title: Reducing Dilution and Analysis Time in Online Comprehensive Two-Dimensional Liquid Chromatography by Active Modulation.
abstract: Online comprehensive two-dimensional liquid chromatography (LC × LC) offers ways to achieve high-performance separations in terms of peak capacity (exceeding 1000) and additional selectivity to realize applications that cannot be addressed with one-dimensional chromatography (1D-LC). However, the greater resolving power of LC × LC comes at the price of higher dilutions (thus, reduced sensitivity) and, often, long analysis times (>100 min). The need to preserve the separation attained in the first dimension ((1)D) causes greater dilution for LC × LC, in comparison with 1D-LC, and long analysis times to sample the (1)D with an adequate number of second dimension separations. A way to significantly reduce these downsides is to introduce a concentration step between the two chromatographic dimensions. In this work we present a possible active-modulation approach to concentrate the fractions of (1)D effluent. A typical LC × LC system is used with the addition of a dilution flow to decrease the strength of the (1)D effluent and a modulation unit that uses trap columns. The potential of this approach is demonstrated for the separation of tristyrylphenol ethoxylate phosphate surfactants, using a combination of hydrophilic interaction and reversed-phase liquid chromatography. The modified LC × LC system enabled us to halve the analysis time necessary to obtain a similar degree of separation efficiency with respect to UHPLC based LC × LC and of 5 times with respect to HPLC instrumentation (40 compared with 80 and 200 min, respectively), while at the same time reducing dilution (DF of 142, 299, and 1529, respectively) and solvent consumption per analysis (78, 120, and 800 mL, respectively).
authors.affiliation: TI-COAST, Van 't Hoff Institute for Molecular Sciences, Science Park 904, 1098 XH Amsterdam, Netherlands.|Van 't Hoff Institute for Molecular Sciences, Science Park 904 1098 XH Amsterdam, Netherlands.
authors.forename: Andrea F G
authors.initials: AF
authors.lastname: Gargano
authors.affiliation: Syngenta, Jealott's Hill International Research Centre, Bracknell, Berkshire RG42 6EY, United Kingdom.
authors.forename: Mike
authors.initials: M
authors.lastname: Duffin
authors.affiliation: Syngenta, Jealott's Hill International Research Centre, Bracknell, Berkshire RG42 6EY, United Kingdom.
authors.forename: Pablo
authors.initials: P
authors.lastname: Navarro
authors.affiliation: Van 't Hoff Institute for Molecular Sciences, Science Park 904 1098 XH Amsterdam, Netherlands.
authors.forename: Peter J
authors.initials: PJ
authors.lastname: Schoenmakers