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Suspect screening and quantification of trace organic explosives in wastewater using solid phase extraction and liquid chromatography-high resolution accurate mass spectrometry

Research output: Contribution to journalArticlepeer-review

Helena Rapp-Wright, Gillian McEneff, Bronagh Murphy, Sally Gamble, Ruth Morgan, Matthew Beardah, Leon Barron

Original languageEnglish
Pages (from-to)11-21
Number of pages11
JournalJournal of Hazardous Materials
Volume329
Early online date6 Jan 2017
DOIs
Accepted/In press4 Jan 2017
E-pub ahead of print6 Jan 2017
Published5 May 2017

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Abstract

The first comprehensive assessment of 34 solid phase extraction sorbents is presented for organic explosive residues in wastewater prior to analysis with liquid chromatography-high resolution accurate mass spectrometry (LC-HRMS). A total of 18 explosives were selected including nitramines, nitrate esters, nitroaromatics and organic peroxides. Three polymeric divinylbenzene-based sorbents were found to be most suitable and one co-polymerised with n-vinyl pyrrolidone offered satisfactory recoveries for 14 compounds in fortified wastewater (77–124%). Limits of detection in matrix ranged from 0.026–23 μg L−1 with R2 ≥ 0.98 for most compounds. The method was applied to eight 24-h composite wastewater samples from a London wastewater works and one compound, 2,4-dinitrotoluene, was determined over five days between 332 and 468 g day−1 (225–303 ng L−1). To further exploit the suspect screening capability, 17 additional explosives, precursors and transformation products were screened in spiked wastewater samples. Of these, 14 were detected with recoveries from 62 to 92%, highlighting the broad applicability of the method. To our knowledge, this represents the first screen of explosives-related compounds in wastewater from a major European city. This method also allows post-analysis detection of new or emerging compounds using full-scan HRMS datasets to potentially identify and locate illegal manufacture of explosives via wastewater analysis.

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