Australian Centre for Research on Separation Science (ACROSS), School of Science and Health, University of Western Sydney (Parramatta), Sydney, NSW, Australia.
J Chromatogr A. 2012 Dec 28;1270:204-11. doi: 10.1016/j.chroma.2012.11.009. Epub 2012 Nov 9.
A new column format known as parallel segmented flow has recently been introduced, whereby improvements in column performance are observed. These improvements are achieved via the separation of eluent from the column core from that of the column wall region. The segmentation of flow is accomplished immediately as the eluent exits the column through the use of a multi-channel end fitting. The ratio of flow exiting through the column central port relative to the peripheral ports, known as the segmentation ratio, can be tuned to optimise chromatographic performance. Investigations into the use of parallel segmented flow chromatography columns have demonstrated increased sensitivity and theoretical plates in analytical scale isocratic separations, but so far no studies have detailed the performance of these columns in gradient elution. The current study addresses the performance of parallel segmented flow columns in gradient elution, detailing the reproducibility of the gradient at various segmentation ratios and compares the performance to conventional columns. The study found that there was no observable difference in the gradient shape, or reproducibility of the gradient profiles generated at any segmentation ratio, tested on three different types of stationary phases. A separation of an 11-component test mixture verified that the primary advantage of parallel segmented flow columns was that the peak volume was reduced in proportion to the segmentation ratio.
最近引入了一种称为并行分段流的新柱格式，通过该格式可以观察到柱性能的提高。这些改进是通过将洗脱液从柱芯与柱壁区域分离来实现的。通过在洗脱液从柱中流出时使用多通道端配件，即可立即实现流的分段。从柱中心端口流出的流量与外围端口的流量之比，称为分段比，可以进行调整以优化色谱性能。对平行分段流色谱柱的使用进行的研究表明，在分析规模的等度分离中提高了灵敏度和理论塔板数，但到目前为止，尚无研究详细介绍这些柱在梯度洗脱中的性能。本研究探讨了在梯度洗脱中平行分段流柱的性能，详细说明了在各种分段比下梯度的重现性，并将其性能与传统柱进行了比较。研究发现，在三种不同类型的固定相上测试时，在任何分段比下，梯度形状或梯度轮廓的重现性均无明显差异。对 11 组分测试混合物的分离验证了平行分段流柱的主要优点是，峰体积与分段比成比例减小。
