Development of Wall-Coated Open Tubular Columns and Their Application to Nano Liquid Chromatography Coupled to Tandem Mass Spectrometry

Author(s)

Santos, Natalia G. P. ; Medina, Deyber A. V. ; Lancas, Fernando M.

• Document type: Journal article
• Source: Molecules; v. 28, n. 13, p. 15-pg., 2023-07-01.

Abstract

This work presents a study on the application of wall open tubular column (WCOT) in liquid chromatography coupled with tandem mass spectrometry. Each process step reports the column preparation method in detail, subdivided into column pretreatment, silanization, stationary phase coating, and immobilization. Then, an evaluation of the parameters that can affect the efficiency of these columns was made. Atrazine, clomazone, and metolachlor were used as probes during this step. Factors such as stationary phase composition, length, internal diameter, stationary phase mass employed, and injection volume were investigated. In addition, with the help of Knox and Poppe graphs, the columns' performance was evaluated to determine the optimal flow rate and the speed-efficiency relationship, respectively. Based on the results, the best configurations for the WCOT column application to the LC system were defined: length-8 m; inner diameter-25 & mu;m; mass of OV-210-2.5% m/v; and, injection volume-100 nL. Finally, the optimized WCOT column developed in this work was coupled with a commercially-packed trapping column in the nano liquid chromatography system (nanoLC). In this configuration, more significant results were obtained regarding separation resolution, with Rs = 5.9 achieved for the most retained pair of analytes (clomazone and metolachlor). (AU)

• FAPESP's process: 15/15462-5 - Employment of graphene as sorbent in miniaturized sample preparation techniques.
• Grantee: Bruno Henrique Fumes
• Support Opportunities: Scholarships in Brazil - Doctorate
• FAPESP's process: 19/22724-7 - Novel instrumental approaches for automated and miniaturized analytical methods for the detection of organic compounds by liquid chromatography coupled to mass spectrometry
• Grantee: Deyber Arley Vargas Medina
• Support Opportunities: Scholarships in Brazil - Post-Doctoral
• 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: 14/07347-9 - Development of novel materials and devices for miniaturized sample preparation techniques in the area of food safety
• Grantee: Fernando Mauro Lanças
• Support Opportunities: Regular Research Grants
• FAPESP's process: 19/26263-4 - Development of open tubular capillary columns for micro and nano liquid chromatography coupled to sequential mass spectroscopy
• Grantee: Natalia Gabrielly Pereira dos Santos
• Support Opportunities: Scholarships in Brazil - Doctorate (Direct)