和PUF/XAD-2柱上的110种化合物进行半定量测定。最后,GFF上的27个化合物和PUF/XAD-2柱上的138个化合物只能定性地测定。对于PUF/XAD-2样品的测定，确定了由于基体效应引起的信号抑制(LC)或信号增强(GC)。优化方法的方法定量限范围为GFF上目标化合物的30至240pg/m3，在PUF/XAD-2柱上为8至60pg/m3。通过荷兰农业区的环境空气样本证明了该方法的适用性。
