Biomaterial Database

Evaluation of automated micro solid phase extraction tips (micro-SPE) for the validation of a LC-MS/MS bioanalytical method. 2006

Jim X Shen, and Cristina I Tama, and Roger N Hayes

Schering-Plough Research Institute, 181 Passaic Ave, Summit, NJ 07091, United States.

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.

UI	MeSH Term	Description	Entries
D002853	Chromatography, Liquid	Chromatographic techniques in which the mobile phase is a liquid.	Liquid Chromatography
D000818	Animals	Unicellular or multicellular, heterotrophic organisms, that have sensation and the power of voluntary movement. Under the older five kingdom paradigm, Animalia was one of the kingdoms. Under the modern three domain model, Animalia represents one of the many groups in the domain EUKARYOTA.	Animal,Metazoa,Animalia
D001331	Automation	Controlled operation of an apparatus, process, or system by mechanical or electronic devices that take the place of human organs of observation, effort, and decision. (From Webster's Collegiate Dictionary, 1993)	Automations
D014230	Triazoles	Heterocyclic compounds containing a five-membered ring with two carbon atoms and three nitrogen atoms with the molecular formula C2H3N3.	Triazole
D015203	Reproducibility of Results	The statistical reproducibility of measurements (often in a clinical context), including the testing of instrumentation or techniques to obtain reproducible results. The concept includes reproducibility of physiological measurements, which may be used to develop rules to assess probability or prognosis, or response to a stimulus; reproducibility of occurrence of a condition; and reproducibility of experimental results.	Reliability and Validity,Reliability of Result,Reproducibility Of Result,Reproducibility of Finding,Validity of Result,Validity of Results,Face Validity,Reliability (Epidemiology),Reliability of Results,Reproducibility of Findings,Test-Retest Reliability,Validity (Epidemiology),Finding Reproducibilities,Finding Reproducibility,Of Result, Reproducibility,Of Results, Reproducibility,Reliabilities, Test-Retest,Reliability, Test-Retest,Result Reliabilities,Result Reliability,Result Validities,Result Validity,Result, Reproducibility Of,Results, Reproducibility Of,Test Retest Reliability,Validity and Reliability,Validity, Face
D051381	Rats	The common name for the genus Rattus.	Rattus,Rats, Laboratory,Rats, Norway,Rattus norvegicus,Laboratory Rat,Laboratory Rats,Norway Rat,Norway Rats,Rat,Rat, Laboratory,Rat, Norway,norvegicus, Rattus
D052617	Solid Phase Microextraction	A solventless sample preparation method, invented in 1989, that uses a fused silica fiber which is coated with a stationary phase. It is used for sample cleanup before using other analytical methods.	Microextraction, Solid Phase,Solid Phase Microextractions
D053719	Tandem Mass Spectrometry	A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection.	Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem