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http://dx.doi.org/10.5806/AST.2012.25.1.076

Analysis of dutasteride in human serum by LC-MS/MS  

Nam, Hye-Seon (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Nam, Kyong-Hee (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Jung, Su-Hee (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Lee, Jang-Woo (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Kang, Jin-Yeong (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Hong, Soon-Keun (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Kim, Tae-Sung (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Jung, Ki-Kyung (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Kang, Tae-Seok (Toxicology Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Yoon, Hae-Jung (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Lee, Kwang-Ho (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Rhee, Gyu-Seek (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Korea Food and Drug Administration)
Publication Information
Analytical Science and Technology / v.25, no.1, 2012 , pp. 76-82 More about this Journal
Abstract
The determination and confirmation of dutasteride in human serum was performed by a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Beclomethasone as an internal standard (I.S.) was added to the serum and the mixed sample was pretreated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE). The mass transitions of dutasteride and I.S. monitored in multiple reaction monitoring (MRM) were m/z 529.6${\rightarrow}$461.5 and m/z 409.3${\rightarrow}$391.2, respectively, and the retention times were 6.45 and 5.46 min, respectively. The calibration curve was linear in the concentration range of 0.5~30.0 ng/mL ($R^2$= 0.9999) and the limit of quantitation (LOQ) was found to be 0.5 ng/mL. The recovery of dutasteride was shown to be 66~72%. The intra-day assay precision and accuracy were in the range 3.5~5.5% and 85.7~89.9%, respectively, and the interday assay precision and accuracy were in the range 4.2~5.8% and 90.8~95.8%, respectively.
Keywords
Dutasteride; LC-MS/MS; human serum;
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