Publication
Validation and application of an UPLC–MS/MS method for the quantification of synthetic cannabinoids in urine samples and analysis of seized materials from the Portuguese market
| dc.contributor.author | Simões, Susana Sadler | |
| dc.contributor.author | Silva, Inês | |
| dc.contributor.author | Castañera Ajenjo, Antonio | |
| dc.contributor.author | Dias, Mário João | |
| dc.date.accessioned | 2017-11-16T12:51:52Z | |
| dc.date.available | 2017-11-16T12:51:52Z | |
| dc.date.issued | 2014-10 | |
| dc.description.abstract | An UPLC-MS/MS method using ESI+ionization and MRM was developed and fully validated according to international guidelines for the qualitative and quantitative analysis of nine synthetic cannabinoids and/or their metabolites in urine samples (1mL). Prior to extraction the samples were subjected to an enzymatic hydrolysis using β-glucuronidase followed by a SPE procedure using Oasis(®) HLB 3cc (60mg) columns. The chromatographic separation was performed with an Acquity UPLC(®) HSS T3 (50mm×2.1mm i.d., 1.8μm) reversed-phase column using a gradient with methanol-ammonium formate 2mM (0.1% formic acid) and with a run time of 9.5min. The method was validated in terms of selectivity, capacity of identification, limits of detection (0.01-0.5ng/mL) and quantification (0.05-0.5ng/mL), recovery (58-105%), carryover, matrix effect, linearity (0.05-50ng/mL), intra-assay precision, inter-assay accuracy and precision (CV<20%). The method was applied to 80 authentic samples, five of them (6.2%) were confirmed or suspected to be positive for the metabolites JWH-018 N-hydroxypentyl and JWH-018 N-pentanoic acid of JWH-018 and for the metabolite JWH-122 N-(5-hydroxypentyl) of JWH-122, and three of them in association with THC and/or THCCOOH (substances included in the method, together with the 11-OH-THC). Additionally, 17 spice products were analyzed, for which were confirmed the presence of the following substances: AM-2201, JWH-018, JWH-022 JWH-073, JWH-122, JWH-203, JWH-210, JWH-250, HU-210 and RCS-4, according to the comparison with authentic reference material and published data. The analytical method developed allowed the analysis of synthetic cannabinoids and the notification of the first cases in Portugal. | pt_PT |
| dc.description.version | info:eu-repo/semantics/publishedVersion | pt_PT |
| dc.identifier.citation | Forensic Sci Int. 2014 Oct;243:117-25. doi: 10.1016/j.forsciint.2014.07.022. | pt_PT |
| dc.identifier.doi | 10.1016/j.forsciint.2014.07.022 | pt_PT |
| dc.identifier.issn | 0379-0738 | |
| dc.identifier.uri | http://hdl.handle.net/10400.26/19347 | |
| dc.language.iso | eng | pt_PT |
| dc.peerreviewed | yes | pt_PT |
| dc.publisher | Elsevier | pt_PT |
| dc.relation.publisherversion | https://doi.org/10.1016/j.forsciint.2014.07.022 | pt_PT |
| dc.rights.uri | http://creativecommons.org/licenses/by-nc-nd/4.0/ | pt_PT |
| dc.subject | Synthetic cannabinoids | pt_PT |
| dc.subject | Spice | pt_PT |
| dc.subject | UPLC–MS/MS | pt_PT |
| dc.subject | Urine | pt_PT |
| dc.title | Validation and application of an UPLC–MS/MS method for the quantification of synthetic cannabinoids in urine samples and analysis of seized materials from the Portuguese market | pt_PT |
| dc.type | journal article | |
| dspace.entity.type | Publication | |
| oaire.citation.endPage | 125 | pt_PT |
| oaire.citation.startPage | 117 | pt_PT |
| oaire.citation.title | Forensic Science International | pt_PT |
| oaire.citation.volume | 243 | pt_PT |
| rcaap.embargofct | Política de copyright do editor | pt_PT |
| rcaap.rights | restrictedAccess | pt_PT |
| rcaap.type | article | pt_PT |