Preparation and evaluation of 1,6-hexanediol ethoxylate diacrylate-based alkyl methacrylate monolithic capillary column for separating small molecules

Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography

“…Although the recently developed HEDA-based alkyl methacrylate monolithic columns could efficiently separate PUHs in 5 min [24], poorer retention of other polar analytes such as aflatoxins was found using the HEDA-based monolithic columns. In this study, we utilized EDMA as the cross-linker and incorporated MAA with alkyl methacrylates to increase the hydrophilicity of the synthesized polymeric monoliths for separating polar molecules by reversedphase capillary LC analysis.…”

“…A number of review articles have been published to discuss the chemistry of monolith polymerization [16,17] as well as the development and applications [18][19][20][21] of polymer-based monoliths. In previous studies, various polymer-based monolithic stationary phases were successfully utilized to separate large biomolecules such as proteins [4,6,21,22] and/or small molecules [5,8,23,24]. In addition to chromatographic separation, the polymer-based monoliths have also been utilized as solid-phase extraction (SPE) sorbents for sample pre-treatment in various bioanalytical and environmental applications [25,26].…”

“…In order to control the properties of polymeric monoliths, various investigations have been carried out by different research groups [3][4][5]24,27]. By altering the polymerization time intervals, Nischang and Brüggemann [5] synthesized a series of poly(butyl methacrylate-co-ethylene dimethacrylate) [poly(BMA-co-EDMA)] monolithic stationary phases for separating small molecules such as alkylbenzenes.…”

“…In the study, efficient separation of six alkylbenzenes was obtained using the monolithic column prepared by a polymerization time interval as short as 30 min. Lin et al [24] utilized 1,6-hexanediol ethoxylate diacrylate (HEDA) as the cross-linker to prepare alkyl methacrylate monoliths. HEDA contained two ether-linkages in the alkyl bridge to offer additional dipole-dipole interactions between polar analytes, such as phenylurea herbicides (PUHs), and monolithic stationary phases.…”

“…Fast separation of PUHs was achieved in 5 min by applying a steep gradient (25-80% acetonitrile-water in 3 min) at a flow velocity of 5.43 mm s À1 (i.e., 16 mL min À1 ). In addition to dipole-dipole interactions [24,27], incorporating p-p interactions [28,29] between analytes and stationary phases were also employed to prepare alkyl methacrylate-based monoliths to separate relatively polar small molecules. Cheng et al [29] synthesized a series of alkyl methacrylate (C 4 -C 18 ) monoliths using divinylbezene (DVB) as the cross-linker to provide additional p-p interactions for analyzing aromatic sulfonamide antibiotics by on-line preconcentration CEC-MS. Smirnov et al [30] prepared a series of poly(DVB-co-ethylvinylbenzene-co-2-hydroxyethyl methacrylate) [poly(DVB-co-EVB-co-HEMA)] monolithic stationary phases in glass columns (3 mm i.d.…”