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DOI: 10.1055/s-0028-1088339
© Georg Thieme Verlag KG Stuttgart · New York
Quantitative Determination of Ophiopogonin D by Liquid Chromatography/Electrospray Ionization Mass Spectrometry and its Pharmacokinetics in Rat
Publication History
Received: November 13, 2007
Revised: August 25, 2008
Accepted: August 28, 2008
Publication Date:
13 November 2008 (online)
Abstract
A sensitive and rapid liquid chromatography-mass spectrometric method for the determination of ophiopogonin D in rat plasma was developed and validated. Chromatographic separation was performed on a C18 column using a step gradient program with the mobile phase of 0.5 mmol/L ammonium chloride solution and acetonitrile. Ophiopogonin D was quantified using an electrospray negative ionization mass spectrometry in the selected ion monitoring (SIM) mode using digoxin as an internal standard. Good linearity was obtained in the concentration range of 2.5 – 480.0 ng/mL (r2 = 0.9984). The lower limit of quantification (LLOQ) and lower limit of detection (LLOD) were 2.5 ng/mL and 1.0 ng/mL, respectively. Both the intra- and inter-day precision was less than 8.9 % and the accuracy was within 97.5 – 107.3 %. The pharmacokinetic study of ophiopogonin D in rats was then defined using the method after intravenous dosing (77.0 μg/kg). The plasma concentration-time profile for ophiopogonin D was best fitted to an open two-compartment model with a clearance of 0.024 ± 0.010 L/min/kg and a terminal half life of 17.29 ± 1.70 min. A comparison of the pharmacokinetics of ophiopogonin D as a pure compound and as a component of ’SHENMAI’ injection revealed a significantly smaller clearance of ophiopogonin D (0.007 ± 0.002 L/min/kg) for the latter formulation, consistent with an inhibition by one or more other components in the formulation.
Key words
ophiopogonin D - Radix Ophiopogonis - Ophiopogon japonicus Ker-Gawl. - Liliaceae - ’SHENMAI’ injection - LC-ESI-MS - method validation - pharmacokinetics
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China Pharmaceutical University
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