In-tube solid-phase microextraction with a dummy molecularly imprinted monolithic capillary coupled to ultra-performance liquid chromatography-tandem mass spectrometry to determine cannabinoids in plasma samples

Author(s)

Marchioni, Camila ^[1] ; Vieira, Tatiana Manzini ^[2] ; Miller Crotti, Antonio Eduardo ^[2] ; Crippa, Jose Alexandre ^[3] ; Costa Queiroz, Maria Eugenia ^{[2, 1]}

Affiliation

^[1] Univ Sao Paulo, Fac Ciencias Farmaceut Ribeirao Preto, Ave Bandeirantes 3900, BR-14040901 Sao Paulo, SP - Brazil

^[2] Univ Sao Paulo, Fac Filosofia Ciencias & Letras Ribeirao Preto, Dept Quim, Ave Bandeirantes 3900, BR-14040901 Sao Paulo, SP - Brazil

^[3] Univ Sao Paulo, Ribeirao Preto Med Sch, Dept Neurosci & Behav, Sao Paulo, SP - Brazil

• Document type: Journal article
• Source: Analytica Chimica Acta; v. 1099, p. 145-154, FEB 22 2020.
• Web of Science Citations: 0

Abstract

A selective and sensitive method that uses automated in-tube solid-phase microextraction coupled to ultra-performance liquid chromatography-tandem mass spectrometry (in-tube SPME/UHPLC-MS/MS) was developed to determine cannabidiol (CBD) and Delta 9-tetrahydrocannabinol (Delta 9-THC) in plasma samples. A new dummy molecularly imprinted monolithic capillary (MIP monolith) for in-tube SPME was prepared by in situ polymerization in a fused silica capillary; hydrogenated cannabidiol was employed as dummy template. Fourier Transform Infrared Spectroscopy (FTIR) confirmed that the synthesis reagents were incorporated into the polymer chain. On the basis of the microscopy images (scanning electron microscopy - SEM and transmission electron microscopy - TEM), the MIP monolithic phase presented larger pores than the non-imprinted monolithic phase (NIP monolith), as well as a skeleton comprising clusters consisting of microspheres. By optimizing the polymerization conditions, the MIP monolith specifically recognized CBD and Delta 9-THC. The MIP monolith had CBD and Delta 9-THC sorption capacity of 148.05 and 44.49 ng cm(-3), respectively. The capillary was reused over fifty times without significant changes in its extraction efficiency. For both CBD and Delta 9-THC, in-tube SPME/UHPLC eMS/MS presented linear range from 10 to 300 ng mL(-1), precision with coefficient of variation (CV) values ranging from 0.2% to 19.1% (LLOQ), and accuracy with relative standard deviation (RSD) values spanning from -9.3% to 19.6% (LLOQ). The developed method was successfully applied to determine cannabinoid levels in plasma samples from volunteer patients in treatment with CBD. (C) 2019 Elsevier B.V. All rights reserved. (AU)

• FAPESP's process: 17/02147-0 - Single drop chromatography and its coupling to mass spectrometry: instrumental strategies, development of materials, automation and analytical applications
• Grantee: Fernando Mauro Lanças
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 16/13639-8 - Column-switching liquid chromatography-Tandem mass spectrometry for determination of endocannabinoids and cannabinoids in biological samples from patients with Parkinson's Disease
• Grantee: Camila Marchioni
• Support Opportunities: Scholarships in Brazil - Doctorate (Direct)