Characterization of stationary phases based on polysiloxanes thermally immobilized onto silica and metalized silica using supercritical fluid chromatography with the solvation parameter model
Characterization of stationary phases based on polysiloxanes thermally immobilized onto silica and metalized silica using supercritical fluid chromatography with the solvation parameter model
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DOI：
10.1016/j.chroma.2013.09.055
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发表时间：
2013-11-08
影响因子：
4.1
通讯作者：
West, Caroline
中科院分区：
文献类型：
--
作者：
da Silva, Carla G. A.;Collins, Carol H.;West, Caroline
通过将聚合物固定在二氧化硅或金属化二氧化硅上制备的固定相（SP）由于更好地保护残留的硅烷醇或刘易斯酸位点以及易于制备而被用于反相高效液相色谱（RP-HPLC）中。另一方面，在填充柱超临界流体色谱（SFC）中使用这样的相之前没有报道。十四个不同的SP的基础上的聚硅氧烷（苯基，C1，C8，C14，C18）热固定到不同的支持（二氧化硅，钛化二氧化硅，锆化二氧化硅）和一个化学键合和封端的C18固定相具有双锆化二氧化硅支持，其特征在于具有相同的SFC条件（CO2与10%的甲醇，25摄氏度，15.0 MPa的背压）。基于对85种测试化合物测量的保留因子和线性溶剂化能关系（LSER）（即基于Abraham描述符的溶剂化参数模型）实现表征。将聚硅氧烷SP与商业C18键合二氧化硅（Kromasil C18）以及天然二氧化硅和金属化二氧化硅载体进行比较，以更好地阐明固定相化学对色谱行为的影响。共比较了19个固定相。结果突出了由柱组提供的极性的多样性。的聚硅氧烷主链有助于显着的SP极性证明了一个经典的烷基烷烃键合SP的比较。金属化也似乎修改SP的极性特性，特别是对碱性化合物。示例应用说明了这些SP在SFC中对制药和化妆品行业感兴趣的化合物分析的适用性。(C)2013 Elsevier B. V.保留所有权利。
Stationary phases (SP) prepared by immobilization of polymers on silica or metalized silica are interesting for use in reversed-phase high-performance liquid chromatography (RP-HPLC) due to better protection of residual silanols or Lewis acid sites, as well as ease of preparation. On the other hand, there are no previous reports of the use of such phases in packed column supercritical fluid chromatography (SFC). Fourteen different SPs based on polysiloxanes (phenyl, C1, C8, C14, C18) thermally immobilized onto different supports (silica, titanized silica, zirconized silica) and one chemically bonded and end-capped C18 stationary phase having a doubly zirconized silica support, were characterized with identical SFC conditions (CO2 with 10% of methanol, 25 degrees C, 15.0 MPa backpressure). Characterization was achieved based on retention factors measured for 85 test compounds and linear solvation energy relationships (LSER), namely the solvation parameter model based on Abraham descriptors. The polysiloxane SP were compared to a commercial C18-bonded silica (Kromasil C18), and to the native silica and metalized silica supports to better unravel the effects of stationary phase chemistry on chromatographic behavior. Together, 19 stationary phases were compared. The results highlight the variety of polarities provided by the column set. The polysiloxane backbone contributes significantly to the SP polarity as evidenced by the comparison to a classical alkylsiloxane-bonded SP. Metalization also appears to modify the polar characteristics of the SP, particularly toward basic compounds. Sample applications illustrate the applicability of these SP in SFC to the analysis of compounds of interest to the pharmaceutical and cosmetic industries. (C) 2013 Elsevier B.V. All rights reserved.