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Loop-based multiple heart-cutting two-dimensional liquid chromatography for target analysis in complex matrices.

Matthias Pursch1, Stephan Buckenmaier2

  • 1†Dow Deutschland Anlagengesellschaft mbH, Analytical Technology Center (ATC), Industriestr. 1, 77836 Rheinmuenster, Germany.

Analytical Chemistry
|April 22, 2015
PubMed
Summary
This summary is machine-generated.

Loop-based multiple heart-cutting (MHC) two-dimensional liquid chromatography (2D-LC) effectively quantifies hexabromocyclododecane (HBCD) in polystyrene. This advanced technique overcomes limitations of traditional 1D-LC for complex polymer additive analysis.

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Area of Science:

  • Analytical Chemistry
  • Chromatography
  • Polymer Analysis

Background:

  • Quantifying polymer additives like hexabromocyclododecane (HBCD) in complex matrices is challenging with conventional methods.
  • One-dimensional liquid chromatography (1D-LC) fails to separate HBCD isomers from polystyrene (PS) components, hindering accurate quantification.
  • High chromatographic resolution is necessary for precise analysis of additives within polymer samples.

Purpose of the Study:

  • To present loop-based multiple heart-cutting (MHC) 2D-LC as a solution for high-resolution quantification of polymer additives.
  • To demonstrate the application of MHC 2D-LC for determining HBCD in polystyrene samples.
  • To evaluate the separation power, accuracy, and repeatability of MHC 2D-LC for complex matrix analysis.

Main Methods:

  • Employed loop-based multiple heart-cutting (MHC) two-dimensional liquid chromatography (2D-LC).
  • Utilized a column set with phenyl (1D) and C18 (2D) stationary phases for enhanced separation.
  • Heart-cuts from the 1D chromatogram were sequentially reinjected onto the 2D column for analysis.

Main Results:

  • MHC 2D-LC achieved baseline separation of HBCD from the PS background in the second dimension.
  • Demonstrated linearity for spiked polymer samples over a concentration range of 0.02-1.00 wt % HBCD.
  • Established a limit of quantitation of 0.01 wt % HBCD and achieved excellent repeatability (RSD of 0.7%) for real samples.

Conclusions:

  • MHC 2D-LC provides the necessary separation, accuracy, and repeatability for quantifying challenging polymer additives like HBCD.
  • This technique offers an elegant solution for complex samples where conventional 1D-LC fails.
  • The method is suitable for the accurate determination of HBCD in polystyrene matrices.