Development of a validated high-throughput LC-ESI-MS method for determination of sirolimus on dried blood spots

被引:43
|
作者
Rao, R. Nageswara [1 ]
Maurya, Pawan K. [1 ]
Ramesh, M. [2 ]
Srinivas, R. [2 ]
Agwane, Sachin B. [3 ]
机构
[1] Indian Inst Chem Technol, Div Analyt Chem, HPLC Grp, Hyderabad 500007, Andhra Pradesh, India
[2] Indian Inst Chem Technol, Natl Ctr Mass Spectrometry, Hyderabad 500007, Andhra Pradesh, India
[3] Indian Inst Chem Technol, Div Pharmacol, Hyderabad 500007, Andhra Pradesh, India
关键词
sirolimus; dried blood spots; monolithic column; high-throughput; LC-ESI-MS; PERFORMANCE LIQUID-CHROMATOGRAPHY; TANDEM MASS-SPECTROMETRY; WHOLE-BLOOD; ONLINE EXTRACTION; HPLC-MS/MS; RAPAMYCIN; IMMUNOSUPPRESSANTS; QUANTIFICATION; CYCLOSPORINE;
D O I
10.1002/bmc.1450
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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 (C) 2010 John Wiley & Sons, Ltd.
引用
收藏
页码:1356 / 1364
页数:9
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