Arid
DOI10.1016/j.forsciint.2017.12.018
Development and validation of a solid phase extraction sample cleanup procedure for the recovery of trace levels of nitro-organic explosives in soil
Thomas, Jennifer L.1; Donnelly, Christopher C.1; Lloyd, Erin W.1; Mothershead, Robert F., II2; Miller, Mark L.3
通讯作者Miller, Mark L.
来源期刊FORENSIC SCIENCE INTERNATIONAL
ISSN0379-0738
EISSN1872-6283
出版年2018
卷号284页码:65-77
英文摘要

An improved cleanup method has been developed for the recovery of trace levels of 12 nitro-organic explosives in soil, which is important not only for the forensic community, but also has environmental implications. A wide variety of explosives or explosive-related compounds were evaluated, including nitramines, nitrate esters, nitroaromatics, and a nitroalkane. Fortified soil samples were extracted with acetone, processed via solid phase extraction (SPE), and then analyzed by gas chromatography with electron capture detection. The following three SPE sorbents in cartridge format were compared: Empore (TM) SDB-XC, Oasis (R) HLB, and Bond Elut NEXUS cartridges. The NEXUS cartridges provided the best overall recoveries for the 12 explosives in potting soil (average 48%) and the fastest processing times (<30 min). It also rejected matrix components from spent motor oil on potting soil. The SPE method was validated by assessing limit of detection (LOD), processed sample stability, and interferences. All 12 compounds were detectable at 0.02 mu g explosive/gram of soil or lower in the three matrices tested (potting soil, sand, and loam) over three days. Seven explosives were stable up to seven days at 2 mu g/g and three were stable at 0.2 mu g/g, both in processed loam, which was the most challenging matrix. In the interference study, five interferences above the determined LOD for soil were detected in matrices collected across the United States and in purchased all-purpose sand, potting soil, and loam. This represented a 3.2% false positive rate for the 13 matrices processed by the screening method for interferences. The reported SPE cleanup method provides a fast and simple extraction process for separating organic explosives from matrix components, facilitating sample throughput and reducing instrument maintenance. In addition, a comparison study of the validated SPE method versus conventional syringe filtration was completed and highlighted the benefits of sample cleanup for removing matrix interferences, while also providing lower supply cost, order of magnitude lower LODs for most explosives, higher percent recoveries for complex matrices, and fewer instrument maintenance issues. Published by Elsevier Ireland Ltd.


英文关键词Organic explosives Soil Cleanup Solid phase extraction Gas chromatography Electron capture detection
类型Article
语种英语
国家USA
收录类别SCI-E
WOS记录号WOS:000425880700009
WOS类目Medicine, Legal
WOS研究方向Legal Medicine
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/209322
作者单位1.Fed Bur Invest, Counterterrorism & Forens Sci Res Unit, Visiting Scientist Program, Fed Bur Invest Lab Div, 2501 Invest Pkwy, Quantico, VA USA;
2.Fed Bur Invest, Explos Unit, Fed Bur Invest Lab Div, 2501 Invest Pkwy, Quantico, VA USA;
3.Fed Bur Invest, Counterterrorism & Forens Sci Res Unit, Fed Bur Invest Lab Div, 2501 Invest Pkwy, Quantico, VA 22135 USA
推荐引用方式
GB/T 7714
Thomas, Jennifer L.,Donnelly, Christopher C.,Lloyd, Erin W.,et al. Development and validation of a solid phase extraction sample cleanup procedure for the recovery of trace levels of nitro-organic explosives in soil[J],2018,284:65-77.
APA Thomas, Jennifer L.,Donnelly, Christopher C.,Lloyd, Erin W.,Mothershead, Robert F., II,&Miller, Mark L..(2018).Development and validation of a solid phase extraction sample cleanup procedure for the recovery of trace levels of nitro-organic explosives in soil.FORENSIC SCIENCE INTERNATIONAL,284,65-77.
MLA Thomas, Jennifer L.,et al."Development and validation of a solid phase extraction sample cleanup procedure for the recovery of trace levels of nitro-organic explosives in soil".FORENSIC SCIENCE INTERNATIONAL 284(2018):65-77.
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