SYNTHESIS AND CHARACTERIZATION OF HIGHLY STABLE BONDED PHASES FOR HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY COLUMN PACKINGS
SYNTHESIS AND CHARACTERIZATION OF HIGHLY STABLE BONDED PHASES FOR HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY COLUMN PACKINGS
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DOI：
10.1021/ac00176a003
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发表时间：
1989-01-01
影响因子：
7.4
通讯作者：
FARLEE, RD
中科院分区：
文献类型：
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作者：
KIRKLAND, JJ;GLAJCH, JL;FARLEE, RD
合成了两种新型硅烷改性二氧化硅，并用色谱和光谱技术对其进行了表征。这些新的键合相明显比以前的键合相硅更稳定地水解；保留和色谱柱效率是可比的。第一种类型使用双功能（或“双齿”）硅烷，其中两个硅原子上各含有一个反应性原子，通过桥接基团（如- o -或-(CH2)n-）连接。第二种类型使用在硅烷原子上具有至少两个大基团（例如，异丙基）的单官能硅烷。这些庞大的基团为硅烷和二氧化硅表面之间形成的Si-O-Si键提供空间保护。新型键合相二氧化硅在低ph流动相中具有高重复性的梯度洗脱和高效液相色谱分离多肽和蛋白质。
Two new classes of silane-modified silicas were synthesized and characterized by chromatographic and spectroscopic techniques. These new bonded phases are significantly more stable toward hydrolysis than previous bonded-phase silicas; retention and column efficiency are comparable. The first type uses bifunctional (or "bidentate") silanes containing one reactive atom on each of two silicon atoms that connect through a bridging group such as -O- or -(CH2)n-. The second type uses a monofunctional silane with at least two bulky groups (e.g., isopropyl) on the silane atom. These bulky groups provide steric protection to the Si-O-Si bond formed between the silane and the surface of the silica. The new bonded-phase silicas exhibit highly reproducible gradient elution high-performance liquid chromatography separations of peptides and proteins with low-pH mobile phases.