Liquid chromatography-tandem mass spectrometry determination of synthetic cathinones and phenethylamines in influent wastewater of eight European cities.
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).
Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain.
Richard
R
Bade
Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain.
Lubertus
L
Bijlsma
Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain.
Juan V
JV
Sancho
Norwegian Institute for Water Research (NIVA), Gaustadalléen 21, 0349 Oslo, Norway; Faculty of Medicine, University of Oslo, PO Box 1078, Blindern, 0316 Oslo, Norway.
Jose A
JA
Baz-Lomba
IRCCS-Istituto di Ricerche Farmacologiche "Mario Negri", Department of Environmental Health Sciences, Via La Masa 19, 20156 Milan, Italy.
Sara
S
Castiglioni
University of Bath, Department of Chemistry, Faculty of Science, Bath BA2 7AY, UK.
Erika
E
Castrignanò
KWR Watercycle Research Institute, Chemical Water Quality and Health, P.O. Box 1072, 3430 BB Nieuwegein, The Netherlands.
Ana
A
Causanilles
Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain; IRCCS-Istituto di Ricerche Farmacologiche "Mario Negri", Department of Environmental Health Sciences, Via La Masa 19, 20156 Milan, Italy.
Emma
E
Gracia-Lor
University of Bath, Department of Chemistry, Faculty of Science, Bath BA2 7AY, UK.
Barbara
B
Kasprzyk-Hordern
Toxicological Center, Department of Pharmaceutical Sciences, Campus Drie Eiken, University of Antwerp, Universiteitsplein 1, 2610 Antwerp, Belgium.
Juliet
J
Kinyua
Eawag, Swiss Federal Institute of Aquatic Science and Technology, CH-8600 Dübendorf, Switzerland.
Ann-Kathrin
AK
McCall
Toxicological Center, Department of Pharmaceutical Sciences, Campus Drie Eiken, University of Antwerp, Universiteitsplein 1, 2610 Antwerp, Belgium.
Alexander L N
ALN
van Nuijs
Eawag, Swiss Federal Institute of Aquatic Science and Technology, CH-8600 Dübendorf, Switzerland.
Christoph
C
Ort
Department of Environmental Engineering, Technical University of Denmark, Miljøvej, Building 115, DK-2800 Kgs. Lyngby, Denmark.
Benedek G
BG
Plósz
Department of Environmental Engineering, Technical University of Denmark, Miljøvej, Building 115, DK-2800 Kgs. Lyngby, Denmark.
Pedram
P
Ramin
IRCCS-Istituto di Ricerche Farmacologiche "Mario Negri", Department of Environmental Health Sciences, Via La Masa 19, 20156 Milan, Italy.
Nikolaos I
NI
Rousis
Norwegian Institute for Water Research (NIVA), Gaustadalléen 21, 0349 Oslo, Norway; Faculty of Medicine, University of Oslo, PO Box 1078, Blindern, 0316 Oslo, Norway.
Yeonsuk
Y
Ryu
Norwegian Institute for Water Research (NIVA), Gaustadalléen 21, 0349 Oslo, Norway.
Kevin V
KV
Thomas
KWR Watercycle Research Institute, Chemical Water Quality and Health, P.O. Box 1072, 3430 BB Nieuwegein, The Netherlands; Institute for Biodiversity and Ecosystem Dynamics, University of Amsterdam, P.O. Box 94248, 1090 GE Amsterdam, The Netherlands.
Pim
P
de Voogt
IRCCS-Istituto di Ricerche Farmacologiche "Mario Negri", Department of Environmental Health Sciences, Via La Masa 19, 20156 Milan, Italy.
Ettore
E
Zuccato
Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain. Electronic address: felix.hernandez@uji.es.
Félix
F
Hernández
D000470:Alkaloids / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods; D002947:Cities; D004784:Environmental Monitoring; D005060:Europe; D013287:Illicit Drugs / Q000032:analysis*; D010627:Phenethylamines / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods; D062065:Wastewater / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D000470:Alkaloids; D013287:Illicit Drugs; D010627:Phenethylamines; D062065:Wastewater; D014874:Water Pollutants, Chemical; C023665:cathinone
Matrix effects; New psychoactive substances; Stability; Triple quadrupole; Ultra high-performance liquid chromatography; Wastewater