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Development of a validated high‐throughput LC‐ESI‐MS method for determination of sirolimus on dried blood spots
Author(s) -
Rao R. Nageswara,
Maurya Pawan K.,
Ramesh M.,
Srinivas R.,
Agwane Sachin B.
Publication year - 2010
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.1450
Subject(s) - chemistry , chromatography , electrospray ionization , dried blood , spots , extraction (chemistry) , sirolimus , solvent , electrospray , mass spectrometry , chromatographic separation , high performance liquid chromatography , analytical chemistry (journal) , biochemistry , organic chemistry
A high‐throughput liquid chromatography–electrospray ionization mass spectrometric (LC–ESI‐MS) method for screening of sirolimus on dried blood spots (DBS) was developed and validated. It involves solvent extraction of a punch of DBS followed by reversed‐phase LC on a relatively new monolithic column consisting of a silica rod with bimodal pore structure and detection by ESI‐MS. The run time was less than 3 min with a very low backpressure at a flow rate of 0.5 mL/min. The method can analyze more than 100 samples in an 8 h working day, including sample preparation. The assay was linear from 1 to 100 ng/mL. The mean recovery was 92.42%. The mean inter‐day and intra‐day precisions were 1.23 and 1.41%, respectively. The developed method is simple, rapid and useful for clinical applications. Copyright © 2010 John Wiley & Sons, Ltd.