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Towards a generic variable column length method development strategy for samples with a large variety in polarity

机译:针对极性多种多样的样品的通用可变柱长方法开发策略

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The development of a novel set-up for the sequential analysis of compounds with a large variety in polarity on HILIC and reversed-phase columns, coupled in series, is discussed. For this purpose, a commercially available ultra-high performance LC system, equipped with two switching valves is employed. The switching valves allow connecting the HILIC and reversed-phase columns either in series or in parallel to the system. An interface to couple the HILIC and reversed-phase columns is developed and optimized. The sample is first injected onto a HILIC column. Apolar compounds in the sample are not retained and will elute close to or within the void volume of the HILIC column. Accurate switching of the valves allows redirecting these compounds towards a trap loop while more polar compounds are retained and separated on the HILIC column. After separation and detection of the polar compounds, the configuration of the valves is switched again to direct the apolar compounds from the trap loop towards a reversed-phase column for separation. To deal with the incompatibility of the mobile phases of HILIC and reversed-phase column separations, commercially available jet weaver mixers are included in the set-up to allow for an intermediate solvent exchange. The proof-of-concept is demonstrated for the analysis of pharmaceuticals that can be found in waste water and surface water. It is demonstrated that the set-up provides robust analyses with peak capacities that are intermediate to one-dimensional and two-dimensional separations. (C) 2014 Elsevier B.V. All rights reserved.
机译:讨论了一种新的装置的开发,该装置用于在串联和串联的HILIC和反相色谱柱上顺序分析具有多种极性的化合物。为此,使用了配有两个切换阀的市售超高性能液相色谱系统。切换阀允许将HILIC色谱柱和反相色谱柱串联或并联连接至系统。开发和优化了将HILIC和反相色谱柱耦合的接口。首先将样品注入HILIC色谱柱。样品中的非极性化合物不会保留,会洗脱到HILIC色谱柱的空隙体积附近或之内。阀门的准确切换可将这些化合物重定向至捕集环,同时更多极性化合物保留并在HILIC色谱柱上分离。在分离和检测出极性化合物之后,再次切换阀的配置,以将非极性化合物从捕集环引向反相色谱柱进行分离。为了处理HILIC流动相和反相柱分离的不相容性,在此装置中包括了可商购的喷射织造混合器,以进行中间溶剂交换。该概念证明可用于分析废水和地表水中的药物。事实证明,该设置提供了稳健的分析,其峰容量介于一维和二维分离之间。 (C)2014 Elsevier B.V.保留所有权利。

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