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PredicateObject
rdf:type
lifeskim:mentions
pubmed:issue
5
pubmed:dateCreated
2010-1-29
pubmed:abstractText
A sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method, followed by a 96-well protein precipitation, has been developed and fully validated for the determination of Phakellistatin 13 (PK13), a new cyclic heptapeptide isolated from the sponge Phakellia fusca Thiele, in rat plasma. After protein precipitation of the plasma samples (50 microL) in a 96-well plate by methanol (200 microL) containing the internal standard Pseudostellarin B (20 ng/mL), the plate was vortex mixed for 3 min. Following filtration for 5 min, the filtrate was directly injected into the LC-MS/MS system. The analytes were separated on an XB-C18 analytical column (5 microm, 50 mm x 4.6 mm i.d.) using an eluent of methanol-water (85:15, v/v) and detected by electrospray ionization mass spectrometry in the negative multiple reaction monitoring mode with a chromatographic run time of 5.0 min. The method was sensitive with a lower limit of quantification (LLOQ) of 0.1 ng/mL, with good linearity (r > 0.999) over the quantitation range of 0.1-5 ng/mL. The validation results demonstrated that this method was significantly specific, accurate, precise, and was successfully applied in measuring levels of PK13 in rat plasma following intravenous administration of 20, 50, and 100 microg/kg of peptide in rats, respectively, which was suitable for the preclinical pharmacokinetic studies on PK13.
pubmed:language
eng
pubmed:journal
pubmed:citationSubset
IM
pubmed:chemical
pubmed:status
MEDLINE
pubmed:month
Nov
pubmed:issn
1618-2650
pubmed:author
pubmed:issnType
Electronic
pubmed:volume
395
pubmed:owner
NLM
pubmed:authorsComplete
Y
pubmed:pagination
1461-9
pubmed:meshHeading
pubmed:year
2009
pubmed:articleTitle
Quantitative determination of Phakellistatin 13, a new cyclic heptapeptide, in rat plasma by liquid chromatography/tandem mass spectrometry: application to a pharmacokinetic study.
pubmed:affiliation
Shanghai Key Laboratory for Pharmaceutical Metabolite Research, Shanghai Research Center for Drug (Chinese Materia Medica) Metabolism, School of Pharmacy, Second Military Medical University, No.325 Guohe Road, Shanghai 200433, China.
pubmed:publicationType
Journal Article, Research Support, Non-U.S. Gov't, Evaluation Studies