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KMID : 0369820150450060601
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Jorunal of Korean Pharmaceutical Sciences
2015 Volume.45 No. 6 p.601 ~ p.609
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Development of liquid chromatography tandem mass spectrometry method for determination of spironolactone in human plasma: application to a bioequivalence study of Daewon Spiracton tablet® (spironolactone 50 mg)
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Lee Jeong-Hun
An Tae-Gil
Kim Su-Jung
Shim Wang-Seob
Lee Kyung-Tae
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Abstract
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A sensitive LC?MS/MS method was developed and fully validated for the determination of spironolactone in human plasma using spironolactone-d6 as an internal standard (IS) after one-step liquid?liquid extraction with methyl tert-butyl ether: methylene chloride (MC) = 8:2 (v/v). Detection was performed using electrospray ionization in positive ion multiple reaction monitoring mode by monitoring the transitions: m/z 341.2 → 107.2 for spironolactone and m/z 347.1 → 107.2 for IS. Chromatographic separation was performed on a Cadenza CD-C18 column (3.0 × 100 mm i.d. 3 μm) with an isocratic mobile phase, which consisted of 0.1 % formic acid in water: methanol (30: 70, v/v), with a gradient flow rate as follow: 0?3.2 m, 320 μL/min; 3.2?3.5 m, 320?180 μL/min; 3.5?6.7 m, 180 μL/min; 6.7?7.0 m, 180?320 μL/min. The calibration curve was linear (correlation coefficients were >0.99) over the concentration range (0.5?150 ng/mL). The intraday and interday precisions ranged 0.89?6.00 and 1.20?10.511 %, respectively, and its accuracies ranged 96.90?105.08 and 97.99?104.13 %, respectively. The devised method was successfully applied in a bioequivalence study of two formulations of spironolactone, Spiracton tablet® and Aldactone tablet® in 50 healthy Korean male volunteers following single oral administration.
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KEYWORD
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Spironolactone, Bioequivalence study, Liquid chromatography-tandem mass spectrometry, Method validation
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