Delapril and Manidipine Measurements by Liquid Chromatography—Tandem Mass Spectrometry in a Pharmaceutical Formulation

Abstract

A simple, specific, fast and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous analysis of delapril (DEL) and manidipine (MAN) from their combination formulation was developed and validated using fesoterodine as the internal standard (IS). The LC-MS/MS method was carried out on a Luna C8 column (50 × 3.0 mm i.d., 3 µm) with a mobile phase consisting of methanol and 10 mmol L(-1) ammonium acetate (90 : 0, v/v), run at a flow rate of 0.25 mL min(-1). The mass spectrometry method was performed employing positive electrospray ionization operating in multiple reaction monitoring mode, monitoring the transitions of m/z 453.1 → 234.1 for DEL, m/z 611.1 → 167.0 for MAN and m/z 412.2 → 223.0 for IS. The total analysis time was 3 min and the method was linear in the concentration range of 6-1080 ng mL(-1) and 2-360 ng mL(-1) for DEL and MAN, respectively. Parameters investigated for the method validation, such as the specificity, linearity, precision, accuracy and robustness, gave results within the acceptable range. Moreover, the proposed method was successfully applied for the simultaneous determination of DEL and MAN and the results were compared to validated liquid chromatography and capillary electrophoresis methods showing non-significant differences (P = 0.9).

Delapril and Manidipine Main Degradation Products: LC-UV and LC-ESI-MS Evaluations, Decay Kinetic, andin vitroCytotoxicity Studies

“…5,1,1.5,2,2.5,3,3.5 and 4 hours for DEL;1,2,3,4,5,6,7,8,9 and 10 hours for MAN) and diluted with mobile phase to final theoretical concentrations of 60 µg mL -1 of DEL and 20 µg mL -1 of MAN for LC-UV analysis.…”

“…[1][2][3][4] There is no official analytical method available for estimation of DEL and MAN in pharmaceutical formulation yet. Accordingly, a liquid chromatography coupled with mass spectrometry (LC-MS/MS), [5] liquid chromatography with UV detection (LC-UV), [6] and capillary electrophoresis [7] methods for simultaneous determination of DEL and MAN in commercial tablet were developed by our research group recently. In these last two studies, stress testing were performed to provide stability-indicating properties for analytical methods, and thus used to determine the analytes in the presence of degradation products.…”

The study of separation of delapril’s s-cis/s-trans isomers and development and validation of an analytical method for the estimation of delapril by reversed-phase liquid chromatography

“…Many analytical methods have been reported in the literature for the measurement of delapril in combination with manidipine in drug formulation such as liquid chromatographytandem mass spectrometry 3 , RP-LC 4 , UV spectrophotometry 5 and micellar electrokinetic chromatography 6 . Moreover, V. Todeschini and al.…”

Multicomponent Spectrophotometric Method for Simultaneous Analysis of Delapril and Indapamide in Tablets

“…However, the current literature reveals a few number of publications related of drugs in single dosage form or in association with others drugs. For DEL determination, these studies were performed by liquid chromatography (5), liquid chromatography-tandem mass spectrometry (6), capillary electrophoresis (7), and derivative spectrophotometry (8). On the other hand, British Pharmacopoeia, European Pharmacopoeia and United States Pharmacopoeia present official methods by liquid chromatography and spectrophotometry for IND assay in tablets and raw materials.…”