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  • Method for the quantitative analysis of cilostazol and its metabolites in human plasma using LC/MS/MS.

Method for the quantitative analysis of cilostazol and its metabolites in human plasma using LC/MS/MS.

Journal of pharmaceutical and biomedical analysis (2001-08-23)
S L Bramer, P N Tata, S S Vengurlekar, J H Brisson
ABSTRACT

An LC/MS/MS method for the simultaneous determination of cilostazol, a quinolinone derivative, and three active metabolites, OPC-13015, OPC-13213, and OPC-13217, in human plasma was developed and validated. Cilostazol, its metabolites, and the internal standard, OPC-3930 were extracted from human plasma by liquid-liquid partitioning followed by solid-phase extraction (SPE) on a Sep-Pak silica column. The eluent from the SPE column was then evaporated and the residue reconstituted in a mixture of methanol/ammonium acetate buffer (pH 6.5) (2:8 v/v). The analytes in the reconstituted solution were resolved using reversed-phase chromatography on a Supelcosil LC-18-DB HPLC column by an 17.5-min gradient elution. Cilostazol, its metabolites, and the internal standard were detected by tandem mass spectrometry with a Turbo Ionspray interface in the positive ion mode. The method was validated over a linear range of 5.0-1200.0 ng/ml for all the analytes. This method was demonstrated to be specific for the analytes of interest with no interference from endogenous substances in human plasma or from several potential concomitant medications. For cilostazol and its metabolites, the accuracy (relative recovery) of this method was between 92.1 and 106.4%, and the precision (%CV) was between 4.6 and 6.5%. During the validation, standard curve correlation coefficients equalled or exceeded 0.999 for cilostazol and its metabolites. These data demonstrate the reliability and precision of the method. The method was successfully cross-validated with an established HPLC method.

MATERIALS
Product Number
Brand
Product Description

Supelco
SUPELCOSIL LC-NH2-NP HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-S HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
SUPELCOSIL LC-NH2-NP Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18-S HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-S HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 3 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 30 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 7.5 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
SUPELCOSIL LC-18 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 3 mm
Supelco
SUPELCOSIL LC-18-DB HPLC Column, 3 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
SUPELCOSIL LC-18-DB Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-18-DB Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm