Lipophilic benzamide and anilide derivatives as high-performance liquid chromatography internal standards: application to sirolimus (rapamycin) determination

Journal of Chromatography. B, Biomedical Sciences and Applications
G M FerronW J Jusko

Abstract

Finding a suitable internal standard in reversed-phase high-performance liquid chromatography is often difficult. A general approach for selecting and synthesizing the proper internal standard is presented and applied to a validated method for quantitation of sirolimus in several biological matrices. A series of fifteen N-alkylbenzamides, N-alkyltoluamides and N-alkanoylanilines with a log P range of 3.51 to 6.68 were synthesized as internal standards; N-undecyl-o-toluamide was evaluated most extensively. Sirolimus quantitation involves a simple sample clean-up procedure followed by isocratic chromatography on a heated C18 analytical column with an 70% methanol-water mobile phase and ultraviolet detection at 278 nm. This method was linear from 2.5 to 200 ng with a limit of quantitation of 2.5 ng using a 1-ml blood sample. Sirolimus recovery was above 72.1%. The intra-day and inter-day coefficients of variation were less than 11.7%. Several drugs and sirolimus metabolites do not interfere with the analysis. This method was used to measure sirolimus in blood from rats, rabbits and humans.

References


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Citations

Jul 21, 2005·Clinical Pharmacokinetics·Sunita Bond StentonMary H H Ensom
Jul 17, 2013·Biomedical Chromatography : BMC·Xianqin WangJianshe Ma
Oct 28, 2014·Journal of Biomedical Materials Research. Part a·Xiaoxiang Zhu, Richard D Braatz
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Feb 7, 2014·FASEB Journal : Official Publication of the Federation of American Societies for Experimental Biology·Kristin P BibeeSamuel A Wickline
Oct 10, 2018·Bulletin of Mathematical Biology·Koyel Chakravarty, D C Dalal
Sep 8, 2019·Journal of Theoretical Biology·Mohammadreza DorvashIman Tavassoly
Aug 24, 2020·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Sasidharan L SreejithRenjith Sasi

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