Wei Qiuhong, Su Hongjiu, Gao Diannan, Wang Shudong
Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, P. R. China.
University of Chinese Academy of Sciences, Beijing, P. R. China.
Chirality. 2019 Mar;31(3):164-173. doi: 10.1002/chir.23044. Epub 2019 Jan 11.
Coating cellulose tris (3,5-dimethylphenylcarbamate) (CDMPC) on silica gels with large pores have been demonstrated as an efficient way for the preparation of chiral stationary phase (CSP) for high-performance liquid chromatography (HPLC). During the process, a number of parameters, including the type of coating solvent, amount of coating, and the method for subsequent solvent removing, have been proved to affect the performance of the resultant CSPs. Coating times and the concentration of coating solution, however, also makes a difference to CSPs' performance by changing the arrangement of cellulose derivatives while remaining the coating amount constant, have much less been studied before, and thereby, were systematically investigated in this work. Results showed that CSPs with more coating times exhibited higher chiral recognition and column efficiency, suggesting that resolution was determined by column efficiency herein. Afterwards, we also investigated the effect of coating amount on the performance of CSPs, and it was shown that the ability of enantio-recognition did not increase all the time as the coating amount; and four of seven racemates achieved best resolution when the coating amount reached to 18.37%. At the end, the reproducibility of CDMPC-coated CSPs were further confirmed by two methods, ie, reprepared the CSP-0.15-3 and reevaluated the effect of coating times.
在大孔硅胶上涂覆三（3,5-二甲基苯基氨基甲酸酯）纤维素（CDMPC）已被证明是制备高效液相色谱（HPLC）手性固定相（CSP）的有效方法。在此过程中，已证明许多参数，包括涂覆溶剂的类型、涂覆量以及后续溶剂去除方法，都会影响所得CSP的性能。然而，涂覆次数和涂覆溶液的浓度，在保持涂覆量不变的情况下，也会通过改变纤维素衍生物的排列对CSP的性能产生影响，此前对此研究较少，因此，本工作对此进行了系统研究。结果表明，涂覆次数较多的CSP表现出更高的手性识别能力和柱效，表明在此分辨率由柱效决定。之后，我们还研究了涂覆量对CSP性能的影响，结果表明对映体识别能力并非随涂覆量一直增加；七种外消旋体中有四种在涂覆量达到18.37%时达到最佳分离度。最后，通过两种方法进一步证实了CDMPC涂覆CSP的重现性，即重新制备CSP-0.15-3并重新评估涂覆次数的影响。
