TY - JOUR
T1 - Development and validation of an LC-MS assay for finasteride and its application to prostate cancer prevention trial sample analysis
AU - Chen, Xiaohong
AU - Gardner, Erin R.
AU - Price, Douglas K.
AU - Figg, William D.
N1 - Funding Information:
* E.R. Gardner: This research was supported by the Intramural Research Program of the NIH, National Cancer Institute, Center for Cancer Research.
Funding Information:
The authors thank Southwest Oncology Group (SWOG) for the support during this study. This work is supported by National Cancer Institute, NIH, Department of Health and Human Services grant P01CA106451.
Funding Information:
This project has been funded in whole or in part with federal funds from the National Cancer Institute, National Institutes of Health, under contract N01-CO-12400.* The content of this publication does not necessarily reflect the views or policies of the Department of Health and Human Services, nor does mention of trade names, commercial products, or organizations imply endorsement by the US Government.
PY - 2008/4
Y1 - 2008/4
N2 - An analytical method is developed and validated for the quantitative determination of finasteride, a potent 5 α-reductase inhibitor, in human plasma. Calibration curves are linear in the concentration range of 1 to 100 ng/mL. Sample pretreatment involves a liquid-liquid extraction with ethyl acetate using 0.2 mL aliquots of plasma. Finasteride and the internal standard (beclomethasone) are separated on a Waters Symmetry Shield RP18 column (50 x 2.1 mm, 3.5 μm) and eluted using a gradient mobile phase composed of acetonitrile and 10mM ammonium acetate with 0.1% formic acid. The column eluant is monitored by mass spectrometry with electrospray ionization. A complete validation of the method is performed. For quality control samples at three different concentrations that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from 95.2% to 101% and 3.4% to 7.3%, respectively. The developed method is subsequently applied to measure the steady state finasteride concentration of patients who participated in the Prostate Cancer Prevention Trial.
AB - An analytical method is developed and validated for the quantitative determination of finasteride, a potent 5 α-reductase inhibitor, in human plasma. Calibration curves are linear in the concentration range of 1 to 100 ng/mL. Sample pretreatment involves a liquid-liquid extraction with ethyl acetate using 0.2 mL aliquots of plasma. Finasteride and the internal standard (beclomethasone) are separated on a Waters Symmetry Shield RP18 column (50 x 2.1 mm, 3.5 μm) and eluted using a gradient mobile phase composed of acetonitrile and 10mM ammonium acetate with 0.1% formic acid. The column eluant is monitored by mass spectrometry with electrospray ionization. A complete validation of the method is performed. For quality control samples at three different concentrations that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from 95.2% to 101% and 3.4% to 7.3%, respectively. The developed method is subsequently applied to measure the steady state finasteride concentration of patients who participated in the Prostate Cancer Prevention Trial.
UR - http://www.scopus.com/inward/record.url?scp=41749089618&partnerID=8YFLogxK
U2 - 10.1093/chromsci/46.4.356
DO - 10.1093/chromsci/46.4.356
M3 - Article
C2 - 18402729
AN - SCOPUS:41749089618
SN - 0021-9665
VL - 46
SP - 356
EP - 361
JO - Journal of Chromatographic Science
JF - Journal of Chromatographic Science
IS - 4
ER -