Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume
47, Number 6, July 2009, pp. 473-477
Highly Sensitive LC–MS–MS Analysis
of a Pharmaceutical Compound in Human Plasma Using Monolithic
Phase-Based On-line Extraction
Raymond Naxing Xu, Phillip Vaca, Matthew J.
Rieser, and Tawakol A. El-Shourbagy
Abbott Laboratories, Department of Drug Analysis, 100 Abbott
Park Road, Abbott Park, IL 60064
Monolithic columns have been used in recent years
for fast chromatographic separation due to their high permeability
and low backpressure. We have explored the potential of monolithic
material as sample preparation tool in bioanalytical applications.
By taking advantage of monolithic columns’ online concentration
capability, we have developed a highly sensitive liquid chromatography–tandem
mass spectrometry assay for quantitative determination of a pharmaceutical
compound in human plasma. The assay was fully validated to satisfy
the requirements of precision and accuracy, selectivity, matrix
effect, and reproducibility. A linear dynamic range from 0.011
ng/mL to 12.3 ng/mL was established as the calibration standard.
The percentage of bias for quality control samples was between –9.9%
and –2.5%. Coefficient of variation, a measurement of precision,
was within 9.9%. On-line extraction with monolithic support provided
adequate sample cleanup and on-line concentration of the analyte.
The assay exhibited good tolerance to matrix effect and has been
applied successfully to a clinical study. The incurred sample
analysis showed that original and repeat values were within ±10.1%
for all assay samples.
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