Chemical anchoring of lauryl methacrylate-based reversed phase monolith to 1/16鈥?o.d. polyetheretherketone tubing

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• 作者：Shin Shu^a ; Hiroharu Kobayashi^a ; Masaki Okubo^a ; Akhmad Sabarudin^a ; Michio Butsugan^b ; Tomonari Umemura^a ; ^{umemura@apchem.nagoya-u.ac.jp}
• 关键词：Reversed-phase HPLC ; PEEK ; Organic polymer monolith ; Microbore column ; Lauryl-methacrylate
• 刊名：Journal of Chromatography A
• 出版年：2012
• 期刊代码：47_00219673
• 类别：ch
• 出版时间：15 June, 2012
• 卷：1242
• 期：Complete
• 页码：59-66
• 文件大小：885 K

摘要

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鈥?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 掳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 渭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 渭m) for amylbenzene (separation factor k = 40) and low flow resistance of 0.5 MPa/10 cm at a normal flow rate of 50 渭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.