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KMID : 0369820120420060353
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Jorunal of Korean Pharmaceutical Sciences
2012 Volume.42 No. 6 p.353 ~ p.360
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Determination of 3α-hydroxytibolone by LC/MS/MS with electrospray ionization method and its application to bioequivalence study in human plasma
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Ban Eun-Mi
Shin Hye-Seoung
Kim Sung-Tae
Kim Chong-Kook
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Abstract
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A specific and sensitive liquid chromatography?tandem mass spectrometry (LC/MS/MS) in the negative electrospray ionization mode was developed and validated in order to analyze 3α-hydroxytibolone (3α-OH-tibolone), major metabolite of tibolone in human plasma sample using only 200 μL of plasma. 3α-OH-tibolone and 3α-OH-tibolone-d6 (internal standard, IS) in plasma were derivatized with p-toluenesulfonyl isocyanate after extraction using ethyl acetate. The dye residue and by-products was excluded using HLB Oasis SPE cartridge after derivertization. Separation of derivatized 3α-OH-tibolone and IS was performed on a C18 column within 6 min. The assay showed linearity in concentration ranges of 0.2?20 ng/mL. Intra-day precision and accuracy ranged from 0.77 to 5.0 % and from 98.0 to 100.56 %, respectively. Inter-assay precision and accuracy ranged from 1.49 to 5.00 % and from 99.75 to 100.94 %, respectively. A specific, reproducible and sensitive LC/MS/MS method for quantification of 3α-OH-tibolone in human plasma was successfully applied to evaluate the bioequivalence of tibolone in human volunteer following single oral administration of 5 mg tibolone.
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KEYWORD
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Tibolone, 3α-Hydroxytibolone, Liquid chromatography?tandem mass spectrometry (LC/MS/MS), Bioequivalence
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