Update on compatibility assessment of empagliflozin with the selected pharmaceutical excipients employed in solid dosage forms by thermal, spectroscopic and chromatographic techniques

Niguram, Prakash; Polaka, Surya Narayana; Rathod, Rajeshwari; Kalia, Kiran; Kate, Abhijeet S.

doi:10.1080/03639045.2020.1716371

Cited by 15 publications

(7 citation statements)

References 26 publications

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“…The new model requires melting point, melting enthalpy and molar volume of empagliflozin drug, and these values are obtained from literature and group contribution methods. From literature 31 , the melting point of empagliflozin drug (426.1 K), molar volume (3.2699 × 10 –4 m 3 /mol) and melting enthalpy (60.238 kJ/mol) are calculated based on literature, Immirzi and Perini 63 and Jain et al, methods 66 , respectively. The new model makes use of objective function given in Eq.…”

Section: Resultsmentioning

confidence: 99%

“…Empagliflozin is an inhibitor of sodium-glucose co-transporter-2 (SGLT2), the transporters primarily responsible for the re-absorption of glucose in the kidney. Further, it is useful in reducing the risk of cardiovascular death in adults with type 2 diabetes mellitus and cardiovascular disease 31 . Sufficient drug dosage is very essential for those treatments and this is achieved through a proper particle size.…”

Section: Introductionmentioning

confidence: 99%

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Experimental solubility and thermodynamic modeling of empagliflozin in supercritical carbon dioxide

Sodeifian

Garlapati

Razmimanesh

et al. 2022

Sci Rep

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The solubility of empagliflozin in supercritical carbon dioxide was measured at temperatures (308 to 338 K) and pressures (12 to 27 MPa), for the first time. The measured solubility in terms of mole faction ranged from 5.14 × 10–6 to 25.9 × 10–6. The cross over region was observed at 16.5 MPa. A new solubility model was derived to correlate the solubility data using solid–liquid equilibrium criteria combined with Wilson activity coefficient model at infinite dilution for the activity coefficient. The proposed model correlated the data with average absolute relative deviation (AARD) and Akaike’s information criterion (AICc), 7.22% and − 637.24, respectively. Further, the measured data was also correlated with 11 existing (three, five and six parameters empirical and semi-empirical) models and also with Redlich-Kwong equation of state (RKEoS) along with Kwak-Mansoori mixing rules (KMmr) model. Among density-based models, Bian et al., model was the best and corresponding AARD% was calculated 5.1. The RKEoS + KMmr was observed to correlate the data with 8.07% (correspond AICc is − 635.79). Finally, total, sublimation and solvation enthalpies of empagliflozin were calculated.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Experimental solubility and thermodynamic modeling of empagliflozin in supercritical carbon dioxide

Sodeifian

Garlapati

Razmimanesh

et al. 2022

Sci Rep

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“…34,35 U svrhu ispitivanja fizikalno-kemijske stabilnosti aktivnih sastavnica u procesu razvoja fiksne kombinacije uspješno se pri-mjenjuju razne kromatografske, termalne i spektroskopske tehnike. [36][37][38][39][40][41][42] Princip ispitivanja fizikalno-kemijske kompatibilnosti sastavnica naizgled je jednostavan iako interpretacija rezultata ne dovodi uvijek do jednoznačnih rezultata. Utvrđivanje kompatibilnosti temelji se na usporedbi rezultata dobivenih provođenjem studija te primjenom raznih tehnika s ciljem fizikalno-kemijske karakterizacije čistih sastavnica i njihovih smjesa (slika 2).…”

Section: Ispitivanje Fizikalno-kemijske Kompatibilnosti Sastavnicaunclassified

Ispitivanje fizikalno-kemijske kompatibilnosti lijekova primjenom analitičkih tehnika: pregled istraživanja razvoja fiksne kombinacije 5-aminosalicilata i folne kiseline

Jeličić

2022

Kemija U Industriji

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With the use of fixed-dose drug combinations, the potential risk of non-adherence needs to be minimised, which is particularly important in patients with chronic diseases. The development of such dosage form is a complex process in which an important role is played by testing the physicochemical compatibility of the components intended for the manufacture of the desired product. Various analytical techniques, such as thermoanalytical (DSC, DTA), spectroscopic (FTIR, XRPD) and chromatographic (HPLC), in combination with certain degradation studies, such as forced degradation and isothermal degradation, are often used. In this review, on the example of the development of a fixed-dose combination of 5-aminosalicylate and folic acid, procedures suitable for testing the compatibility of drug components, as well as analytical techniques and various ways of interpretation of results are described.

