Simultaneous spectrophotometric determination of compounds having relatively disparate absorbance and concentration ranges; application to antidiabetic formulation of linagliptin and metformin

Abdalla, Ola M.; Abdel‐Megied, Ahmed M.; Saad, Ahmed S.; Soliman, Shymaa S.

doi:10.1016/j.saa.2018.05.064

Cited by 23 publications

(8 citation statements)

References 8 publications

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“…Analytical methods are available for the routine determination of LIN in bulk and pharmaceutical dosage forms by spectrophotometry, 10 High Performance Liquid Chromatography (HPLC) 11 and Ultra Performance Liquid Chromatography (UPLC) 12 . In addition, some bioanalytical methods were reported for LIN ‐ related to its pharmacology, kinetics and drug interactions 13–16 .…”

Section: Introductionmentioning

confidence: 99%

Application of online liquid chromatography/quadrupole time‐of‐flight electrospray ionization tandem mass spectrometry for structural characterization of linagliptin degradation products and related impurities

Yadav

Dornala

Swain

et al. 2020

Rapid Comm Mass Spectrometry

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Linagliptin is a drug used for the management of type 2 diabetes, which is a leading cause of global ill health and mortality. Impurities can affect the quality and safety of drug products and eventually may affect human health. A robust, sensitive and reliable analytical method is required to detect, characterize, quantify and control the presence of impurities in finished pharmaceutical products such as linagliptin. Methods: Linagliptin was stressed under harsh conditions as in the ICH Q1A (R2) guidelines to generate degradation products. The degradation products and process-related impurities were separated using an InertSustain C8 column (4.6 mm × 150 mm, 5 μm) and characterized by tandem quadrupole time-of-flight mass spectrometry in positive mode electrospray ionization. The developed method was validated according to the ICH Q2 (R1) guidelines. Results: Upon forced degradation, 12 degradation products were obtained (6 in oxidative stress and 3 in each of acid and alkaline hydrolysis). The special finding here was the presence of a pair of isomeric degradation products in acid hydrolysis and the formation of degradation products in base hydrolysis and oxidative degradation caused by the use of acetonitrile as a diluent. The 12 degradation products and 6 process-related substances were successfully identified using liquid chromatography/tandem mass spectrometry. Conclusions: A reversed-phase high-performance liquid chromatography method was developed and validated for the separation of the 12 degradation products and 6 process-related impurities. Structural characterization of all impurities was carried out using fragmentation pathways obtained from tandem mass spectrometry. The method was sufficiently sensitive and reproducible for quality control of linagliptin and for further research studies. 1 | INTRODUCTION Diabetes is an important cause of ill health and mortality and is a risk factor for other diseases. 1 According to the International Diabetes Federation report in 2017, in that year 425 million people were Amrej Singh Yadav and Divya Dornala contributed equally to this work.

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Section: Introductionmentioning

confidence: 99%

Application of online liquid chromatography/quadrupole time‐of‐flight electrospray ionization tandem mass spectrometry for structural characterization of linagliptin degradation products and related impurities

Yadav

Dornala

Swain

et al. 2020

Rapid Comm Mass Spectrometry

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“…3,9 A farmacopeia brasileira descreve os métodos titulométrico não-aquoso e o espectrofotométrico na região do UV. 4 Na literatura os métodos espectroscópico, 6,10 cromatográfico, 11 potenciométrico 12 e voltamétrico 13 19 A quantificação do cloridrato de ranitidina em diferentes matrizes tem sido realizada por meio de técnicas eletroanalítica, 20 espectrofotométrica 21 e cromatográfica. 22 A farmacopeia brasileira recomenda que a quantificação seja realizada empregando as técnicas espectrofotométrica no UV ou cromatográfica.…”

Section: Figura 1 Estrutura Química Do Cloridrato De Ciclobenzaprinaunclassified

Conductometric Determination of Hydrochlorides in Tablet Formulations as Proposal of Experimental Activity

Gois¹,

Borba²,

Silva³

2019

Rev. Virtual Quim

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In the present article it is described the quantification of cyclobenzaprine, metformin, metoclopramide and ranitidine hydrochlorides in tablet formulations using silver nitrate as titrant and conductometric titration, as a suggestion for an experimental activity in graduate courses. The conductometric titration was applied for hydrochlorides determination in four tablet formulations and the results are in good accordance with the declared values of manufacturers, at a 95 % confidence level. The experimental activity is simple and low coast, which enables it to be used in experimental activities on teaching laboratories improve student learning.

