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  • 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.

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.

Forensic science international (2014-08-16)
Susana Sadler Simões, Inês Silva, Antonio Castañera Ajenjo, Mário João Dias
RESUMEN

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.

MATERIALES
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Formic acid solution, BioUltra, 1.0 M in H2O
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Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
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Ethyl Acetate, Pharmaceutical Secondary Standard; Certified Reference Material
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Ethyl acetate
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Ethyl acetate
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Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
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Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard
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Sodium phosphate dibasic, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, E 339, anhydrous, 98-100.5% (calc. to the dried substance)
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Ethyl acetate, puriss., meets analytical specification of Ph. Eur., BP, NF, ≥99.5% (GC)
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Ethyl acetate, ACS reagent, ≥99.5%
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Acetonitrile, biotech. grade, ≥99.93%
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Ethyl acetate, ACS reagent, ≥99.5%
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Sodium phosphate dibasic, puriss. p.a., ACS reagent, anhydrous, ≥99.0% (T)
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Hexane, suitable for HPLC, ≥97.0% (GC)