Supowit Samuel D, Roll Isaac B, Dang Viet D, Kroll Kevin J, Denslow Nancy D, Halden Rolf U
The Biodesign Institute, Center for Environmental Security and Global Security Initiative, 781 E. Terrace Mall, Arizona State University, Tempe, AZ 85287-5904.
Department of Physiological Sciences and Center for Environmental and Human Toxicology, University of Florida, Gainesville, FL 32611.
Sci Rep. 2016 Feb 24;6:21886. doi: 10.1038/srep21886.
We designed and evaluated an active sampling device, using as analytical targets a family of pesticides purported to contribute to honeybee colony collapse disorder. Simultaneous sampling of bulk water and pore water was accomplished using a low-flow, multi-channel pump to deliver water to an array of solid-phase extraction cartridges. Analytes were separated using either liquid or gas chromatography, and analysis was performed using tandem mass spectrometry (MS/MS). Achieved recoveries of fipronil and degradates in water spiked to nominal concentrations of 0.1, 1, and 10 ng/L ranged from 77 ± 12 to 110 ± 18%. Method detection limits (MDLs) were as low as 0.040-0.8 ng/L. Extraction and quantitation of total fiproles at a wastewater-receiving wetland yielded concentrations in surface water and pore water ranging from 9.9 ± 4.6 to 18.1 ± 4.6 ng/L and 9.1 ± 3.0 to 12.6 ± 2.1 ng/L, respectively. Detected concentrations were statistically indistinguishable from those determined by conventional, more laborious techniques (p > 0.2 for the three most abundant fiproles). Aside from offering time-averaged sampling capabilities for two phases simultaneously with picogram-per-liter MDLs, the novel methodology eliminates the need for water and sediment transport via in situ solid phase extraction.
我们设计并评估了一种主动采样装置,将一系列据称导致蜜蜂蜂群崩溃失调的农药作为分析目标。使用低流量多通道泵将水输送到一系列固相萃取柱,实现了对大量水和孔隙水的同时采样。分析物通过液相色谱或气相色谱进行分离,并使用串联质谱(MS/MS)进行分析。在加标至标称浓度为0.1、1和10 ng/L的水中,氟虫腈及其降解产物的回收率为77±12%至110±18%。方法检测限低至0.040 - 0.8 ng/L。在一个接纳废水的湿地中对总氟虫腈进行萃取和定量,地表水和孔隙水中的浓度分别为9.9±4.6至18.1±4.6 ng/L和9.1±3.0至12.6±2.1 ng/L。检测到的浓度与通过传统的、更繁琐的技术测定的浓度在统计学上没有差异(三种最主要的氟虫腈的p值>0.2)。除了能够同时为两个相提供皮克/升检测限的时间平均采样能力外,这种新方法无需通过原位固相萃取进行水和沉积物的运输。