1 3
DOI 10.1007/s10337-016-3156-3
Chromatographia (2016) 79:1333–1341
ORIGINAL
Novel Monolithic Stationary Phase with Surface‑Grafted
Triphenyl Selector for Reversed‑Phase Capillary
Electrochromatography
Tahar Mekhalif
1,2
· Seydina Ibrahima Kebe
1
· Mohamed Guerrouache
1
·
Noureddine Belattar
2
· Marie Claude Millot
1
· Benjamin Carbonnier
1
Received: 21 March 2016 / Revised: 26 July 2016 / Accepted: 28 July 2016 / Published online: 9 August 2016
© Springer-Verlag Berlin Heidelberg 2016
Keywords Capillary electrochromatography · Phenyl-like
monolith · Reversed-phase · Trityl
Introduction
It is well accepted that one of the major advantages of
polymer-based monolithic stationary phases is the ease
and flexibility of their synthesis owing to the wide range
of available monomers incorporating side chains of inter-
est as chromatographic selectors [1–4]. This is particularly
true regarding the development of miniaturized chromato-
graphic columns, where the polymeric monolith approach
allows avoiding drawbacks inherent to the packing of small
diameter particles into narrow-bore tubes as-well as the
tedious fabrication of retaining frits. Inspired by the suspen-
sion polymerization protocols applied to the synthesis of
porous polymer beads, free radical polymerization remains
the most widely used method for the design of such mono-
lithic columns. Thermal initiation was first implemented
for the free radical copolymerization of functional mono-
mers and crosslinkers in the presence of porogenic sol-
vents [5, 6]. Photochemically driven conditions were con-
sidered for the first time in 1997 and proved well suited to
the spatially controlled incorporation of monolithic mate-
rials within the confines of microchannels [7]. These two
initiation methods are compatible with (meth)acrylate and
styrenic monomers offering the possibility for a vast range
of separation applications. Zwitterionic/betaine, hydroxyl-,
and amine-containing monomers have been used to prepare
monoliths for the separation of hydrophilic solutes under
normal phase [8], and hydrophilic interaction [9, 10] liquid
(electro)chromatography conditions.
Similar to the case of particulate stationary phases,
a large number of studies aimed at applying monolithic
Abstract A triphenylmethylamine-functionalized mono-
lithic capillary column was newly designed for reversed-
phase capillary electrochromatographic applications.
Incorporation of the three phenyl rings-containing selector
(also referred to as trityl selector) was achieved through
post-polymerization functionalization of a generic mono-
lithic matrix bearing nucleophilic-sensitive hydroxysuc-
cinimide moieties. Such a 3D polymer matrix was obtained
through UV-induced in situ free radical copolymerization
of N-acryloxysuccinimide and ethylene dimethacrylate.
The separation properties of the trityl monolithic capillary
column were initially evaluated vis-à-vis polycyclic aro-
matic hydrocarbons, as model hydrophobic compounds,
and compared to the separation ability of a benzylamine-
functionalized monolithic capillary column prepared using
the same generic monolithic matrix. Electrochromato-
graphic separation of phenols and anilines was also consid-
ered, and our preliminary results suggest the occurrence of
hydrophobic interactions due to the aromatic and non-polar
nature of the surface-grafted trityl selector. The triphenyl
monolithic capillary column exhibited relative standard
deviation values (% RSD) below 4.1 % for the here-stud-
ied chromatographic parameters, namely, retention factor,
selectivity, resolution, and efficiency.
* Benjamin Carbonnier
carbonnier@icmpe.cnrs.fr
1
Université Paris-Est, ICMPE (UMR7182), CNRS, UPEC,
94320 Thiais, France
2
Département de Biologie, Laboratoire de Biochimie
Appliquée, Faculté des Sciences, Université Ferhat Abbas,
19000 Sétif, Algeria