Liquid chromatography-tandem mass spectrometry determination of synthetic cathinones and phenethylamines in influent wastewater of eight European cities

Richard Bade, Lubertus Bijlsma, Juan V. Sancho, Jose A. Baz-Lomba, Sara Castiglioni, Erika Castrignanò, Ana Causanilles, Emma Gracia-Lor, Barbara Kasprzyk-Hordern, Juliet Kinyua, Ann Kathrin McCall, Alexander L.N. van Nuijs, Christoph Ort, Benedek G. Plósz, Pedram Ramin, Nikolaos I. Rousis, Yeonsuk Ryu, Kevin V. Thomas, Pim de Voogt, Ettore ZuccatoFelix Hernández

Research output: Contribution to journalArticle

Abstract

The popularity of new psychoactive substances (NPS) has grown in recent years, with certain NPS commonly and preferentially consumed even following the introduction of preventative legislation. With the objective to improve the knowledge on the use of NPS, a rapid and very sensitive method was developed for the determination of ten priority NPS (N-ethylcathinone, methylenedioxypyrovalerone (MDPV), methylone, butylone, methedrone, mephedrone, naphyrone, 25-C-NBOMe, 25-I-NBOMe and 25-B-NBOMe) in influent wastewater. Sample clean-up and pre-concentration was made by off-line solid phase extraction (SPE) with Oasis MCX cartridges. Isotopically labelled internal standards were used to correct for matrix effects and potential SPE losses. Following chromatographic separation on a C18column within 6 min, the compounds were measured by tandem mass spectrometry in positive ionization mode. The method was optimised and validated for all compounds. Limits of quantification were evaluated by spiking influent wastewater samples at 1 or 5 ng/L. An investigation into the stability of these compounds in influent wastewater was also performed, showing that, following acidification at pH 2, all compounds were relatively stable for up to 7 days. The method was then applied to influent wastewater samples from eight European countries, in which mephedrone, methylone and MDPV were detected. This work reveals that although NPS use is not as extensive as for classic illicit drugs, the application of a highly sensitive analytical procedure makes their detection in wastewater possible. The developed analytical methodology forms the basis of a subsequent model-based back-calculation of abuse rate in urban areas (i.e. wastewater-based epidemiology).

Original languageEnglish
Pages (from-to)1032-1041
Number of pages10
JournalChemosphere
Volume168
DOIs
Publication statusPublished - Feb 1 2017

Fingerprint

Phenethylamines
Liquid chromatography
Waste Water
Tandem Mass Spectrometry
Liquid Chromatography
Mass spectrometry
liquid chromatography
Wastewater
mass spectrometry
wastewater
Solid Phase Extraction
Epidemiology
Acidification
oasis
Street Drugs
epidemiology
Legislation
Ionization
acidification
cathinone

Keywords

  • Matrix effects
  • New psychoactive substances
  • Stability
  • Triple quadrupole
  • Ultra high-performance liquid chromatography
  • Wastewater

ASJC Scopus subject areas

  • Environmental Chemistry
  • Chemistry(all)

Cite this

Liquid chromatography-tandem mass spectrometry determination of synthetic cathinones and phenethylamines in influent wastewater of eight European cities. / Bade, Richard; Bijlsma, Lubertus; Sancho, Juan V.; Baz-Lomba, Jose A.; Castiglioni, Sara; Castrignanò, Erika; Causanilles, Ana; Gracia-Lor, Emma; Kasprzyk-Hordern, Barbara; Kinyua, Juliet; McCall, Ann Kathrin; van Nuijs, Alexander L.N.; Ort, Christoph; Plósz, Benedek G.; Ramin, Pedram; Rousis, Nikolaos I.; Ryu, Yeonsuk; Thomas, Kevin V.; de Voogt, Pim; Zuccato, Ettore; Hernández, Felix.

In: Chemosphere, Vol. 168, 01.02.2017, p. 1032-1041.

Research output: Contribution to journalArticle

Bade, R, Bijlsma, L, Sancho, JV, Baz-Lomba, JA, Castiglioni, S, Castrignanò, E, Causanilles, A, Gracia-Lor, E, Kasprzyk-Hordern, B, Kinyua, J, McCall, AK, van Nuijs, ALN, Ort, C, Plósz, BG, Ramin, P, Rousis, NI, Ryu, Y, Thomas, KV, de Voogt, P, Zuccato, E & Hernández, F 2017, 'Liquid chromatography-tandem mass spectrometry determination of synthetic cathinones and phenethylamines in influent wastewater of eight European cities', Chemosphere, vol. 168, pp. 1032-1041. https://doi.org/10.1016/j.chemosphere.2016.10.107
Bade, Richard ; Bijlsma, Lubertus ; Sancho, Juan V. ; Baz-Lomba, Jose A. ; Castiglioni, Sara ; Castrignanò, Erika ; Causanilles, Ana ; Gracia-Lor, Emma ; Kasprzyk-Hordern, Barbara ; Kinyua, Juliet ; McCall, Ann Kathrin ; van Nuijs, Alexander L.N. ; Ort, Christoph ; Plósz, Benedek G. ; Ramin, Pedram ; Rousis, Nikolaos I. ; Ryu, Yeonsuk ; Thomas, Kevin V. ; de Voogt, Pim ; Zuccato, Ettore ; Hernández, Felix. / Liquid chromatography-tandem mass spectrometry determination of synthetic cathinones and phenethylamines in influent wastewater of eight European cities. In: Chemosphere. 2017 ; Vol. 168. pp. 1032-1041.
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