†Dow Deutschland Anlagengesellschaft mbH, Analytical Technology Center (ATC), Industriestr. 1, 77836 Rheinmuenster, Germany.
‡Agilent Technologies, Research and Development, Hewlett-Packard-Str. 8, 76337 Waldbronn, Germany.
Anal Chem. 2015 May 19;87(10):5310-7. doi: 10.1021/acs.analchem.5b00492. Epub 2015 May 4.
Loop-based multiple heart-cutting (MHC) two-dimensional liquid chromatography (2D-LC) is presented as a solution to quantify target components in complex matrices, such as additives in polymers, at very high chromatographic resolution. The determination of hexabromocyclododecane (HBCD) in polystyrene (PS) is described. One dimensional ((1)D) LC analysis with UV detection did not allow quantitation of the main isomers of HBCD due to peak overlap with polymer components. MHC 2D-LC analysis provided the separation power, accuracy, and repeatability needed for quantitative analysis of the additives of interest. Heart-cuts from peaks of the (1)D-chromatogram or entire regions of interest are sampled into loops, where they remain parked until their sequential reinjection onto the second dimension ((2)D) column. A column set consisting of phenyl ((1)D) and C18 ((2)D) stationary phases gave baseline separation in (2)D between HBCD and PS background. Linearity for spiked polymer samples was achieved over a range of 0.02-1.00 wt % HBCD relative to the amount of polymer. The limit of quantitation was estimated at 0.01 wt % HBCD in PS. A peak area RSD of 0.7% obtained for ten replicates of a real sample demonstrated excellent repeatability of the analysis. MHC 2D-LC is an elegant solution for quantitative analyses of difficult-to-separate samples when conventional (1)D separation fails.
基于循环的多次心脏切割（MHC）二维液相色谱（2D-LC）可用于解决在复杂基质中定量目标成分的问题，例如聚合物中的添加剂，同时实现非常高的色谱分辨率。本文介绍了使用 MHC 2D-LC 对聚苯乙烯（PS）中的六溴环十二烷（HBCD）进行定量分析的方法。一维（1D）LC 分析结合紫外检测无法定量 HBCD 的主要异构体，因为它们与聚合物成分的峰重叠。MHC 2D-LC 分析提供了所需的分离能力、准确性和重复性，可用于定量分析感兴趣的添加剂。从 1D 色谱峰的心脏切割或整个感兴趣区域被采样到循环中，在那里它们保持停留状态，直到它们顺序地重新注入到第二维（2D）柱上。由苯基（1D）和 C18（2D）固定相组成的柱组在 2D 中实现了 HBCD 和 PS 背景之间的基线分离。对于添加聚合物样品，在相对于聚合物量的 0.02-1.00wt% HBCD 范围内实现了线性。在 PS 中，HBCD 的定量限估计为 0.01wt%。对于真实样品的十个重复，获得的峰面积 RSD 为 0.7%，表明分析具有出色的重复性。当常规 1D 分离失败时，MHC 2D-LC 是一种用于分离困难样品的定量分析的优雅解决方案。
