Chemical anchoring of lauryl methacrylate-based reversed phase monolith to 1/16" o.d. polyetheretherketone tubing
Chemical anchoring of lauryl methacrylate-based reversed phase monolith to 1/16" o.d. polyetheretherketone tubing
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DOI：
10.1016/j.chroma.2012.04.030
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发表时间：
2012-06-15
影响因子：
4.1
通讯作者：
Umemura, Tomonari
中科院分区：
文献类型：
--
作者：
Shu, Shin;Kobayashi, Hiroharu;Umemura, Tomonari
在本文中，我们描述了一种制备易于使用的反相整体微孔柱的方法。使用外径为1/16 "、内径为1.0 mm的聚醚醚酮（PEEK）管作为柱壳（空柱），其中甲基丙烯酸月桂酯（LMA）与二甲基丙烯酸乙烯酯（EDMA）共聚。为了将聚合物整料化学锚在管壁上，通过以下两步程序预处理内壁表面。(1)将50%硫酸填充到PEEK管中并静置6小时以在表面上产生磺酸根基团。(2)在用Milli-Q水洗涤后，使磺化的PEEK表面与二氯甲烷（或丙酮）中的IM甲基丙烯酸缩水甘油酯在40 ° C下接触4小时，以经由磺酸酯基团和环氧基团的反应引入甲基丙烯酰基。通过在乙腈-水（50：50，v/v）洗脱液中在50-750 μ L/min（对应于1.7-25.5 mm/s）的流速范围内分离一系列烷基苯来评价所得整料的机械强度和柱效率。聚（LMA-co-EDMA）整料提供2000理论塔板/10 cm的可接受柱效率戊基苯（HETP值为50 μ m）（分离因子k = 40）和在50 μ L/min的正常流速下0.5MPa/10 cm的低流动阻力。甲基丙烯酰化的PEEK管紧紧地保持整料，整体柱具有良好的耐压性能，最高可达15 MPa。允许以比正常高15-20倍的流速快速分离。(C)2012爱思唯尔有限公司版权所有。
In this paper, we describe a method for the preparation of easy-to-use reversed-phase monolithic microbore columns. Polyetheretherketone (PEEK) tubing with an outer diameter of 1/16 '' and an inner diameter of 1.0 mm was used as a column housing (empty column), and in it lauryl methacrylate (LMA) was copolymerized with ethylene dimethacrylate (EDMA). In order to chemically anchor the polymer monolith to the tube wall, the inner wall surface was pretreated by the following two-step procedure. (1) 50% sulfuric acid was filled into the PEEK tubing and left to stand for 6 h to generate sulfonate groups on the surface. (2) After washing with Milli-Q water, the sulfonated PEEK surface was brought into contact with 1 M glycidyl methacrylate in dichloromethane (or acetone) at 40 degrees C for 4 h to introduce methacryloyl groups via the reaction of sulfonate groups and epoxy groups. Mechanical strength and column efficiency of the resulting monoliths were evaluated through the separation of a series of alkylbenzenes in acetonitrile-water (50:50, v/v) eluent over the flow rate range of 50-750 mu L/min (corresponding to 1.7-25.5 mm/s). The poly(LMA-co-EDMA) monolith provided acceptable column efficiency of 2000 theoretical plates/10 cm (HETP value of 50 mu m) for amylbenzene (separation factor k = 40) and low flow resistance of 0.5 MPa/10 cm at a normal flow rate of 50 mu L/min. The methacryloylated PEEK tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 15 MPa. allowing rapid separation at a 15-20 fold higher flow rate than normal. (C) 2012 Elsevier B.V. All rights reserved.