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Reversed-phase functionalised multi-lumen capillary as combined concentrator, separation column, and ESI emitter in capillary-LC-MS


Sanz Rodriguez, E and Lam, SC and Haddad, PR and Paull, B, Reversed-phase functionalised multi-lumen capillary as combined concentrator, separation column, and ESI emitter in capillary-LC-MS, Chromatographia, 83, (1) pp. 197-209. ISSN 0009-5893 (2019) [Refereed Article]

Copyright Statement

Copyright 2018 Springer-Verlag GmbH Germany, part of Springer Nature

DOI: doi:10.1007/s10337-018-3629-7


For the first time, a multi-lumen capillary (MLC) (126 parallel channels of 4.2 m i.d) has been modified to produce a C18-functionalised silica porous layer open tubular (PLOT) capillary column for both on-capillary preconcentration and separation. The modified multi-lumen capillary used in this dual mode provided significant advantages over typical nano/capillary-LCMS systems, in that it facilitated both higher sample loading capacity, the use of elevated flow rates, and simplified equipment requirements. Following modification, 100% of the channels displayed a homogenous porous silica layer, 257  36 nm thick. The PLOT-MLC was first evaluated for on-capillary solid-phase extraction. Extraction of caffeine, ofloxacin, atrazine, and diuron was carried out offline using an 8-cm-long PLOT-MLC, with quantification achieved using HPLC coupled to a quadrupole-time of flight (QTOF) mass spectrometer. The results confirmed reversed-phase selectivity and average recoveries obtained were around 70%. Subsequently, a 65-cm-long PLOT-MLC was evaluated as a separator column using a capillary liquid chromatography (Cap-LC) system equipped with a nano-injector and coupled to the mass spectrometer. The short PLOT-MLC provided a baseline separation in isocratic mode [water:acetonitrile (each with 0.1% formic acid) = 70:30, v/v] of ofloxacin, atrazine, and diuron. Finally, direct coupling of the PLOT-MLC with the QTOF via a capillary electrosprayer facilitated the simultaneous use of the modified capillary as a solid-phase concentrator, separator column (carrying out concentration-focusing-separation on the PLOT-MLC) and electrospray emitter. This configuration greatly simplifies the traditional capillary-LCMS equipment requirements, via the removal of all connectors and additional capillary between injector and MS inlet, and is demonstrated herein with large volume sample loading and step-gradient elution/separation with sensitive MS detection.

Item Details

Item Type:Refereed Article
Keywords:liquid chromatography, mass spectrometry, multi-lumen capillary, C18-funtionalised fused silica, porous layer open tubular columns
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Separation science
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Sanz Rodriguez, E (Dr Estrella Sanz Rodriguez)
UTAS Author:Lam, SC (Mr Shing Chung Lam)
UTAS Author:Haddad, PR (Professor Paul Haddad)
UTAS Author:Paull, B (Professor Brett Paull)
ID Code:129223
Year Published:2019 (online first 2018)
Funding Support:Australian Research Council (IC140100022)
Web of Science® Times Cited:2
Deposited By:Chemistry
Deposited On:2018-11-16
Last Modified:2019-03-12

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