Journal
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
Volume 42, Issue 5, Pages 573-580Publisher
ELSEVIER
DOI: 10.1016/j.jpba.2006.05.025
Keywords
warfarin; supercritical fluid chromatography; automation; bioanalysis; LC-MS/MS
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Chiral separation for the analysis of enantiomers in biological fluids by HPLC often takes relatively long chromatography time compared to achiral analysis. The advantage of fast mass transfer in packed-column supercritical fluid chromatography (pSFC) and the high-flow compatibility of APCI-MS/MS were applied to develop a fast bioanalytical method for R/S-warfarin in human plasma. Presented here are the main challenges encountered during method development of a sermi-automated liquid extraction SFC-MS/MS method. The selection of internal standard, robustness of the SFC equipment, and carryover issues are discussed. The method has high-throughput: the chromatography time is at least two-fold faster than the our fastest previous method; and the liquid/liquid extraction time of 96 samples is less than 20 min using a Tecan Genesis (R) RSP 100 pipetting station and a Tomtec Quadra-96 (R) workstation. The standard curve range was 13.6-2500 ng/ml. Precision of QC concentrations from four validation runs was 7.0% for R-warfarin and 6.0% C.V. for S-warfarin; and the bias was 3.7 and 3.2% R.E., respectively. The method is sensitive, accurate, selective and robust, and was applied to a drug-interaction clinical study with rapid turnaround of sample analysis. (c) 2006 Elsevier B.V. All rights reserved.
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