Abstract
The use of psychoactive substances is a serious problem in today’s society and reliable methods of analysis are necessary to confirm their occurrence in biological matrices. In this work, a green sample preparation technique prior to HPLC-MS analysis was successfully applied to the extraction of 14 illicit drugs from urine samples. The isolation procedure was a dispersive liquid–liquid microextraction based on the use of a low transition temperature mixture (LTTM), composed of choline chloride and sesamol in a molar ratio 1:3 as the extracting solvent. This mixture was classified as LTTM after a thorough investigation carried out by FTIR and DSC, which recorded a glass transition temperature at −71 °C. The extraction procedure was optimized and validated according to the main Food and Drug Administration (FDA) guidelines for bioanalytical methods, obtaining good figures of merit for all parameters: the estimated lower limit of quantitation (LLOQ) values were between 0.01 µg L−1 (bk-MMBDB) and 0.37 µg L−1 (PMA); recoveries, evaluated at very low spike levels (in the ng-µg L−1 range), spanned from 55% (MBDB) to 100% (bk-MMBDB and MDPV); finally, both within-run and between-run precisions were lower than 20% (LLOQ) and 15% (10xLLOQ).
Highlights
The fight against illicit drug use is still a current and central issue in all countries
In order to prepare a green solIvnenotrdthearttoisplirqeupiadreatargoroementseomlvpeenrat ttuhraet,iCs hliCqul iadndatSreosom temperature, choline chloride:sesamol in a molar ratio 1:3 (ChCl) and Ses were selected as the hydrogenwbeornedsealecccetepdtoars(tHhBeAh)ydanrodghenydbroongdenacbcoenpdtodro(nHoBrA(H) aBnDd),hydrogen bond donor (HBD), respectively, because of their phreysspiceoctcihveemly,icbaelccahuasreaoctfetrhisetiircps hanydsicfoorchbeeminigcanlacthuararal,cctehreiastpic, s and for being natural, cheap, and low-toxicity compounds
The 1:1 ture crystallizes completely, whmiliexttuhree1c:2ryasntadll1iz:4ems cioxtmuprelsetaeplyp,ewarhailsectlhoeu1d:y2 laiqnudid1:s4, imndixi-tures appear as cloudy liquids, cating the occurrence of partiailncdryicsattailnligzathtieono.ccInudrreeendc,eCohfCpla:Srteisalwcrityhstaalmlizoalatirorna.tiIondoefe1d:3, ChCl:Ses with a molar ratio of was selected as the extracting s1o:3lvwenatsinsetlheectfeodlloaws tihneg eDxLtrLaMctEinogpseorlavteionntsintothheavfoelaloswtaibnlge dispersive liquid–liquid microextraction (DLLME) operations to have a liquid at sub-ambient temperastutarbelceolniqduitidionatss(u20b-°aCm).bient temperature conditions (20 ◦C)
Summary
The fight against illicit drug use is still a current and central issue in all countries. As reported by the European Monitoring Center for Drugs and Drug Addiction, in the last year, it was estimated that more than 29% of European people have tried illicit drugs during their lifetime. Drug consumption in Europe covers a wider range of substances than in the past, in line with poly-drug abuse, which is very common among both regular and occasional users. “New psychoactive substances” are analogues of well-known drugs such as cannabinoids, hallucinogens, and psychostimulants [1]. They include many synthetic cathinones (SCs), arylcyclohexylamines, phenethylamines, and tryptamines.
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