Green analytical toxicology method for determination of synthetic cathinones in oral fluid samples by microextraction by packed sorbent and liquid chromatography-tandem mass spectrometry

Autor(es)

da Cunha, Kelly Francisco ; Oliveira, Karina Diniz ; Costa, Jose Luiz

• Tipo de documento: Artigo Científico
• Fonte: Forensic Toxicology; v. N/A, p. 13-pg., 2023-07-28.

Resumo

PurposeWe developed and validated a method for quantitative analysis of ten synthetic cathinones in oral fluid (OF) samples, using microextraction by packed sorbent (MEPS) for sample preparation followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS).MethodOF samples were collected with a Quantisal & TRADE; device and 200 & mu;L was extracted using a C18 MEPS cartridge installed on a semi-automated pipette and then analyzed using LC-M/SMS.ResultsLinearity was achieved between 0.1 and 25 ng/mL, with a limit of detection (LOD) of 0.05 ng/mL and a limit of quantification (LOQ) of 0.1 ng/mL. Imprecision (% relative standard deviation) and bias (%) were better than 11.6% and 7.5%, respectively. The method had good specificity and selectivity against 9 different blank OF samples (from different donors) and 68 pharmaceutical and drugs of abuse with concentrations varying between 400 and 10,000 ng/mL. No evidence of carryover was observed. The analytes were stable after three freeze/thaw cycles and when kept in the autosampler (10 & DEG;C) for up to 24 h. The method was successfully applied to quantify 41 authentic positive samples. Methylone (mean 0.6 ng/mL, median 0.2 ng/mL), N-ethylpentylone (mean 16.7 ng/mL, median 0.35 ng/mL), eutylone (mean 39.1 ng/mL, median 3.6 ng/mL), mephedrone (mean 0.5 ng/mL, median 0.5 ng/mL), and 4-chloroethcathinone (8.1 ng/mL) were quantified in these samples.ConclusionMEPS was an efficient technique for Green Analytical Toxicology purposes, which required only 650 & mu;L organic solvent and 200 & mu;L sodium hydroxide, and the BIN cartridge had a lifespan of 100 sample extractions. (AU)

• Processo FAPESP: 17/02147-0 - Cromatografia líquida em uma gota e seu acoplamento com espectrometria de massas: estratégias instrumentais, desenvolvimento de materiais, automatização e aplicações analíticas
• Beneficiário: Fernando Mauro Lanças
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 20/10809-5 - Técnicas de microextração em toxicologia forense
• Beneficiário: José Luiz da Costa
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 18/11849-0 - A toxicologia das Novas Substâncias Psicoativas (NSP): epidemiologia do consumo através da análise de amostras de fluido oral e caracterização de seu metabolismo in vitro
• Beneficiário: Kelly Francisco da Cunha
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 18/00432-1 - A Toxicologia das Novas Substâncias Psicoativas (NSP): epidemiologia do consumo através da análise de amostras de cabelo e fluido oral
• Beneficiário: José Luiz da Costa
• Modalidade de apoio: Auxílio à Pesquisa - Regular