Shortcomings of protein removal prior to high performance liquid chromatographic analysis - A case study using method development for BAY 11-7082

During the analytical method development for BAY 11-7082 ((E)-3-[4-methylphenylsulfonyl]-2-propenenitrile), using HPLC-MS-MS and HPLC-UV, we observed that the protein removal process (both ultrafiltration and precipitation method using organic solvents) prior to HPLC brought about a significant reduction in the concentration of this compound. The use of a structurally similar internal standard, BAY 11-7085 ((E)-3-[4-t-butylphenylsulfonyl]-2-propenenitrile), was not effective in compensating for the loss of analyte as the extent of reduction was different to that of the analyte. We present here a systematic investigation of this problem and a new validated method for the determination of BAY 11-7082. (c) 2006 Elsevier B.V. All rights reserved.

Glazing to entry, Mt. Nebo House

Leadlight windows with stained glass feature panes and timber muntins over french doors with matching leadlight sidelights.

Dining room, Mt. Nebo House

Interior view showing fireplace and mezzanine.

Hallway, Mt. Nebo House

Hallway off main entry to house.

Dormer window, Mt. Nebo House

Arched head leadlight and casement windows with stained glass feature panes and timber muntins. View through window from interior.

Dormer window, Mt. Nebo House

Arched head leadlight window with stained glass feature panes and timber muntins.

Garage-studio interior, Mt. Nebo House

Timber framing and roof skylight detail inside garage-studio.

Upper level, C House, Coorparoo, Brisbane

View along North-West elevation upper level.