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

TY - JOUR

T1 - Suspect screening and quantification of trace organic explosives in wastewater using solid phase extraction and liquid chromatography-high resolution accurate mass spectrometry

AU - Rapp-Wright, Helena

AU - McEneff, Gillian

AU - Murphy, Bronagh

AU - Gamble, Sally

AU - Morgan, Ruth

AU - Beardah, Matthew

AU - Barron, Leon

PY - 2017/5/5

Y1 - 2017/5/5

N2 - 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.

AB - 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.

KW - 2,4-dinitrotoluene

KW - Energetic materials

KW - Micro-pollutants

KW - Sample preparation

KW - Sewage epidemiology

UR - https://www.scopus.com/pages/publications/85010002503

U2 - 10.1016/j.jhazmat.2017.01.008

DO - 10.1016/j.jhazmat.2017.01.008

M3 - Article

SN - 0304-3894

VL - 329

SP - 11

EP - 21

JO - Journal of Hazardous Materials

JF - Journal of Hazardous Materials

ER -