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“…A similar study used PXRD and other isothermal techniques to establish compatibility between propafenone HCl and lactose monohydrate [ 29 ]. Further studies reported PXRD as one of the spectroscopic methods for conducting API using excipient assessments to support the stability data for pharmaceutical products [ 30 , 31 , 32 ]. As there is evidence to support using PXRD to monitor formulation changes in pharmaceutical development, this study employed the technique as a tool to possibly detect changes in the diffractograms of the L-T 4 formulations used in the stability studies.…”

Section: Introductionmentioning

confidence: 99%

“…These experiments were carried out at a more elevated temperature than recommended by the International Conference on Harmonization (ICH Q1A(R2)), namely 40 ± 2 °C/75% RH ± 5% RH for accelerated studies; the rationale behind this was to quickly identify excipients that would cause potential stability failures [ 33 ]. Thermal stress testing was used to evaluate the compatibility of ketorolac and empagliflozin with some common excipients, and it suggested the benefits of these studies for achieving a lower risk for formulation failure [ 30 , 34 ]. In addition to placing samples under the ICH recommended conditions for accelerated study, the current research investigated the potency of L-T 4 tablets stored at 50 ± 2 °C/75% RH ± 5% RH as a potential predictor of the formulation’s accelerated and real-time stability.…”

Section: Introductionmentioning

confidence: 99%

Potency and Powder X-ray Diffraction (PXRD) Evaluation of Levothyroxine Sodium Tablets under Ambient, Accelerated, and Stressed Conditions

Okezue,

Byrn,

Probost

et al. 2023

Pharmaceuticals

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Levothyroxine tablets, although highly prescribed in the United States, have been one of the most frequently recalled products. Because of the importance of the medication, several efforts have been put in place by the United States Food and Drug Administration (US FDA) to control the quality of levothyroxine tablets available to patients using the drug. The choice of excipients used in the formulation has been shown to impact the hygroscopicity and microenvironment, and ultimately the stability of the levothyroxine tablets formulations. Based on information generated from the US FDA Enforcement Report database, one of the main reasons for recalls is the low potency of different batches of the product. The yearly product recall trends for levothyroxine formulations were determined using the FDA Enforcement Report database. Three brands of levothyroxine tablets were selected with excipient lists similar to those products that have been historically recalled. The samples were placed at ambient (~23 °C), accelerated stability (40 °C/75% RH), and stress (50 °C/75% RH) conditions for up to 6 months. Sample potencies were determined at 0, 1.5, 3, and 6 months using the methods for assay and impurities in the United States Pharmacopeia (USP) monograph for levothyroxine tablets. Additional sample monitoring was conducted by overlaying the initial powder X-ray diffractograms (PXRD) of the samples from 0 months with the patterns generated thereafter. There has been a decline in the number of levothyroxine tablets recalled over the years. The highest numbers of recalls were recorded in the years 2013 [33] and 2020 [23]; no recalls occurred in the years 2019 and 2022. All of the brands evaluated met the USP 95.0–105.0% assay requirements at 1.5 months under accelerated conditions; only one of the brands complied at 3 months. Under ambient conditions, two brands were stable at 6 months, with borderline assay results. For stability, levothyroxine was found in microgram quantities in the formulations and PXRD could not detect changes at these low levels. However, we found some distinguishing data for samples under stress conditions.

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Update on compatibility assessment of empagliflozin with the selected pharmaceutical excipients employed in solid dosage forms by thermal, spectroscopic and chromatographic techniques

Cited by 15 publications

References 26 publications

Experimental solubility and thermodynamic modeling of empagliflozin in supercritical carbon dioxide

Experimental solubility and thermodynamic modeling of empagliflozin in supercritical carbon dioxide

Ispitivanje fizikalno-kemijske kompatibilnosti lijekova primjenom analitičkih tehnika: pregled istraživanja razvoja fiksne kombinacije 5-aminosalicilata i folne kiseline

Potency and Powder X-ray Diffraction (PXRD) Evaluation of Levothyroxine Sodium Tablets under Ambient, Accelerated, and Stressed Conditions

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