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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, Lam, SC ORCID: 0000-0001-5247-8397, Haddad, PR and Paull, B ORCID: 0000-0001-6373-6582 2018 , 'Reversed-phase functionalised multi-lumen capillary as combined concentrator, separation column, and ESI emitter in capillary-LC-MS' , Chromatographia , pp. 1-13 , doi:

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For the first time, a multi-lumen capillary (MLC) (126 parallel channels of 4.2 µm 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-LC–MS 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-LC–MS 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 Type: Article
Authors/Creators:Sanz Rodriguez, E and Lam, SC and Haddad, PR and Paull, B
Keywords: liquid chromatography, mass spectrometry, multi-lumen capillary, C18-funtionalised fused silica, porous layer open tubular columns
Journal or Publication Title: Chromatographia
Publisher: Vieweg
ISSN: 0009-5893
DOI / ID Number:
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Copyright 2018 Springer-Verlag GmbH Germany, part of Springer Nature

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