Concurrent determination of ezetimibe and its phase-I and II metabolites by HPLC with UV detection: Quantitative application to various in vitro metabolic stability studies and for qualitative estimation in bile

Basha, Shaik Jafar Sadik; Naveed, Shaik Abdul; Tiwari, Nirbhay Kumar; Shashikumar, Dhanya; Syed, Mustafa; Kumar, Thammera Ranjith; Kumar, Nyavanandi Vijay; Rao, Nadipalli Prabhakar; Nanduri, Srinivas; Mullangi, Ramesh; Srinivas, Nuggehally R.

doi:10.1016/j.jchromb.2007.02.053

Cited by 44 publications

(29 citation statements)

References 18 publications

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“…These included theophylline [7], ranitidine hydrochloride [9] (reported in articles concerning the HPLC-UV determination of ezetimibe), metformin hydrochloride [17], fenofibrate [18] and nitrendipine [19] (for which the reported analytical wavelengths were close to the one used in our investigation). For all the substances tested, 1 μg mL −1 methanolic solutions were prepared.…”

Section: Internal Standardmentioning

confidence: 62%

“…The first mobile phase tested was as reported by Basha et al [7]. In a gradient sequence, the following mixture was prepared: 0.05 M aqueous formic acid solution, a mixture of water and acetonitrile 10:90 (v/v), and a mixture of water and methanol 10:90 (v/v).…”

Section: Mobile Phasementioning

confidence: 99%

“…The isocratic flow rate at ambient temperature was 1.5 mL min −1 . For the detection, instead of the mass spectrometer originally used, we used a UV detector set at 250 nm as described in the method of Basha et al [7]. The injection volume of 1 μg mL −1 ezetimibe was 60 μL.…”

Section: Mobile Phasementioning

confidence: 99%

“…Current methods used are generally chromatographic based. Several high-performance liquid chromatographic (HPLC) methods have been elaborated for the analysis of ezetimibe concentrations in plasma, urine, faeces and pharmaceutical dosage forms [3][4][5][6][7][8][9][10], using different types of detectors: UV detectors [3,4,[6][7][8][9][10], mass spectrometry (MS) type detectors [5,8] and scintillation detectors [8].…”

Section: Introductionmentioning

confidence: 99%

“…Most commonly, investigations of ezetimibe concentration in organic samples concern single dose administration [5,7,8], while information for multiple dose is limited. It is of great importance as the terminal half-life of ezetimibe is estimated to be between 16 and 31 h, and after repeated ingestion, the drug has a tendency to accumulate [11].…”

Section: Introductionmentioning

confidence: 99%

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RP-HPLC-UV Determination of ezetimibe in serum: Method development, validation and application to patients chronically receiving the drug

Suchy¹,

Łabuzek²,

Pierzchała³

2013

Acta Chromatographica

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Summary.Ezetimibe is the first in a new class of antihypercholesterolemic drugs. Since it has not long been available on the market, many of its properties may still be revealed. Analytical methods for its determination are scarce, especially regarding serum samples. A simple, fast, and effective high-performance liquid chromatography-ultraviolet (HPLC-UV) method for the determination of ezetimibe concentration in human serum has therefore been developed. Three mobile phases were analysed, and original modifications to the concentration and flow parameters were made. Of five potential internal standards (IS), only nitrendipine was found to be suitable. The analytical wavelength was chosen based on the absorption spectrum of ezetimibe in the mobile phase. Finally, an extraction analysis was performed using two different solvents, and the extrahent volume was optimised. The final method developed was as follows. Single extraction of 1 mL serum sample, spiked with IS, was performed using 10 mL of methyl-t-butyl ether. Separation was obtained at ambient temperature on a Waters C18 Symmetry Shield (4.6 mm × 250 mm, 5 μm) column. The isocratic mobile phase was composed of acetonitrile and 0.1 M ammonium acetate aqueous solution 55:45 (v/v), set at flow rate of 0.75 mL min −1 . Ezetimibe was detected at a wavelength of 232 nm after 5.49 min, and the IS was detected at 8.05 min. The developed method has been validated according to ICH standards. It was found to be specific, precise, accurate and linear over the range 10-800 ng mL −1 with R 2 > 0.998, and detection and quantification limits of 4.60 ng mL −1 and 13.94 ng mL −1 , respectively. The method has been applied to clinical serum samples. The developed technique allowed for successful in vivo assessment of ezetimibe concentrations in samples obtained from hypercholesterolemia patients who are chronically receiving the drug.

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