High-sensitivity method for the determination of LSD and 2-oxo-3-hydroxy-LSD in oral fluid by liquid chromatography-tandem mass spectrometry

Autor(es)

da Cunha, Kelly Francisco ; Magalhaes Kahl, Julia Martinelli ; Fiorentin, Tais Regina ; Oliveira, Karina Diniz ; Costa, Jose Luiz

• Tipo de documento: Artigo Científico
• Fonte: Forensic Toxicology; v. 40, n. 2, p. 10-pg., 2022-04-12.

Resumo

Purpose We have developed and validated a high-sensitivity method to quantify lysergic acid diethylamide (LSD) and 2-oxo-3-hydroxy-LSD (OH-LSD) in oral fluid samples using liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was applied to the quantification of both substances in 42 authentic oral fluid samples. Methods A liquid-liquid extraction was performed using 500 mu L each of samples (oral fluid samples collected using Quantisal (TM) device) and dichloromethane/isopropanol mixture (1:1, v/v). Enzymatic hydrolysis was evaluated to cleave glucuronide metabolites. Results The limit of quantification was 0.01 ng/mL for both LSD and OH-LSD. The linearity was assessed between 0.01 and 5 ng/mL. Imprecision and bias were not higher than 10.2% for both analytes. Extraction recovery was higher than 69%. The analytes were stable in the autosampler at 10 degrees C for 24 h, and up to 30 days at 4 and -20 degrees C. The method was applied to the analysis of 42 oral fluid samples. LSD was detected in all samples (concentrations between 0.02 and 175 ng/mL), and OH-LSD was detected in 20 samples (concentrations between 0.01 and 1.53 ng/mL). Conclusions A high-sensitive method was fully validated and applied to authentic samples. To our knowledge, this is the first work to report concentrations of LSD and OH-LSD in authentic oral fluid samples. (AU)

• Processo FAPESP: 20/07470-6 - Desenvolvimento de método miniaturizado de extração para determinação de cetamina e seus metabólitos em amostras de fluido oral usando microextração líquido-líquido dispersiva (DLLME)
• Beneficiário: Júlia Martinelli Magalhães Kahl
• Modalidade de apoio: Bolsas no Brasil - Iniciação Científica
• 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: 20/10809-5 - Técnicas de microextração em toxicologia forense
• Beneficiário: José Luiz da Costa
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• 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