Isolation and Characterization of Photodegradation Impurity in Budesonide Drug Product Using LC-MS and NMR Spectroscopy

Bhutnar, Arun D.; Khapare, Sachin; Desai, Anita; Dsouza, Smitha

doi:10.4236/ajac.2017.87034

Cited by 10 publications

(4 citation statements)

References 14 publications

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“…Lastly, no significant loss of content was observed during a 3-month stability study, and no significant degradation (i. e. > 0.5 % of the total budesonide) was observed. Rapid photodegradation was observed when the final formulation was stored in transparent glass vials in the lightconfirming previous reports and emphasizing the need for photoprotection [23].…”

Section: Discussionsupporting

confidence: 89%

Paediatric formulation: budesonide 0.1 mg/mL viscous oral solution for eosinophilic esophagitis using cyclodextrins

Hosselet

Villon

et al. 2018

Pharmaceutical Technology in Hospital Pharmacy

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Abstract Background Viscous oral solutions of budesonide (dose range: 1 mg to 2 mg) have long been used to treat eosinophilic oesophagitis in children. The objective of the present study was to provide a convenient paediatric pharmaceutical formulation of a viscous budesonide solution at a dose level of 0.1 mg/mL, using cyclodextrin as a solubilizer. Methods Solubility studies were performed with γ-cyclodextrin and hydroxypropyl-β-cyclodextrin, and viscosity was tested with a Brookfield viscometer. The stability of the final formulation was tested in a climatic chamber. Levels of budesonide, budesonide impurities and degradation products were assayed using the HPLC–UV method described for the budesonide-related substance assay in the European Pharmacopoeia monograph. Results The solubility of budesonide increased linearly with both cyclodextrins. Gamma cyclodextrin (complexation efficiency: 0.147) was preferred to hydroxypropyl-β-cyclodextrin (complexation efficiency: 0.064) as a solubilizing agent. Hydroxypropylcellulose (1 % m/v) was added to increase viscosity, and sucralose was added to improve palatability. The sterilized, filtered, final formulation was stable for at least 3 months when packed aseptically in sterile 15 mL type 1 amber glass vials. Conclusions We have developed a convenient, stable, preservative-free, viscous formulation of a budesonide solution for the hospital- and home-based treatment of paediatric patients.

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Section: Discussionsupporting

confidence: 89%

Paediatric formulation: budesonide 0.1 mg/mL viscous oral solution for eosinophilic esophagitis using cyclodextrins

Hosselet

Villon

et al. 2018

Pharmaceutical Technology in Hospital Pharmacy

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“…1H,2H,2H,2.99 (t,J=5.0 Hz,1H,1H,1H,2H,1H,3H,4H,2H, + , 431.2434 andC25H34O6Na + , 453.2253). The spectroscopic data obtained for compound 1 were corroborated with the references (Bhutnar et al 2017;Yan et al 2019).…”

Section: Spectral Datasupporting

confidence: 72%

Anti-inflammatory and anti-arthritic effects of compounds from Buddleja coriacea

Ticona

Callisaya²,

Rico

et al. 2022

Natural Product Research

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Buddleja coriacea (B. coriacea) commonly known as "Kiswara" is used as infusions for stomach and joint pain. This study aims to evaluate the in vitro and in vivo anti-inflammatory and anti-arthritic activity was evaluated by measuring inflammatory parameters (TNF-α, C-reactive protein and Fibrinogen) in murine models of the aqueous extract and isolated compounds of B. coriacea. A bio-guided phytochemical analysis based on NMR/MS was performed identifying three (1-3) compounds of the aqueous extract. All compounds inhibited the production of TNF-α in RAW 264.7 cell line, with IC50 of 13.44 (1), 1.13 (2) and 0.57 μM (3), respectively. In addition, compounds 2 and 3 decreased the levels of TNF-α, C-reactive protein and fibrinogen at a concentration of 5 mg/kg in murine models. Our research shows that the compounds isolated from B. coriacea have anti-inflammatory and anti-arthritic properties, providing scientific evidence for the traditional use of this plant species.

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“…The FT-IR spectra of budesonide shows required frequencies like 3486 (O-H stretching), 2956, 2939, 2872 (aliphatic C-H stretching), 1723, 1666 (C=O stretching), 1405, 1393 (-CH 3 bending) and 1164, 1134, 1097 (C-O-C stretching) (cm −1 ) which agree with the essential functional groups present in product. A typical budesonide mass spectra (LCMS/MS API 2000) has m/e ratios corresponding to small fragments along with required molecule ion peak (M + 1 = 431), as reported earlier (Table 3 ) [ 30 , 31 ]. The NMR of budesonide in DMSO-d 6 and the chemical shift values identified in 1 H NMR and 13 C NMR are presented in Tables 4 and 5 .…”

Section: Resultsmentioning

confidence: 53%

Continuous flow process for preparing budesonide

et al. 2022

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Budesonide, a glucocorticosteroid, is used as anti-asthmatic drug that became generic in 2019. Existing preparation methods of budesonide require utilization of corrosive acids and involve expensive purification process. Thus, a new cost-effective continuous flow process for the synthesis of budesonide which belongs to the class of 16,17 acetals of pregnane core, is discussed in the present research findings. Flow reactor parameters such as flow rate, temperature, residence time, solution volumes, anti-solvents and reactor frequency are subjected to investigation on the preparation of molar ratio of budesonide epimers. Further, the suitable parameters entail for obtaining the desired molar ratio of epimers. In another aspect, particle size optimization studies are also performed to get the desired budesonide solid product. A continuous flow process for preparation of budesonide is identified from the present research investigation which can be readily transferred to industrial scale up. Graphical abstract

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Isolation and Characterization of Photodegradation Impurity in Budesonide Drug Product Using LC-MS and NMR Spectroscopy

Cited by 10 publications

References 14 publications

Paediatric formulation: budesonide 0.1 mg/mL viscous oral solution for eosinophilic esophagitis using cyclodextrins

Paediatric formulation: budesonide 0.1 mg/mL viscous oral solution for eosinophilic esophagitis using cyclodextrins

Anti-inflammatory and anti-arthritic effects of compounds from Buddleja coriacea

Continuous flow process for preparing budesonide

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