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Schlemmer, B; Gatschelhofer, C; Pieber, TR; Sinner, FM; Buchmeiser, MR.
Poly(cyclooctene)-based monolithic columns for capillary high performance liquid chromatography prepared via ring-opening metathesis polymerization.
J Chromatogr A. 2006; 1132(1-2):124-131 Doi: 10.1016/j.chroma.2006.07.058
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Leading authors Med Uni Graz
Sinner Frank Michael
Co-authors Med Uni Graz
Gatschelhofer Christina
Pieber Thomas
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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).
Find related publications in this database (using NLM MeSH Indexing)
Chromatography, High Pressure Liquid - instrumentation
Chromatography, High Pressure Liquid - methods
Drug Stability -
Heptanes - chemistry
Microscopy, Electron - methods
Molecular Structure -
Naphthalenes - chemistry
Polymers - chemical synthesis
Polymers - chemistry
Porosity -
Proteins - analysis
Reproducibility of Results -

Find related publications in this database (Keywords)
monolithic media
ring-opening metathesis polymerization (ROMP)
capillary HPLC
proteins
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