Polymeric ionic liquid open tubular capillary column for on-line in-tube SPME coupled with UHPLC-MS/MS to determine endocannabinoids in plasma samples

Author(s)

Souza, Israel D. ^[1] ; Hantao, Leandro W. ^[2] ; Queiroz, Maria Eugenia C. ^[1]

Affiliation

^[1] Univ Sao Paulo, Fac Filosofia Ciencias & Letras Ribeirao Preto, Dept Quim, Ribeirao Preto, SP - Brazil

^[2] Univ Estadual Campinas, Inst Quim, Campinas, SP - Brazil

• Document type: Journal article
• Source: Analytica Chimica Acta; v. 1045, p. 108-116, JAN 3 2019.
• Web of Science Citations: 9

Abstract

This manuscript describes the development of wall-coated open tubular capillary column with polymeric ionic liquids (PILs) for on-line in-tube solid phase microextraction coupled with ultra high-performance liquid chromatography tandem mass spectrometry (in-tube SPME/UHPLC-MS/MS) to determine anandamide (AEA) and 2-arachidonoyl glycerol (2 A G) in plasma samples. Selective PILs were synthetized from the {[}VC6IM]{[}Cl], {[}VC16IM]{[}Br], and {[}(VIM)(2)C-10]2 {[}Br] - ionic liquids -by in-situ thermal-initiated polymerization in a fused silica capillary column for in-tube SPME. The synthesis procedure was optimized, and the capillary columns were characterized using spectroscopic and chromatography techniques. The chemically bonded and cross-linked PIL-based sorbent phase (thickness coating: 1.7 mu m) presented high chemical and mechanical stability. Among the sorbents evaluated, the PIL-based capillary, {[}VC16IM]{[}Br]/{[}(VIM)(2)C-10]2 {[}Br] presented the best performance with a sorption capacity of 37,311 ng cm(-3) and 48,307 ng cm(-3) for AEA and 2 A G, respectively. This capillary was reused more than ninety times without significant changes in extraction efficiency. The in-tube SPME-UHPLC-MS/MS method presented a linear range from 0.1 ngmL(-1) to 100 ngmL(-1) for AEA, and from 0.05 ng mL(-1) to 100 ngmL(-1) for 2 A G, with coefficients of determination higher than 0.99, p-value for Lack-of-fit test higher than 0.05 (alpha of 0.05), precision with coefficient of variation (CV) values ranging from 1.6 to 14.0% and accuracy with relative standard deviation (RSD) values from -19.6% to 13.2%. This method was successfully applied to determine AEA and 2 A G in plasma patients with Parkinson's disease. The concentrations in these plasma samples ranged from 0.14 to 0.46 ngmL(-1) for AEA and from <0.05 ng mL(-1) to 0.51 ng mL(-1) for 2-AG. (C) 2018 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: 16/01082-9 - Column switching liquid chromatography coupled to tandem mass spectrometry for the analysis of endocannabinoids in plasma samples
• Grantee: Israel Donizeti de Souza
• Support Opportunities: Scholarships in Brazil - Doctorate
• FAPESP's process: 15/07619-1 - Column switching liquid chromatography coupled to tandem mass spectrometry for the analysis of endocannabinoids and drugs in biological samples
• Grantee: Maria Eugênia Queiroz Nassur
• Support Opportunities: Regular Research Grants