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“…A comprehensive review of the available literature found that a number of analytical techniques, such as spectrophotometric [ 19 , 20 , 21 , 22 , 23 , 24 , 25 , 26 , 27 , 28 , 29 , 30 ], colorimetric [ 31 , 32 , 33 ], spectrofluorometric [ 33 , 34 , 35 ], and high-performance liquid chromatographic [ 36 , 37 , 38 , 39 ] methods, were described for the detection of linagliptin. It has been determined that colorimetric is more specific than spectrophotometry (UV region).…”

Section: Introductionmentioning

confidence: 99%

“…It has been determined that colorimetric is more specific than spectrophotometry (UV region). The methods used to analyse the LGN singly or in combination are cited in references [ 19 , 20 , 21 , 22 , 23 , 24 , 25 , 26 , 27 , 28 , 29 , 30 ], which were based on the molecular absorption technique. These methods are sensitive, but they are not as selective as the method being studied.…”

Section: Introductionmentioning

confidence: 99%

Thermodynamic and Computational (DFT) Study of Non-Covalent Interaction Mechanisms of Charge Transfer Complex of Linagliptin with 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and Chloranilic acid (CHA)

2022

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This study describes the non-covalent interactions of the charge transfer complex (CT), which was responsible for the synthesis of Linagliptin (LNG) with 2, 3-Dichloro-5, 6-Dicyano-1, 4-benzoquinone (DDQ), or with chloranilic acid (CHA) complexes in acetonitrile (MeCN) at temperatures of (25 ± 2 °C). Then, a UV–Vis spectrophotometer was utilized to identify Linagliptin (LNG) from these complexes. For the quantitative measurement of Linagliptin in bulk form, UV–Vis techniques have been developed and validated in accordance with ICH criteria for several aspects, including selectivity, linearity, accuracy, precision, LOD, LOQ, and robustness. The optimization of the complex synthesis was based on solvent polarization; the ratio of molecules in complexes; the association constant; and Gibbs energy (ΔG°). The experimental work is supported by the computational investigation of the complexes utilizing density functional theory as well as (QTAIM); (NCI) index; and (RDG). According to the optimized conditions, Beer’s law was observed between 2.5–100 and 5–100 µM with correlation coefficients of 1.9997 and 1.9998 for LGN-DDQ and LGN-CHA complexes, respectively. For LGN-DDQ and LGN-CHA complexes, the LOD and LOQ were (1.0844 and 1.4406 μM) and (3.2861 and 4.3655 μM), respectively. The approach was successfully used to measure LGN in its bulk form with high precision and accuracy.

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Simultaneous spectrophotometric determination of compounds having relatively disparate absorbance and concentration ranges; application to antidiabetic formulation of linagliptin and metformin

Cited by 23 publications

References 8 publications

Application of online liquid chromatography/quadrupole time‐of‐flight electrospray ionization tandem mass spectrometry for structural characterization of linagliptin degradation products and related impurities

Application of online liquid chromatography/quadrupole time‐of‐flight electrospray ionization tandem mass spectrometry for structural characterization of linagliptin degradation products and related impurities

Conductometric Determination of Hydrochlorides in Tablet Formulations as Proposal of Experimental Activity

Thermodynamic and Computational (DFT) Study of Non-Covalent Interaction Mechanisms of Charge Transfer Complex of Linagliptin with 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and Chloranilic acid (CHA)

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