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dc.contributor.authorCaspers, Michael J.
dc.contributor.authorWilliams, Todd D.
dc.contributor.authorLovell, Kimberly M.
dc.contributor.authorLozama, Anthony
dc.contributor.authorButelman, Eduardo R.
dc.contributor.authorKreek, Mary Jeanne
dc.contributor.authorJohnson, Matthew W.
dc.contributor.authorGriffiths, Roland R.
dc.contributor.authorMacLean, Katherine A.
dc.contributor.authorPrisinzano, Thomas E.
dc.date.accessioned2017-01-12T19:33:52Z
dc.date.available2017-01-12T19:33:52Z
dc.date.issued2014-12-21
dc.identifier.citationCaspers, Michael J., Todd D. Williams, Kimberly M. Lovell, Anthony Lozama, Eduardo R. Butelman, Mary Jeanne Kreek, Matthew Johnson, Roland Griffiths, Katherine Maclean, and Thomas E. Prisinzano. "LC-MS/MS Quantification of Salvinorin A from Biological Fluids." Analytical Methods 5.24 (2013): 7042.en_US
dc.identifier.urihttp://hdl.handle.net/1808/22618
dc.description.abstractA facile method for quantifying the concentration of the powerful and widely available hallucinogen salvinorin A (a selective kappa opioid agonist) from non-human primate cerebrospinal fluid (CSF) and human plasma has been developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization (ESI) mode. With CSF solid phase extraction can be avoided completely by simply diluting each sample to 10 % (v/v) acetonitrile, 1 % (v/v) formic acid and injecting under high aqueous conditions for analyte focusing. Extensive plasma sample preparation was investigated including protein precipitation, SPE column selection, and plasma particulate removal. Human plasma samples were centrifuged at 21,000 × gravity for 4 minutes to obtain clear particulate-free plasma, from which 300 μl was spiked with internal standard and loaded onto a C18 SPE column with a 100 mg mL−1 loading capacity. Guard columns (C18, hand packed 1 mm × 20 mm) were exchanged after backpressure increased above 4600psi, about 250 injections. A shallow acetonitrile/water gradient was used, 29 to 33% CH3CN over 8 minutes to elute salvinorin A. Reduction of chemical noise was achieved using tandem mass spectrometry with multiple reaction monitoring while sensitivity increases were observed using a 50 μL injection volume onto a small bore analytical column (C18, 1 mm ID × 50 mm) thus increasing peak concentration. Limits of quantification were found to be 0.0125 ng mL−1 (CSF) and 0.05 ng mL−1 (plasma) with interday precision and accuracy below 1.7 % and 9.42 % (CSF) and 3.47 % and 12.37 % (plasma) respectively. This method was used to determine the concentration of salvinorin A from an in vivo Rhesus monkey study and a trial of healthy human research participants, using behaviorally active doses.en_US
dc.publisherRoyal Society of Chemistryen_US
dc.titleLC-MS/MS quantification of salvinorin A from biological fluidsen_US
dc.typeArticleen_US
kusw.kuauthorWilliams, Todd D.
kusw.kudepartmentMass Spectrometry Laben_US
dc.identifier.doi10.1039/C3AY40810Hen_US
kusw.oaversionScholarly/refereed, author accepted manuscripten_US
kusw.oapolicyThis item meets KU Open Access policy criteria.en_US
dc.rights.accessrightsopenAccess


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