Preparation of methacrylate-based monolith for capillary hydrophilic interaction chromatography and its application in determination of nucleosides in urine
Preparation of methacrylate-based monolith for capillary hydrophilic interaction chromatography and its application in determination of nucleosides in urine
复制标题
毛细管亲水相互作用色谱甲基丙烯酸酯整体柱的制备及其在尿液中核苷测定中的应用
DOI：
10.1016/j.chroma.2011.07.061
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发表时间：
2012-03-09
影响因子：
4.1
通讯作者：
Feng, Yu-Qi
中科院分区：
文献类型：
--
作者：
Chen, Ming-Luan;Wei, Shan-Shan;Feng, Yu-Qi
在100 μ m i.d.的条件下制备了一种新型的聚（N-丙烯酰三（羟甲基）氨基甲烷-co-季戊四醇三丙烯酸酯）（NAHAM-co-PETA）整体柱。毛细管，并研究了毛细管液相色谱法（cLC）。以聚乙二醇（PEG）为致孔剂，二甲基亚砜（DMSO）为溶剂，通过原位聚合法合成了NAHAM和PETA聚合物整体柱。通过改变NAHAM与PETA的比例、PEG的分子量和用量，优化了整体柱的孔结构。为了评价所得聚合物整体柱的分离性能，选择几组模型化合物（包括核苷、苯甲酸和苯胺）进行cLC分离。结果表明，在优化的移动的相条件下，这些模型化合物可以在聚（NAHAM-co-PETA）整体柱上实现基线分离。对于丙烯酰胺，柱效率估计为87，000板/m。此外，该整体柱与在线固相微萃取（SPME）联用，用于尿液中尿苷、腺苷、胞苷、鸟苷的分析。该方法的检出限为40 ~ 52 ng/mL。通过评价日内和日间精密度获得方法重现性，相对标准偏差（RSD）分别小于8.3%和10.2%。加标尿样中目标分析物的回收率范围为86.5%-106.8%。(C)2011 Elsevier B. V.保留所有权利。
A novel poly(N-acryloyltris(hydroxymethyl)aminomethane-co-pentaerythritol triacrylate) (NAHAM-co-PETA) monolith was prepared in the 100 mu m i.d. capillary and investigated for capillary liquid chromatography (cLC). The polymer monolith was synthesized by in situ polymerization of NAHAM and PETA in the presence of polyethylene glycol (PEG) in dimethyl sulfoxide (DMSO) as the porogen. The porous structure of monolith was optimized by changing the ratio of NAHAM to PETA, the molecular weight and amount of PEG. To evaluate the separation performance of the resultant polymer monolith, several groups of model compounds (including nucleosides, benzoic acids and anilines) were selected to perform cLC separation. Our results showed that these model compounds can be baseline separated on the resultant poly(NAHAM-co-PETA) monolithic column with the optimized mobile phases. The column efficiency was estimated to be 87,000 plates/m for acrylamide. In addition, this monolithic column was coupled with on-line solid-phase microextraction (SPME) for the analysis of four nucleosides (uridine, adenosine, cytidine, guanosine) in urine. The limit of detection of the proposed method was in the range from 40 to 52 ng/mL. The method reproducibility was obtained by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) less than 8.3% and 10.2%, respectively. Recoveries of the target analytes from spiked urine samples were ranged from 86.5% to 106.8%. (C) 2011 Elsevier B.V. All rights reserved.