Supercritical Fluid Chromatography x Ultra-High Pressure Liquid Chromatography for Red Chilli Pepper Fingerprinting by Photodiode Array, Quadrupole-Time-of-Flight and Ion Mobility Mass Spectrometry (SFC x RP-UHPLC-PDA-Q-ToF MS-IMS)
Supercritical Fluid Chromatography x Ultra-High Pressure Liquid Chromatography for Red Chilli Pepper Fingerprinting by Photodiode Array, Quadrupole-Time-of-Flight and Ion Mobility Mass Spectrometry (SFC x RP-UHPLC-PDA-Q-ToF MS-IMS)
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DOI：
10.1007/s12161-018-1307-x
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发表时间：
2018-12-01
影响因子：
2.9
通讯作者：
Mondello, Luigi
中科院分区：
文献类型：
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作者：
Donato, Paola;Giuffrida, Daniele;Mondello, Luigi
正相和反相液相色谱（NP-LC x RP-LC）的耦合是二维综合分离中增加正交性的最有效方法之一，是两种真正独立的保留机制。然而，由于流动相的不混相、次级柱头部的峰聚焦差（D-2）、信号干扰和峰退化，这种耦合并不是直接实现的。在本研究中，在第一维（D-1）中使用超临界流体色谱（SFC），并与超高压LC （UHPLC）相结合，以缓解不相容问题，并提供与使用超临界CO2相关的许多优势。在线SFC x RP-UHPLC系统以自动化方式实施，围绕两个2位，六端口开关阀，配备十八烷基硅胶盒，用于有效捕获和聚焦从D-1中洗脱的分析物。添加到SFC出水中的水补充流允许有效地将溶质集中在吸附剂材料上，并减少膨胀的CO2对D-2分离的干扰。除了光电二极管阵列和四极杆飞行时间质谱检测外，基于分析物质量、形状和大小的离子迁移率分离为红辣椒样品中的类胡萝卜素指纹图谱增加了第四个分离维度。
The coupling of normal phase and reversed phase liquid chromatography (NP-LC x RP-LC) is one of the most effective ways to increase orthogonality in two-dimensional comprehensive separations, being the two retention mechanisms truly independent. However, such coupling is not straightforward to implement, due to immiscibility of the mobile phases, poor peak focusing at the head of the secondary column (D-2), signal interferences and peak deterioration. In this research, supercritical fluid chromatography (SFC) was used in the first dimension (D-1), coupled to ultra high pressure LC (UHPLC), to alleviate incompatibility issues and provide a number of advantages related to the use of supercritical CO2. An on-line SFC x RP-UHPLC system was implemented in an automated fashion, around two 2-position, six-port switching valves equipped with octadecyl silica cartridges for effective trapping and focusing of the analytes eluted from D-1. A water make-up flow added to the SFC effluent permitted to efficiently focus the solutes on the sorbent material and to reduce interferences of the expanded CO2 on the D-2 separation. In addition to photodiode array and quadrupole-time-of-flight mass spectrometry detection, ion mobility separation based on analyte mass, shape and size added a fourth separation dimension for carotenoid fingerprinting in a red chilli pepper sample.