Li Hengye, Zhang Xuemeng, Zhang Lin, Wang Xiaojin, Kong Fenying, Fan Dahe, Li Lei, Wang Wei
School of Chemistry and Chemical Engineering, Yancheng Institute of Technology, Yancheng, Jiangsu, 224000, China.
Yancheng Entry-Exit Inspection and Quarantine Bureau, Yancheng, 224000, China.
Anal Chim Acta. 2017 Apr 15;962:104-113. doi: 10.1016/j.aca.2017.01.028. Epub 2017 Jan 30.
A silica stationary phase was designed and synthesized through the co-functionalization of silica with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography applications. The as-synthesized stationary phase was characterized by elemental analysis and Fourier Transform-InfraRed Spectroscopy (FT-IR). Retention mechanisms, including boronate affinity (BA), reversed-phase (RP) and anion-exchange (AE), were involved. Retention mechanism switching was easily realized by adjustment of the mobile phase constitution. Cis-diol compounds could be selectively captured under neutral conditions in BA mode and off-line separated in RP mode. Neutral, basic, acidic and amphiprotic compounds were chromatographed on the column in RP chromatography, while inorganic anions were chromatographed in AE chromatography to characterize the mixed-mode nature of the prepared stationary phase. In addition, the RP performance was compared with an octadecyl silica column in terms of column efficiency (N/m), asymmetry factor (A), retention factor (k) and resolution (Rs). The prepared stationary phase offered multiple interactions with analytes in addition to hydrophobic interactions under RP elution conditions. Based on the mixed-mode properties, off-line 2D-LC, for selective capture and separation of urinary nucleosides, was successfully realized on a single column, demonstrating its powerful application potential for complex samples.
通过硅与乌尔夫型苯基硼酸酯和C12的共官能化设计并合成了一种用于混合模式液相色谱应用的硅胶固定相。通过元素分析和傅里叶变换红外光谱（FT-IR）对合成的固定相进行了表征。涉及的保留机制包括硼酸酯亲和力（BA）、反相（RP）和阴离子交换（AE）。通过调整流动相组成可以轻松实现保留机制的切换。顺式二醇化合物可以在BA模式下在中性条件下被选择性捕获，并在RP模式下离线分离。中性、碱性、酸性和两性化合物在RP色谱中在该柱上进行色谱分析，而无机阴离子在AE色谱中进行色谱分析，以表征所制备固定相的混合模式性质。此外，在柱效（N/m）、不对称因子（A）、保留因子（k）和分离度（Rs）方面，将RP性能与十八烷基硅胶柱进行了比较。在所制备的固定相在RP洗脱条件下，除了疏水相互作用外，还与分析物提供了多种相互作用。基于混合模式特性，在单柱上成功实现了用于选择性捕获和分离尿核苷的离线二维液相色谱，证明了其对复杂样品的强大应用潜力。
