title: A systematic investigation of recovery in preparative reverse phase high performance liquid chromatography/mass spectrometry.
abstract: In this paper we report a systematic recovery study based on reversed phase high performance liquid chromatography (RP-HPLC) separation and mass spectrometric (MS) based fractionation. Factors including a compound's physicochemical properties, column mass loading and presence of impurities were investigated through commercially available compounds. Results suggest that the delay time between MS peak detection and fraction collection, fraction detector's signal-to-noise ratio and compound's base peak width in the chromatogram have the biggest impacts on purification recovery. In an effort to assess sample recovery within our high throughput purification process, re-purification was performed on four compound libraries that were synthesized in-house. Reproducible recoveries (>80%) were achieved in all tests.
authors.affiliation: ArQule, Inc., Woburn, MA 01801, USA.
authors.forename: Xu
authors.initials: X
authors.lastname: Zhang
authors.forename: Wendy
authors.initials: W
authors.lastname: Picariello
authors.forename: Nicole
authors.initials: N
authors.lastname: Hosein
authors.forename: Marc
authors.initials: M
authors.lastname: Towle
authors.forename: Wolfgang
authors.initials: W
authors.lastname: Goetzinger
mesh_terms: D000086:Acetazolamide / Q000302:isolation & purification; D002074:Butanones; D055598:Chemical Phenomena; D002627:Chemistry, Physical; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003348:Cortisone / Q000302:isolation & purification; D013058:Mass Spectrometry / Q000379:methods*; D000077430:Nabumetone; D004364:Pharmaceutical Preparations / Q000302:isolation & purification; D014295:Trimethoprim / Q000302:isolation & purification
chemical_list: D002074:Butanones; D004364:Pharmaceutical Preparations; D014295:Trimethoprim; D000077430:Nabumetone; D000086:Acetazolamide; D003348:Cortisone