The potential of serially coupled alkyl-bonded silica monolithic columns for high resolution separations of pharmaceutical compounds in biological fluids |
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Authors: | G J Dear D N Mallett D M Higton A D Roberts S A Bird H Young R S Plumb I M Ismail |
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Institution: | (1) Structural Identification Group, DMPK Division, GlaxoSmithKline Research and Development, Park Road, SG12 0RZ Ware, Herts, UK |
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Abstract: | Summary In this paper we investigate the potential of alkyl-bonded silica monolithic columns for the isolation and identification
of drug-related components in biological fluids. Up to 6 columns have been connected in series to produce a chromatographic
system with up to 40,000 plates. This high-resolution chromatography system has been coupled to both MS and NMR to enable
efficient detection and characterisation of drug-related components in biological fluids. The use of six coupled columns has
been shown to give enhanced resolution over a high quality silica particulate column packed with 3 μm material which exhibits
the same back pressure. The effect of volume and mass load on the performance of monolithic columns for semi-preparative chromatography
of biological fluids has also been investigated. In these studies it was possible to inject up to 100 mL of neat urine with
no loss of chromatographic performance. Furthermore, upon re-testing, the columns showed similar chromatographic performance.
Again several columns were serially connected, producing enhanced resolution in the semi-preparative mode. |
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Keywords: | Column liquid chromatography Monolithic columns MS and NMR detection Drugs in biological fluids Comparison with conventional packed columns |
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