Susan Steinike (Presenter)
Restek Corporation
Authorship: Paul Connolly, Frances Carroll, Sharon Lupo, Shun-Hsin Liang, Ty Kahler
Restek Corporation, 110 Benner Circle Bellefonte, PA 16823
| Short Abstract The use of liquid chromatography coupled with mass spectrometry (LC-MS/MS) in therapeutic drug monitoring and toxicology labs has increased significantly over the years. LC-MS provides sensitivity, speed, and the ability to simplify sample preparation. The Raptor™ Biphenyl column was developed to complement high-throughput LC-MS/MS analyses by combining the increased efficiency of superficially porous particles (SPP) with the resolution of Ultra Selective Liquid Chromatography™ (USLC™) technology. In this example, a simple dilute and shoot method was developed for 14 common antiepileptic drugs in urine using a Raptor™ Biphenyl column. |
Long Abstract
The use of liquid chromatography coupled with mass spectrometry (LC-MS/MS) in therapeutic drug monitoring and toxicology labs has increased significantly over the years. LC-MS provides sensitivity, speed, and the ability to simplify sample preparation. The Raptor™ Biphenyl column was developed to complement high-throughput LC-MS/MS analyses by combining the increased efficiency of superficially porous particles (SPP) with the resolution of Ultra Selective Liquid Chromatography™ (USLC™) technology. In this example, a simple dilute and shoot method was developed for 14 common antiepileptic drugs in urine using a Raptor™ Biphenyl column.
Human urine samples were diluted in 0.1% formic acid in water and injected into a Shimadzu Nexera UHPLC equipped with an AB SCIEX API 4500™ MS/MS. Detection was performed using electrospray ionization in positive ion mode using scheduled multiple reaction monitoring (MRM). The separation was performed using water and methanol mobile phases modified with 0.1% formic acid under gradient conditions on a Restek Raptor™ Biphenyl 2.7µm, 100 x 2.1mm column.
Linearity and precision and accuracy experiments were performed during method development. Purchased human urine was fortified with 14 drug analytes and their deuterated internal standards. The calibration range for most analytes was from 10 to 1000 ng/mL; R values were all greater than 0.990. Accuracy and precision were determined by fortifying human urine at a concentration of 800 ng/mL prior to dilution. Mean values at this level ranged from 88% to 110% of nominal concentrations for all analytes. Coefficient of variation (CV) was calculated for the determination of precision and ranged from 6.2% to 10.5%.
An easy dilute-and-shoot method was developed for the quantitative measurement of 14 common antiepileptic drugs in human urine. Analytes were quickly and accurately quantified in human urine with a run time of 5.5 minutes with great accuracy and precision.
References & Acknowledgements:
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