UPLC-ESI/Q-TOF MS/MS Method for Determination of Vildagliptin and its Organic Impurities

Abstract

Vildagliptin (VLG) corresponds to a drug used for the treatment of diabetes mellitus. This disease requires continuous treatment, and so the control of impurities present in it is important to assure the quality of this drug. Thus, it is necessary to use sensitive and selective detection techniques and the ultra-performance liquid chromatography is a better option compared with high-performance liquid chromatography because it enhances the separation efficiency with a shorter analysis time and an increased resolution. This research analysis was accomplished by using liquid chromatography/tandem mass spectrometry, and the quantification was performed by using an extracted ion from the VLG drug and its main organic impurities of synthesis. During the validation process, following international standards, the method proved to be linear for the tree substances (R2 = 0.997–0.998) and the analysis of variance showed a non-significant linearity deviation (P > 0.05). Three critical factors were selected to evaluate method robustness with a full factorial experimental design, and the changes in the parameters were found to be not significant for the quantification of VLG and its impurities. The ultra-performance liquid chromatography-tandem mass spectrometry for the determination of impurities in VLG was precise, accurate and robust proving to be effective for analysis in the pharmaceutical industry and to improve the quality, safety and effectiveness of the new drug developed.

Metabolism and Chemical Degradation of New Antidiabetic Drugs (Part II): A Review of Analytical Approaches for Analysis of Gliptins

“…In the next study from the literature [47] separation of VILDA and its next two impurities, i.e., 2-pyrrolidinecarboxamide (VILDA-D4) and 3-amino-1-adamantanol (VILDA-D5) was achieved (Table 3). In addition, the next six degradants of VILDA were reported by Arar et al [48].…”

“…Finally, identification of degradation products of VILDA was performed using an UHPLC-DAD-MS with positive ESI (Table 4). The main objective of the next chromatographic method [47] was to achieve the separation of VILDA from VILDA-D4 and VILDA-D5 (Table 4). Additionally, a simple RP-HPLC-UV method was developed for separation of VILDA and its new degradation products, e.g., VILDA-D6, VILDA-D7, VILDA-D8 and VILDA-D9.…”

Smart Spectrophotometric Method Development for Simultaneous Estimation of Antidiabetic Drugs in Formulations

“…2,7 A number of assay procedures have been described for the assessment of VGT and RGF from different matrix including medicines. VGT has been estimated using UV-Vis spectrophotometry, 8-12 HPLTC, 13 HPLC, 14,15 and LCMS 16 alone and with other antidiabetic agents. The analysis of RGF by spectrophotometry, [17][18][19][20] HPLC, [19][20][21][22] UPLC, 23 and LC-MS 24 has been reported in the literature.…”

Innovative spectrofluorimetric determination of vildagliptin based on a “switch off/on” NS-doped carbon dot nanosensor

“…Different methods have been reported for VLD determination including, spectrophotometric, 5–10 spectrofluorimetric, 11,12 electrochemical, 13,14 and chromatographic methods. 15–19 However, because of the weakly absorbing chromophores in VLD and their significantly blue-shifted maxima, its determination based on direct UV absorption measurement may be prone to interferences from excipients, impurities, or the matrix of biological fluids. The reported spectrofluorimetric methods 11,12 are based on derivatization reactions that required a long time (20–50 minutes) or temperature.…”