A novel bistrimethoxysilylethane hydrolysis aminopropyltrimethoxysilane (BTME-H-APS) silica stationary phase was prepared through a three-step vapour deposition method. Compared to the toluene bonding method, the vapour deposition route has the benefits of lower organic solvent consumption and easy process controlling. The structure of the hybrid modified silica substrate was characterized by Fourier transform infrared spectroscopy and solid-state ¹³C CP/MAS NMR. Following elemental analysis, the surface density of the amine group was calculated at 3.44 μmol m⁻², which is similar to the value of the commercial amine phase. The BTME-H-APS stationary phase exhibited a higher hydrothermal stability and longer service life at high alkaline conditions, due to the relative higher carbon loading and cross-linking degree of the BTME-H-APS phase, which was confirmed by the solid-state ²⁹Si NMR analysis. Then, the chromatographic evaluation demonstrated an equal, or even higher, separation ability in mixed-mode hydrophilic interaction liquid chromatography (HILIC)/reversed-phase liquid chromatography (RPLC), normal-phase liquid chromatography (NPLC) and ion-exchange chromatography (IEC) models on BTME-H-APS compared with a conventional amine column. The BTME-H-APS phase was successfully applied to the separation of carbohydrates in honey for authenticity identification. This bistrimethoxysilylethane hybrid organosilane method reported here can be further applied in the preparation of other stationary phases with increased hydrothermal stability.

中文翻译：

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气相沉积法制备的新型高水热稳定性氨基官能化固定相

通过三步气相沉积法制备了新型的双三甲氧基甲硅烷基乙烷水解氨基丙基三甲氧基硅烷（BTME-H-APS）硅胶固定相。与甲苯键合法相比，气相沉积法具有较低的有机溶剂消耗和易于控制的优点。通过傅立叶变换红外光谱和固态¹³ C CP / MAS NMR表征了杂化改性二氧化硅基质的结构。经过元素分析，胺基的表面密度经计算为3.44μmolm ^-2，类似于商业胺相的价值。由于BTME-H-APS相的相对较高的碳载量和交联度，因此BTME-H-APS固定相在高碱性条件下表现出更高的水热稳定性和更长的使用寿命，这被固相状态²⁹Si NMR分析。然后，色谱评估表明，混合模式亲水相互作用液相色谱（HILIC）/反相液相色谱（RPLC），正相液相色谱（NPLC）和离子交换色谱（与传统胺柱相比，BTME-H-APS上的IEC）模型。BTME-H-APS相已成功应用于蜂蜜中碳水化合物的分离，以进行真伪鉴定。本文报道的这种双三甲氧基甲硅烷基乙烷杂化有机硅烷方法可进一步用于制备具有更高水热稳定性的其他固定相。