Quantification of sirolimus by liquid chromatography-tandem mass spectrometry using on-line solid-phase extraction

Clinical Chemistry and Laboratory Medicine : CCLM
Michael VogeserDietrich Seidel

Abstract

Quantification of the new immunosuppressant sirolimus (syn. rapamycin; Rapamune) in whole blood by chromatography is essential for its clinical use since no immunoassay is available although monitoring is mandatory. Here we report on a rapid and convenient liquid chromatography (LC-tandem mass spectrometry method and describe our practical experience with its routine use. Whole blood samples were hemolyzed and deproteinized using an equal volume (150 microl) of a mixture of methanol/zinc sulfate solution containing the internal standard desmethoxy-rapamycin. After centrifugation, the clear supernatants were submitted to an on-line solid-phase extraction procedure using the polymeric Waters Oasis HLB material, with elution of the extracts onto the analytical column in the back-flush mode by column switching. For analytical chromatography a RP-C18 column was used with 90/10 methanol/2 mM ammonium acetate as the mobile phase. A 1:10 split was used for the transfer to the mass spectrometer, a Micromass Quattro LC-tandem mass spectrometry system equipped with a Z-spray source and used in the positive electrospray ionization mode. The following transitions were recorded: sirolimus, 931>864 m/z, and desmethoxy-rapamycin (I.S.), 901>83...Continue Reading

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Citations

Feb 13, 2007·Analytical and Bioanalytical Chemistry·Jun ZhangLewis Schwartz
Sep 3, 2003·Clinical Biochemistry·Kent C Dooley
Apr 2, 2003·Clinical Chemistry and Laboratory Medicine : CCLM·Michael Vogeser
Aug 28, 2003·Clinical Chemistry and Laboratory Medicine : CCLM·Pierre E WallemacqDonald P Cooper
May 19, 2005·Clinical Chemistry and Laboratory Medicine : CCLM·Michael Vogeser, Ute Spöhrer
Oct 7, 2005·Clinical Chemistry and Laboratory Medicine : CCLM·Michael VogeserUte Spöhrer
Sep 9, 2006·Clinical Chemistry and Laboratory Medicine : CCLM·Michael Vogeser, Ute Spöhrer
Dec 18, 2013·Analytical and Bioanalytical Chemistry·Kelvin Sze-Yin Leung, Bonnie Mei-Wah Fong
Jul 6, 2010·Clinical Biochemistry·Michael Vogeser, Fabian Kirchhoff
May 13, 2005·American Journal of Transplantation : Official Journal of the American Society of Transplantation and the American Society of Transplant Surgeons·Marjo M P C DonnersSylvia Heeneman
Jun 1, 2017·The Analyst·Nicolas GuichardSandrine Fleury-Souverain
May 12, 2004·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Therese KoalVolkhard Kaever
Jun 16, 2004·American Journal of Transplantation : Official Journal of the American Society of Transplantation and the American Society of Transplant Surgeons·Ingo KaczmarekBruno Reichart
May 28, 2019·International Journal of Molecular Sciences·Cristina Alexandra Ciocan-CartitaIoana Berindan-Neagoe
Oct 24, 2002·Current Opinion in Nephrology and Hypertension·David W Holt
May 12, 2004·The Journal of Heart and Lung Transplantation : the Official Publication of the International Society for Heart Transplantation·Jan GroetznerUNKNOWN Munich Lung Transplant Group

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