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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
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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
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4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
Ships in 14 days - from Aldrich Partner.
€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
Ships in 14 days - from Aldrich Partner.
€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
4-Hydroxyindole, 99%
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Supelco
Acetic acid, analytical standard
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
Ships in 14 days - from Aldrich Partner.
€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
Ships in 14 days - from Aldrich Partner.
€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
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4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
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4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Sodium phosphate monobasic monohydrate, BioReagent, suitable for electrophoresis, 98.0-102.0%
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4100025-250MG250 mg
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4100025-1G1 g
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Sigma-Aldrich
Sodium phosphate monobasic monohydrate, BioXtra, for molecular biology, ≥99.5% (T)
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4100025-250MG250 mg
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4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid solution, SAJ first grade, 27.0-33.0%
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4100025-250MG250 mg
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4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, ≥99.7%, SAJ super special grade
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, SAJ first grade, ≥99.0%
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
Ships in 14 days - from Aldrich Partner.
€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, ≥99.7%
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
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4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, JIS special grade, ≥99.7%
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4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, 99.5-100.0%
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4100025-250MG250 mg
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€376.94
4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid, ≥99.7%, for titration in non-aqueous medium
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4100025-250MG250 mg
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4100025-1G1 g
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€615.93
Sigma-Aldrich
Acetic acid solution, 1 M, 1 N
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4100025-250MG250 mg
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4100025-1G1 g
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Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
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SKUVendor SKUPack SizeAvailabilityPriceQuantity
4100025-250MG250 mg
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4100025-1G1 g
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€615.93