Qualitative Screening of Amphetamine- and Ketamine-Type Abuse Drugs in Urine Employing Dual Mode Extraction Column by Liquid Chromatography–Tandem Mass Spectrometry (LC–MS-MS)

Abstract

This manuscript reported a fast and rapid qualitative screening method for abuse drugs in urine by liquid chromatography tandem mass spectrometry (LC-MS/MS). The scope of the abuse drugs under investigation included methamphetamine (MA), amphetamine (AMP), methylenedioxymethamphetamine (MDMA), methylenedioxyamphetamine (MDA), paramethoxymethamphetamine (PMMA), ephedrine, pseudoephedrine, ketamine (KET), deschloroketamine (DCK), 2-fluorodeschloroketamine (2-F-DCK) and deschloro-N-ethylketamine (2-oxo-PCE). The method employed a dual mode extraction (DME) column as a novel clean up method for the urine matrix. To an aliquot of 0.2 mL urine, internal standards (ISTDs) and 0.4 mL of acidified methanol were added. After vortex and centrifugation, the supernatant was passed through a dual mode extraction (DME) column before LC-MS/MS analysis. Chromatographic separation was achieved with a C18 column by gradient elution. The limits of detection (LODs) for MA, AMP, MDMA, MDA and PMMA were 3 ng/mL; whereas those for ephedrine and pseudoephedrine were 10 ng/mL and those for KET, DCK, 2-F-DCK and 2-oxo-PCE were 1 ng/mL. The matrix effects ranged from -12% to 7% (%CV from 4% to 19%). This method is fit for the intended purpose for forensic toxicology, as well as for forensic analysis of drugs facilitating sexual assault (DFSA) and other criminal acts.

Interpol Review of Drug Analysis 2019-2022

“…HS-SPME-IMS method for determination of ketamine and midazolam [ 808 ]; magnetic dispersive SPME coupled with GC-MS for simultaneous determination of tramadol and fluoxetine in water and biological samples [ 809 ]; ultrasound-assisted dispersive SPME technique for simultaneous preconcentration and determination of ultra-trace amount of carbamazepine and phenobarbital [ 810 ]; review focusing on the sensing of DFSA drugs (Rohypnol, flunitrazepam, GHB and ketamine) and potential limitations for real life implementations of the sensors [ 811 ]; optimization and validation of a dried blood spot microwave-assisted extraction LC-MS method for the determination of selected substances from the date-rape drugs group: ketamine, benzodiazepines and cocaine [ 812 ]; simultaneous voltammetric determination of noscapine and lorazepam [ 813 ]; 2022 CV with portable Raman spectroscopy for determination of mephedrone (4-MMC) and 4-methylethcathinone (4-MEC) [ 814 ]; ion-selective electrodes for cocaine, tropane, atropine, and scopolamine [ 815 ]; electrochemical sensor for the simultaneous detection of morphine and methadone [ 816 ]; HPLC method for simultaneous detection of four sedative-hypnotic drugs (diazepam, ketamine, nimetazepam, and xylazine) recovered from spiked beverages [ 817 ]; Vortex-assisted dispersive liquid-liquid microextraction-gas chromatography (VADLLME-GC) determination of residual ketamine, nimetazepam, and xylazine from drug-spiked beverages in liquid, droplet, and dry forms [ 818 ]; LC-MS-MS screening method for MA, AMP, MDMA, MDA, paramethoxymethamphetamine (PMMA), ephedrine, pseudoephedrine, ketamine, deschloroketamine (DCK), 2-fluorodeschloroketamine (2-F-DCK) and 2-oxo-PCE [ 819 ]; enrichment bag-based liquid-phase microextraction (EB-LPME) system to isolate and enrich AMP, MA, MDMA, ketamine, codeine and fentanyl from wastewater [ 820 ].…”