本文選題：親水作用色譜 + 固定相�。� 參考：《分析化學(xué)》2017年05期

【摘要】：以甲基丙烯酰氧乙基二甲基乙酸銨(CBMA)為功能單體,利用表面引發(fā)原子轉(zhuǎn)移自由基聚合(Surface-initiated atom transfer radical polymerization,SI-ATRP)技術(shù),將CBMA接枝到硅膠表面,得到接枝聚合物CBMA的親水作用色譜固定相(Silica-CBMA)。通過(guò)改變SI-ATRP反應(yīng)體系中單體的濃度,制備了3種不同接枝量的親水作用色譜固定相�？疾炝薙ilica-CBMA固定相對(duì)有機(jī)酸類(lèi)化合物的分離性能以及流動(dòng)相中pH值、鹽濃度、水含量等因素對(duì)溶質(zhì)保留行為的影響。結(jié)果表明,在親水作用色譜模式下,Silica-CBMA固定相對(duì)有機(jī)酸類(lèi)化合物的分離是離子交換作用與親水作用的混合色譜模式。流動(dòng)相中鹽濃度增大,溶質(zhì)保留減弱,符合離子交換作用特征;固定相和溶質(zhì)的離子化程度受流動(dòng)相pH值影響較大,pH值增大,溶質(zhì)保留增強(qiáng);而溶質(zhì)的保留時(shí)間隨流動(dòng)相水含量增加而降低則是典型的親水作用色譜特征。使用自制Silica-CBMA柱,建立了蘆丁片中維生素C、蘆丁含量的親水作用色譜測(cè)定方法,操作方法簡(jiǎn)單,為強(qiáng)極性樣品的分離測(cè)定提供了新方法。
[Abstract]:Using methacryloxy ethyl dimethylammonium acetate (CBMA) as the functional monomer, the surface initiated atom transfer radical polymerization (SI-ATRP) technique was used to graft CBMA onto the silica gel surface to obtain the hydrophilic chromatographic stationary phase (Silica-CBMA) of the grafted polymer CBMA. By changing the concentration of monomer in SI-ATRP reaction system, three kinds of hydrophilic interaction chromatographic stationary phases with different grafting amount were prepared. The separation performance of Silica-CBMA fixed relative organic acids and the effects of pH value, salt concentration and water content in the mobile phase on the retention behavior of solute were investigated. The results showed that the separation of organic acids fixed by Silica-CBMA was a mixed chromatographic model of ion exchange and hydrophilicity under hydrophilic interaction chromatography mode. The concentration of salt in the mobile phase increased, the retention of solute weakened, and the ionization degree of the stationary phase and the solute was greatly affected by the pH value of the mobile phase, and the retention of solute increased. The retention time of solute decreases with the increase of water content in the mobile phase, which is a typical hydrophilic chromatographic feature. A hydrophilic chromatographic method for the determination of vitamin C and rutin in rutin tablets was established by using a self-made Silica-CBMA column. The method is simple and provides a new method for the separation and determination of highly polar samples.
【作者單位】： 寧夏大學(xué)化學(xué)化工學(xué)院;北方民族大學(xué)化學(xué)與化學(xué)工程學(xué)院;
【基金】：國(guó)家自然科學(xué)基金項(xiàng)目(No.31360077) 寧夏自然科學(xué)基金項(xiàng)目(No.NZ13045)資助~~
【分類(lèi)號(hào)】：O657.7

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