title: Evaluation of automated micro solid phase extraction tips (micro-SPE) for the validation of a LC-MS/MS bioanalytical method.
abstract: Automated micro-SPE tips were successfully utilized for the determination of posaconazole in rat plasma. The bioanalytical method using micro-SPE tips was successfully qualified for routine quantitation of posaconazole over the concentration range of 10.0-10,000 ng/mL in rat EDTA plasma. Inter-assay precision, based on percent relative deviation for n=18 replicate quality controls, was < or =5.7%. Inter-assay accuracy based on n=18 replicate quality controls was +/-7.7%. Complete solid phase extraction using micro-SPE tips was demonstrated on a Tomtec liquid handler where >95% recovery for posaconazole was obtained. The micro-SPE tips had sufficient capacity to extract at least 100 microL plasma fortified with 10 microg/mL of posaconazole and the analyte could be efficiently eluted with as little as 60 microL of methanol. Of particular note is the unique ability of these micro-SPE tips to perform exhaustive solid phase extraction more commonly performed when using liquid/liquid extraction.
authors.affiliation: Schering-Plough Research Institute, 181 Passaic Ave, Summit, NJ 07091, United States.
authors.forename: Jim X
authors.initials: JX
authors.lastname: Shen
authors.forename: Cristina I
authors.initials: CI
authors.lastname: Tama
authors.forename: Roger N
authors.initials: RN
authors.lastname: Hayes
mesh_terms: D000818:Animals; D001331:Automation; D002853:Chromatography, Liquid / Q000379:methods*; D051381:Rats; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000295:instrumentation / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014230:Triazoles / Q000097:blood*
chemical_list: D014230:Triazoles; C101425:posaconazole