Evaluation of active solvent modulation to enhance two-dimensional liquid chromatography for target analysis in polymeric matrices

•Active solvent modulation (ASM) applied to polymer 2D-LC analysis.•ASM prevents sample breakthrough in 2D (RPLC) despite 100% THF used in 1D (UHP-SEC).•Signal detectability enhancement of up to factor 20.•Good linearity (R2 > 0.9995) and reproducibility (as low as 0.3% area RSD).•Short heart-cut...

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Bibliographic Details
Published in:Journal of Chromatography A 2018-08, Vol.1562, p.78-86
Main Authors: Pursch, Matthias, Wegener, Antje, Buckenmaier, Stephan
Format: Article
Language:English
Subjects:
2D-LC
Comprehensive
Heart-cutting
Peak focusing
Signal detectability enhancement
Solvent compatibility
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Summary:•Active solvent modulation (ASM) applied to polymer 2D-LC analysis.•ASM prevents sample breakthrough in 2D (RPLC) despite 100% THF used in 1D (UHP-SEC).•Signal detectability enhancement of up to factor 20.•Good linearity (R2 > 0.9995) and reproducibility (as low as 0.3% area RSD).•Short heart-cutting (10 min) and comprehensive (20 min) separations. A new methodology is presented for two-dimensional liquid chromatography (2D-LC) separations of polymers. Active solvent modulation (ASM) was evaluated in its effectiveness to enhance solvent compatibility for both separation dimensions. As an example the determination of target compounds in epoxy resins was used. Ultra-high pressure size-exclusion chromatography was applied in the first dimension using THF as the solvent. The second dimension separation was operated in reversed-phase mode using an acetonitrile/water gradient. ASM prevents sample breakthrough in the second dimension and produces chromatograms that are of great peak shape and high resolution. It enables very sensitive determination of target components down to the low ppm level. The resulting high-speed 2D-LC method (10 min analysis time) showed good linearity (R2 > 0.9995) and reproducibility (as low as 0.3–0.7% peak area RSD). ASM was also applied in comprehensive 2D-LC (SECxLC) mode for characterization of molecular weight and chemical composition distribution of a polymer blend consisting of epoxy novolac and phenol novolac. The SECxLC separation was executed at short run times (20 min). ASM technology can markedly enhance productivity in 2D-LC analysis for many complex sample matrices.
ISSN:0021-9673
DOI:10.1016/j.chroma.2018.05.059