發(fā)布時(shí)間：2018-05-14 02:26

  本文選題：高效液相色譜 + 手性固定相�。� 參考：《色譜》2016年01期

【摘要】：高效液相色譜(HPLC)被廣泛認(rèn)為是分離制備光學(xué)純單一對(duì)映體的最有效方法。在高效液相色譜手性拆分中,手性固定相(CSP)的性能直接影響到色譜柱的手性分離能力。在眾多手性固定相中,鍵合型手性固定相具有溶劑耐受性好,分離模式靈活等優(yōu)點(diǎn),已經(jīng)發(fā)展成為一類(lèi)重要的手性固定相。本文通過(guò)兩步化學(xué)反應(yīng)合成了新型的光學(xué)活性丙烯酰胺衍生物——(S)-1-丙烯酰-2-(N-苯基甲酰胺基)吡咯烷((S)-APACP),采用核磁共振氫譜表征了(S)-APACP的化學(xué)結(jié)構(gòu);通過(guò)3步化學(xué)反應(yīng)制備了鍵合型聚丙烯酰胺衍生物手性固定相,采用熱重分析法表征了聚合物的鍵合量,采用HPLC評(píng)價(jià)了鍵合型手性固定相的識(shí)別能力,分析了影響其手性識(shí)別能力的因素。研究結(jié)果表明,APACP聚合物成功地鍵合到硅膠表面制備了具有良好溶劑耐受性的鍵合型手性固定相,其聚合物鍵合量為10.2%~11.8%,該鍵合型手性固定相對(duì)若干種對(duì)映體顯示了較好的手性識(shí)別能力。
[Abstract]:High performance liquid chromatography (HPLC) is widely regarded as the most effective method for the separation and preparation of optical pure enantiomers. In high performance liquid chromatography (HPLC) chiral resolution, the performance of chiral stationary phase (CSP) has a direct impact on the chiral separation ability of the column. Among the many chiral stationary phases, the bonded chiral stationary phase has been developed into an important chiral stationary phase because of its good solvent tolerance and flexible separation mode. In this paper, a new type of acrylamide derivative, Szoc-1-acrylyl-2-N-phenylformamide, was synthesized by two-step chemical reaction. The chemical structure of Sn-APACP was characterized by nuclear magnetic resonance spectroscopy (NMR). The chiral stationary phase of bonded polyacrylamide derivatives was prepared by three steps chemical reaction. The amount of polymer was characterized by thermogravimetric analysis and the recognition ability of bonded chiral stationary phase was evaluated by HPLC. The factors affecting chiral recognition ability were analyzed. The results show that APACP polymers have been successfully bonded to silica gel surface to prepare a good solvent-tolerant bonded chiral stationary phase. The amount of polymer bonding is 10.2 and 11.8.The chiral fixation of the bonding type shows good chiral recognition ability relative to several enantiomers.
【作者單位】： 哈爾濱工程大學(xué)材料科學(xué)與化學(xué)工程學(xué)院;日本名古屋大學(xué);
【基金】：國(guó)家自然科學(xué)基金項(xiàng)目(51103030) 黑龍江省自然科學(xué)基金項(xiàng)目(E201419) 哈爾濱市科技創(chuàng)新人才研究專(zhuān)項(xiàng)(2013RFLXJ027) 日本大賽璐公司合作研究基金~~
【分類(lèi)號(hào)】：O652.63

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本文編號(hào)：1885921