1 research outputs found
Online and Splitless NanoLC × CapillaryLC with Quadrupole/Time-of-Flight Mass Spectrometric Detection for Comprehensive Screening Analysis of Complex Samples
A novel
multidimensional separation system based on online comprehensive
two-dimensional liquid chromatography and hybrid high-resolution mass
spectrometry has been developed for the qualitative screening analysis
and characterization of complex samples. The core of the system is
a consistently miniaturized two-dimensional liquid chromatography
that makes the rapid second dimension compatible with mass spectrometry
without the need for any flow split. Elevated temperature, ultrahigh
pressure, and a superficially porous sub-3-μm stationary phase
provide a fast second dimension separation and a sufficient sampling
frequency without a first dimension flow stop. A highly loadable porous
graphitic carbon stationary phase is employed in the first dimension
to implement large volume injections that help countervailing dilution
caused by the sampling process between the two dimensions. Exemplarily,
separations of a 99-component standard mixture and a complex wastewater
sample were used to demonstrate the performance of the dual-gradient
system. In the second dimension, 30 s gradients at a cycle time of
1 min were employed. One multidimensional separation took 80–90
min (∼120 min including extended hold and re-equilibration
in the first dimension). This approach represents a cost-efficient
alternative to online LC × LC strategies working with conventionally
sized columns in the rapid second dimension, as solvent consumption
is drastically decreased and analytes still are detectable at environmentally
relevant concentrations