TY - JOUR

T1 - Sewage-based epidemiology in monitoring the use of new psychoactive substances

T2 - Validation and application of an analytical method using LC-MS/MS

AU - Kinyua, Juliet

AU - Covaci, Adrian

AU - Maho, Walid

AU - Mccall, Ann Kathrin

AU - Neels, Hugo

AU - van Nuijs, Alexander L.N.

N1 - Publisher Copyright: © 2015 John Wiley & Sons, Ltd.

PY - 2015/9/1

Y1 - 2015/9/1

N2 - Sewage-based epidemiology (SBE) employs the analysis of sewage to detect and quantify drug use within a community. While SBE has been applied repeatedly for the estimation of classical illicit drugs, only few studies investigated new psychoactive substances (NPS). These compounds mimic effects of illicit drugs by introducing slight modifications to chemical structures of controlled illicit drugs. We describe the optimization, validation, and application of an analytical method using liquid chromatography coupled to positive electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seven NPS in sewage: methoxetamine (MXE), butylone, ethylone, methylone, methiopropamine (MPA), 4-methoxymethamphetamine (PMMA), and 4-methoxyamphetamine (PMA). Sample preparation was performed using solid-phase extraction (SPE) with Oasis MCX cartridges. The LC separation was done with a HILIC (150 x 3mm, 5μm) column which ensured good resolution of the analytes with a total run time of 19min. The lower limit of quantification (LLOQ) was between 0.5 and 5ng/L for all compounds. The method was validated by evaluating the following parameters: sensitivity, selectivity, linearity, accuracy, precision, recoveries and matrix effects. The method was applied on sewage samples collected from sewage treatment plants in Belgium and Switzerland in which all investigated compounds were detected, except MPA and PMA. Furthermore, a consistent presence of MXE has been observed in most of the sewage samples at levels higher than LLOQ.

AB - Sewage-based epidemiology (SBE) employs the analysis of sewage to detect and quantify drug use within a community. While SBE has been applied repeatedly for the estimation of classical illicit drugs, only few studies investigated new psychoactive substances (NPS). These compounds mimic effects of illicit drugs by introducing slight modifications to chemical structures of controlled illicit drugs. We describe the optimization, validation, and application of an analytical method using liquid chromatography coupled to positive electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seven NPS in sewage: methoxetamine (MXE), butylone, ethylone, methylone, methiopropamine (MPA), 4-methoxymethamphetamine (PMMA), and 4-methoxyamphetamine (PMA). Sample preparation was performed using solid-phase extraction (SPE) with Oasis MCX cartridges. The LC separation was done with a HILIC (150 x 3mm, 5μm) column which ensured good resolution of the analytes with a total run time of 19min. The lower limit of quantification (LLOQ) was between 0.5 and 5ng/L for all compounds. The method was validated by evaluating the following parameters: sensitivity, selectivity, linearity, accuracy, precision, recoveries and matrix effects. The method was applied on sewage samples collected from sewage treatment plants in Belgium and Switzerland in which all investigated compounds were detected, except MPA and PMA. Furthermore, a consistent presence of MXE has been observed in most of the sewage samples at levels higher than LLOQ.

KW - LC-MS/MS

KW - Methoxetamine

KW - Novel psychoactive substances (NPS)

KW - Sewage epidemiology

KW - Wastewater

UR - http://www.scopus.com/inward/record.url?scp=84940956769&partnerID=8YFLogxK

U2 - 10.1002/dta.1777

DO - 10.1002/dta.1777

M3 - Journal article

C2 - 25655588

AN - SCOPUS:84940956769

VL - 7

SP - 812

EP - 818

JO - Drug Testing and Analysis

JF - Drug Testing and Analysis

SN - 1942-7603

IS - 9

ER -