Abstract

A highly sensitive, accurate and rapid analytical method based on reversed-phase liquid chromatography/electrospray ionization tandem mass spectrometry (RP-LC-ESI-MS/MS) has been developed and validated for the determination of repaglinide in human plasma using cetirizine as an internal standard (IS). The method was validated over a linear range of 0.5 - 100 ng/ml. After addition of IS, analytes were extracted from the plasma samples by liquid-liquid extraction using tert-butyl methyl ether as. The dried residue was reconstituted with 500 μL of mobile phase consisting of water/methanol/acetonitrile (62.5:20:17.5, v/v/v) and 0.2% formic acid. Chromatographic separations were achieved on a C18 analytical column. The analytes were detected with a triple quadrupole mass spectrometer using turbo V? ion spray source with positive ionization in multiple reaction monitoring (MRM) mode using MRM transitions m/z 453.3 > 162.2 and m/z 389.0 > 201.1 for the drug and IS, respectively. The proposed method was fully validated in terms of linearity, accuracy, precision, specificity, sensitivity, recovery and stability, giving results within the acceptable range. This method was successfully applied for a large number of authentic human plasma samples from a bioequivalence study.

Highlights

  • Repaglinide, (S)-2-Ethoxy-4-[2-[[3-methyl-1-[2-(1-piperidinyl)phenyl]butyl]amino]-2-oxoethyl]benzoic acid, isHow to cite this paper: Fayyad, M.K. and Ghanem, E.H. (2014) Liquid Chromatography Tandem Mass Spectrometry Method for Determination of Anti-Diabetic Drug Repaglinide in Human Plasma

  • Sensitivity (Lower Limit of Quantification, LLOQ) The lowest standard concentration on the calibration curve is accepted as the lower limit of quantification if the following conditions are met: the analyte response at the LLOQ should be at least five times the response compared to blank response; at the same time; the analyte peak should be identifiable, discrete, and reproducible with a precision of ±20% and accuracy ranging between 80% - 120%

  • Calibration Curves The calibration curves were constructed from a blank sample, a zero sample, and ten concentrations of repaglinide including the LLOQ, ranging from 0.5 to 100 ng/mL

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Summary

Introduction

Repaglinide, (S)-2-Ethoxy-4-[2-[[3-methyl-1-[2-(1-piperidinyl)phenyl]butyl]amino]-2-oxoethyl]benzoic acid, isHow to cite this paper: Fayyad, M.K. and Ghanem, E.H. (2014) Liquid Chromatography Tandem Mass Spectrometry Method for Determination of Anti-Diabetic Drug Repaglinide in Human Plasma. How to cite this paper: Fayyad, M.K. and Ghanem, E.H. (2014) Liquid Chromatography Tandem Mass Spectrometry Method for Determination of Anti-Diabetic Drug Repaglinide in Human Plasma. American Journal of Analytical Chemistry, 5, 281290. H. Ghanem a novel, fast-acting, oral anti-diabetic agent derived from carbamoylmethyl benzoic acid. Fast-acting, oral anti-diabetic agent derived from carbamoylmethyl benzoic acid It is used in the treatment of type 2 diabetes mellitus which is known as non-insulin dependent diabetes mellitus NIDDM [1]

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