Liquid chromatography-tandem mass spectrometry method for the simultaneous analysis of multiple hallucinogens, chlorpheniramine, ketamine, ritalinic acid, and metabolites, in urine.
Maria Del Mar Ramirez Fernandez, Marleen Laloup, Michelle Wood, Gert de Boeck, Manuel López-rivadulla, Pierre Wallemacq, Nele Samyn
Journal of Analytical Toxicology October 1, 2007 DOI: 10.1093/jat/31.8.497 (opens in new tab)
Study at a glance
AI-extracted from the abstract| Characteristics | Method validation study Peer reviewed |
|---|---|
| Population | Human urine samples |
| Topics | Ketamine LSD Esketamine |
| Keywords | Drug detection Substance analysis Drug testing Forensic toxicology Clinical toxicology Drug screening Metabolite detection Drug identification Lc-ms Liquid chromatography-mass spectrometry Bioanalysis Chemical analysis Laboratory techniques Bioanalytical methods Urine analysis Biofluid analysis Human sample analysis Clinical samples Urine testing Biological sample analysis Human urine Psychoactive substances Hallucinogens Chlorpheniramine Illicit drugs Drug metabolites Pharmaceuticals Controlled substances |
| Citations | 47 |
| Key points | A validated LC-MS/MS method enables simultaneous quantification of multiple hallucinogens, chlorpheniramine, ketamine, ritalinic acid, and their metabolites in human urine with limits of quantification as low as 0.05 ng/mL for LSD. |
Abstract
A validated method for the simultaneous analysis of multiple hallucinogens, chlorpheniramine, ketamine, ritalinic acid, and several metabolites is presented. The procedure comprises a sample clean-up step, using mixed-mode solid-phase extraction followed by liquid chromatography (LC)-tandem mass spectrometry analysis. Chromatographic separation was achieved using a Sunfire C(8) column eluted with a mixture of formate buffer, methanol, and acetonitrile. The applied LC gradient ensured the elution of all the drugs examined within 14 min and produced chromatographic peaks of acceptable symmetry. Selectivity of the method was achieved by a combination of retention time and two precursor-product ion transitions for the non-deuterated analogues. Validation of the method was performed using 500 microL of urine. The limits of quantification (LOQ) for LSD and 2-oxo-3-hydroxy-LSD were 0.05 and 1 ng/mL, respectively, and ranged, for the other hallucinogens, from 0.5 to 10 ng/mL. Linear and quadratic regression was observed from the LOQ of each compound to 12.5 ng/mL for LSD, 50 ng/mL for 2-oxo-3-hydroxy-LSD and 500 ng/mL for the others (r(2) > 0.99). Precision for the QC samples, spiked at a minimum of two concentrations, was calculated [%CV and %bias 87% for all the analytes. Furthermore, the processed samples were demonstrated to be stable in the autosampler for at least 24 h. Finally, the validated method was applied to the determination of chlorpheniramine, ketamine, LSD, and psilocin in authentic urine samples.