Development and Validation of Spectrophotometric Methods for the Determination and Spectroscopic Characterization of Vildagliptin Using Ii -Acceptors in Pharmaceutical Preparations
Abstract:Three simple, quick and sensitive methods are described for the spectrophotometric determination of vildagliptin (VLD) in pharmaceutical preparations. The methods are based on formation of colored charge transfer (CT) complexes between VLD as n-electron donor and chloranilic acid (CA), tetrachloro-1,4-benzoquinone (p-chloranil), 7,7,8,8-tetracyanoquinodimethane (TCNQ) as π-acceptors. The colored products were quantitated spectrophotometrically at 520, 535 and 842 nm for CA, p-chloranil and TCNQ methods, respec… Show more
“…It could be taken alone or with other antidiabetic medications 1 . Various methods have been published for the estimation of VIL using UV spectrophotometric 2,3 , spectrofluorimetric 4,5 , liquid chromatographic methods [6][7][8][9][10][11] and voltammetric method 12 .…”
“…It could be taken alone or with other antidiabetic medications 1 . Various methods have been published for the estimation of VIL using UV spectrophotometric 2,3 , spectrofluorimetric 4,5 , liquid chromatographic methods [6][7][8][9][10][11] and voltammetric method 12 .…”
“…Vildagliptin is not listed in any pharmacopeia. A literature survey revealed that the determination of vildagliptin alone is performed by HPLC in plasma and pharmaceutical formulations , spectrophotometry and spectroflourimetry using the charge transfer complex technique with chloranilic acid, p ‐chloranil and 7,7,8,8‐tetracyanoquinodimethane . Spectrophotometric determinations have been reported using 1,2‐naphthoquinone‐4‐sulfonic acid and 4‐chloro‐7‐nitrobenzofurazan and after reaction with bromocresol green and bromothymol blue .…”
Robust high‐performance liquid chromatography and thin‐layer chromatography methods were adopted for the determination of vildagliptin in the presence of l‐proline, an in‐process impurity. The high‐performance liquid chromatography separation of vildagliptin and l‐proline was achieved on a cyano 250 × 4.6 mm, 5 μm column using 0.04 M phosphate buffer containing 0.2% triethylamine pH 5.5/methanol (22:78 v/v) as a mobile phase with an isocratic elution at 1 mL/min and 210 nm UV detection. Vildagliptin determination was in range of 5–40 μg/mL with a detection limit of 0.532 μg/mL. Qualitative and quantitative responses were evaluated by the application of Youden's test and statistical analysis to assess the high‐performance liquid chromatography method robustness, and system suitability limits were calculated based on the robustness test results. The thin‐layer chromatography method is based on the separation of vildagliptin and l‐proline on silica gel F254 using chloroform/methanol/glacial acetic acid (7:2:1 v/v/v) as a developing system, visualization was achieved by exposure to iodine vapor and densitometric measurement at 210 nm in range of 1–40 μg/band with a detection limit of 0.403 μg/band. Least squares regression analysis revealed a linear calibration for high‐performance liquid chromatography and a binomial relationship for thin‐layer chromatography. Full validation agreed with International Conference on Harmonization Q2 (R1) guidelines. Good recoveries were obtained for vildagliptin in drug substance, drug product and by applying the standard addition technique.
“…[2][3][4][5] Development of quantitative analytical method for the estimation of vildagliptin in plasma is very important for studying pharmacokinetic effects and drug-drug interactions. Different analytical methods have been described for the quantification of vildagliptin from formulations and biological samples, including spectrophotometric methods, [6][7] HPLC, [8][9][10][11][12] GC-MS, 13 and capillary electrophoresis. 14 These methods are not sensitive for the quantification in terminal plasma concentration of vildagliptin during pharmacokinetic studies comprising lower dose of vildagliptin.…”
Background: Vildagliptin, a dipeptidyl peptidase-4 inhibitor, is one of the potent oral antidiabetic agent. Objective: The objective of the present work was to establish a rapid, sensitive and validated capillary electrophoresis Quadrupole Time-of-flight Mass Spectrometry method from rat plasma. Methodology: Vildagliptin was estimated in rat plasma after precipitation of plasma proteins by acetonitrile, using sitagliptin as internal standard. For separation of vildagliptin from plasma components, fused silica capillary with background electrolyte consisting of 0.25 mM ammonium formate buffer, with SL composition of 50:50 methanol and water consisting of 0.25% of formic acid, pumped at a flow rate of 0.2 ml/min was used. Electron spray ionization with positive ion multiple reaction mode was applied for detection of analytes. Results: Newly developed method showed good calibration curve in the concentration range of 1 -500 ng/ml with excellent correlation coefficient (r
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