Cellulose tris(3,5-dimethylphenylcarbamate)-coated zirconia as a chiral stationary phase for HPLC.
Cellulose tris(3,5-dimethylphenylcarbamate)-coated zirconia as a chiral stationary phase for HPLC.
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纤维素三（3,5-二甲基苯基氨基甲酸酯）涂层氧化锆作为 HPLC 的手性固定相。
DOI：
10.1021/ac990021f
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发表时间：
1999
影响因子：
7.4
通讯作者：
Carr,PW
中科院分区：
文献类型：
--
作者：
Castells,CB;Carr,PW
本工作中，我们探索了用纤维素三（3，5-二甲基苯基氨基甲酸酯）（CDMPC）包覆的多孔氧化锆微粒作为手性化合物的高效液相色谱分离载体。预先烧结但未再羟基化的氧化锆表面为沉积手性聚合物提供了稳定的表面。用漫反射红外光谱法研究了氧化锆涂层前的表面，发现涂层在750 °C处理5 h后仍有羟基残留。系统地改变沉积的手性聚合物的量，并且通过氮吸附测定法评估所得颗粒的孔结构。还进行了填充有这些固定相的柱的动态研究。我们发现，填充有约3 - 4%（w/w）CDMPC（涂覆在2.5 μm氧化锆颗粒上）的色谱柱在负载需求（赋予固定相良好的手性识别能力）和色谱柱的色谱效率之间提供了极好的折衷。初步结果显示，在填充的5厘米柱中，16种外消旋混合物中有9种的分辨率高于1。使用较短的色谱柱并结合减小的粒度以提供足够的分辨率具有减少分析时间和减少洗脱液体积的优点。CDMPC涂层氧化锆柱在相对高的线速度下在正相条件下表现出高稳定性。
In this work we explore the use of microparticulate porous zirconia coated with cellulose tris(3,5-dimethylphenyl- carbamate) (CDMPC) as a support for separation of chiral compounds by HPLC. The surface of zirconia, previously sintered but not rehydroxylated, provides a stable surface for depositing the chiral polymer. Zirconia's surface prior to coating was investigated by diffuse reflectance FT-IR. The spectra indicate the presence of residual hydroxyl groups even after treatment at 750 °C for 5 h. The amount of chiral polymer deposited was systematically varied, and the pore structure of the resulting particles was assessed by nitrogen sorptometry. Dynamic studies of columns packed with these stationary phases were also conducted. We found that columns packed with about 3−4% (w/w) CDMPC coated on 2.5-μm zirconia particles provide an excellent compromise between loading need to impart good chiral recognition ability to the stationary phase and column's chromatographic efficiency. Preliminary results show resolutions higher than 1 for 9 out of 16 racemic mixtures in packed 5-cm columns. The use of shorter columns combined with reduced particle size to provide sufficient resolution has the advantage of decreasing the analysis times and reducing eluent volumes. CDMPC-coated zirconia columns exhibit high stability under normal-phase conditions at relatively high linear velocities.