title: Poly(cyclooctene)-based monolithic columns for capillary high performance liquid chromatography prepared via ring-opening metathesis polymerization.
abstract: Monolithic columns for capillary HPLC were prepared via ring-opening metathesis polymerization (ROMP) from cis-cyclooctene (COE), tris(cyclooct-4-enyl-1-oxy)methylsilane (CL) as monomers, 2-propanol and toluene as porogens and RuCl(2)(Py)(2)(IMesH(2))(CHC(6)H(5)) (Py=pyridine, IMesH(2)=1,3-dimesityl-4,5-dihydroimidazolin-2-ylidene) as initiator within the confines of 200 microm i.d. fused silica columns. For evaluation of the novel monolithic capillary HPLC columns, a protein standard consisting of six proteins in the molecular weight range of 5800-66000 g/mol, i.e. ribonuclease A, insulin, albumin, lysozyme, myoglobin and beta-lactoglobulin, was used. Reproducibility of synthesis was checked by determining the relative standard deviation (RSD) in retention times (t(R)), which was found to be in the range of 2.9-3.9% for all analytes. Variations in polymer kinetics were realized by adding different amounts of free pyridine and had a significant influence on the monolith's morphology, the backpressure and retention times. On the contrary, variations in monomer content and COE to CL ratio showed only minor changes on these parameters. Long-term stability of 1000 runs at 50 degrees C showed excellent stability of the columns and no significant alteration in separation performance was observed in combination with slightly decreased retention times (approx. 1.6-7.2% for all analytes).
authors.affiliation: Leibniz Institut für Oberflächenmodifizierung e.V. (IOM), Permoserstrasse 15, D-04318 Leipzig, Germany.
authors.forename: Bettina
authors.initials: B
authors.lastname: Schlemmer
authors.forename: Christina
authors.initials: C
authors.lastname: Gatschelhofer
authors.forename: Thomas R
authors.initials: TR
authors.lastname: Pieber
authors.forename: Frank M
authors.initials: FM
authors.lastname: Sinner
authors.forename: Michael R
authors.initials: MR
authors.lastname: Buchmeiser
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods*; D004355:Drug Stability; D006536:Heptanes / Q000737:chemistry*; D008854:Microscopy, Electron / Q000379:methods; D015394:Molecular Structure; D009281:Naphthalenes / Q000737:chemistry*; D011108:Polymers / Q000138:chemical synthesis* / Q000737:chemistry; D016062:Porosity; D011506:Proteins / Q000032:analysis; D015203:Reproducibility of Results
chemical_list: D006536:Heptanes; D009281:Naphthalenes; D011108:Polymers; D011506:Proteins