Immobilization of phosphonium-based ionic liquid stationary phases extends their operative range to routine applications in the flavor, fragrance and natural product fields
Immobilization of phosphonium-based ionic liquid stationary phases extends their operative range to routine applications in the flavor, fragrance and natural product fields
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鏻基离子液体固定相的固定化将其操作范围扩展到香料、香料和天然产品领域的常规应用
DOI：
10.1016/j.chroma.2021.462796
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发表时间：
2022
影响因子：
4.1
通讯作者：
Bicchi, Carlo
中科院分区：
文献类型：
--
作者：
Cagliero, Cecilia;Bizzo, Humberto;Rubiolo, Patrizia;Marengo, Arianna;Galli, Stefano;Anderson, Jared L.;Sgorbini, Barbara;Bicchi, Carlo
磷基离子液体由于其独特的选择性和良好的色谱性能，已被证明是气相色谱（GC）中成功的固定相。本研究的重点是使用基于磷衍生物三己基（十四烷基）氯化磷（[P66614+][Cl−]）和三己基（十四烷基）磷双[（三氟甲基）磺酰]亚胺（[P66614+][NTf2−]）的两种il作为GC SPs，这两种il在色谱选择性和保留性方面是互补的。它们在常规分析中的应用受到其较低的最大允许工作温度（MAOT） （[P66614+][Cl−]IL为200°C， [P66614+][NTf2−]为180°C）的限制，这限制了它们在由相对高挥发性分析物组成的样品中的使用。先前在作者实验室进行的一项研究重点是通过优化柱特性和操作条件，将[P66614+][Cl−]IL SP的使用扩展到具有中低挥发性分析物的样品分析。本文研究了在软、硬反应条件下，将[P66614+][Cl−]和[P66614+][NTf2−]il固定在熔融石英柱内壁，以提高其MAOT。结果MAOT或多或少取决于激烈的固定化条件,和达到220°C软固定(所以化生)和240°C硬固定(Ha-Im) [P66614 +] (Cl−)IL列,和200°C forSo-Imand 220°forHa-Imin列涂有[P66614 +] [NTf2−)。固定化的影响分离能力和性能的所有列被评估使用我)Grob测试,(二)模型的混合41个不同极性的化合物,结构,在香精和香精领域具有代表性的不同有机官能团，iii) 37种脂肪酸甲酯的标准混合物，iv)薄荷精油，v)两种倍半萜烯醇（法尼醇和檀香醇）的混合物，vi) 16种农药的标准混合物。这些测试样品也被用来证明两种基于磷的IL SPs在选择性和保留方面的互补性。
Phosphonium-based ionic liquids (ILs) have proven to be successful stationary phases (SPs) for gas chromatography (GC) in several fields of application because of their unique selectivity and good chromatographic properties. This study focuses on the use of two ILs as GC SPs that are based on the phosphonium derivatives trihexyl(tetradecyl)phosphonium chloride ([P66614+] [Cl−]), and trihexyl(tetradecyl)phosphonium bis[(trifluoromethyl)sulfonyl]imide ([P66614+][NTf2−]), which have previously been shown to be complementary in terms of chromatographic selectivity and retention. Their application in routine analysis has been limited by their lower maximum allowable operating temperatures (MAOT) (200 °C for the [P66614+][Cl−] IL and 180 °C for [P66614+][NTf2−]), which restricts their use to samples that consist of analytes with relatively high volatility. A previous study carried out in the Authors’ laboratory focused on extending the use of the [P66614+][Cl−] IL SP to the analysis of samples with analytes of medium-to-low volatility by optimizing column characteristics and operative conditions. This study addresses the immobilization of both the [P66614+][Cl−] and [P66614+][NTf2−] ILs to the inner wall of fused silica columns to increase their MAOT under soft and hard reaction conditions. The resulting MAOT depended on more or less drastic immobilization conditions, and reached 220 °C for soft immobilization (So-Im) and 240 °C for hard immobilization (Ha-Im) in the [P66614+][Cl−] IL columns, and 200 °C forSo-Imand 220° forHa-Imin columns coated with the [P66614+] [NTf2−] IL. The influence of immobilization on the separation power and performance of all the columns has been evaluated using i) the Grob test, ii) a model mixture of 41 compounds of different polarity, structure, and with different organic functional groups representative of the flavor and fragrance field, iii) a standard mixture of 37 fatty acid methyl esters, iv) the peppermint essential oil, v) two mixtures of sesquiterpenic alcohols (farnesols and santalols), and vi) a standard mixture of 16 pesticides. These test samples were also used to demonstrate the complementarity of the two phosphonium-based IL SPs in terms of selectivity and retention.