Identification and characterization of unknown degradation impurities in beclomethasone dipropionate cream formulation using HPLC, ESI-MS and NMR

Elumalai, Sambandan; Thenmozhi, Kathavarayan; Senthilkumar, Sellappan; Shiea, Jentaie; Ponnusamy, Vinoth Kumar

doi:10.1016/j.jpba.2019.02.013

Cited by 8 publications

(7 citation statements)

References 29 publications

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“…A large number of factors can affect the stability of a pharmaceutical product, that includes manufacturing process, stability of the molecule, storage conditions (temperature, exposure to light and humidity), as well as chemical reactions such as oxidation, reduction, hydrolysis, and racemization, which could occur after dilution of the drug before administration. The analyses carried out allowed not only the determination of the stability of the four drugs studied, but also the exclusion of degradation products, and impurities already known in literature for all tested drugs [12,15,16,21] (Figure 3).…”

Section: Resultsmentioning

confidence: 99%

“…This study aims to evaluate the stability in aerosol containers of two mucolytic agents, N-acetylcysteine (300 mg/3 ml) and ambroxol (15 mg /2ml), and two corticosteroids beclomethasone dipropionate (800 μg /2ml) and budesonide (0.50 mg /2ml and 0.25 mg /2ml), after dilution with Sirmione thermal water stored in plastic ampoules, for aerosol therapy. A large number of analytical methods for the determination and quantifi cation of N-acetylcysteine [11,12], ambroxol [13,14], budesonide [15] and beclomethasone dipropionate [16,17] in pharmaceutical preparations have been developed. However, in spite of the structural diversity and different chemical-physical properties of these drugs (Figure 1), mainly due to the presence of excipients (sodium edetate, polysorbate 80, polysorbate 20, and sorbitan laurate) that can interfere with the separation process, no method was found for their simultaneous analysis.…”

Section: Introductionmentioning

confidence: 99%

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Chemical and physical stability of selected drugs for aerosol therapy with Sirmione thermal water

Cuna¹,

Sturani²,

Galfrè³

et al. 2021

Open Journal of Chemistry

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Chemical and physical stability of selected drugs for aerosol therapy with Sirmione thermal water

Cuna¹,

Sturani²,

Galfrè³

et al. 2021

Open Journal of Chemistry

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“…Stock solutions of BDP (800 µg/mL), testosterone (125 µg/mL), methylparaben (1440 µg/mL), ethylparaben (1440 µg/mL), beclomethasone (80 µg/mL), 17-BMM (400 µg/mL), and 21-BMM (400 µg/mL) were all prepared with acetonitrile. Beclomethasone, 17-BMM and 21-BMM are possible by-products produced by the hydrolysis of BDP esters in the formulations 10 11. All stock solutions were stored at room temperature and protected from light.…”

Section: Methodsmentioning

confidence: 99%

Stability assessment and content determination test of oral liquid forms of beclomethasone dipropionate prepared in hospital pharmacy

Saeki,

Sakamoto,

Saito

et al. 2023

Eur J Hosp Pharm

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ObjectivesOral beclomethasone dipropionate (BDP) is known for its use as a therapeutic medicine for gastrointestinal graft-versus-host disease (GI-GVHD). Despite growing demand for oral BDP formulation, no commercial forms have yet been marketed. Therefore, at the Tokyo Metropolitan Cancer and Infectious Disease Centre Komagome Hospital, pharmacists prepare oral liquid forms of BDP for patients with upper GI-GVHD. This study aims to develop a new high performance liquid chromatography (HPLC) method for measuring BDP in the prepared formulations and assessing its quality.MethodsWe developed a new HPLC method for measuring BDP in prepared formulations validated according to international guidelines. Three types of formulations were prepared and analysed using the validated HPLC method. One contains 1 mg of BDP per 30 mL aqueous solution, and the others using ethanol for preparation contain 1 mg of BDP per 15 mL aqueous solution. For stability assessment, the BDP contents were assayed while formulations were stored in plastic bottles for 8 weeks under two different conditions of 25°C in bright light and 4°C in darkness. A content determination test was also conducted to assess the individual contents of BDP and lot-to-lot variation in dosage units.ResultsA stability test demonstrated that the remaining BDP content after the storage period was greater than 90% of the initial content in almost all samples regardless of storage conditions. A content determination test showed thattwo new ethanol-containing formulations contained about 0.1 mg more BDP than the original ethanol-free formulation and it was close to the target BDP content of 1 mg. Furthermore, new formulations had less lot-to-lot BDP variation in dosage units than the original formulation.ConclusionsA new HPLC method for measuring BDP in prepared formulations was developed and validated. The results of the stability test and content determination test indicated that the newly designed formulations were superior to the conventional formulation.

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“…It is well‐known that corticosteroids act as immunomodulatory agents and possess anti‐inflammatory properties (Hotha et al, 2020). HLN is contraindicated for individuals with a history of hypersensitivity, as well as those with fungal skin diseases and untreated bacterial and viral skin diseases such as varicella, herpes simplex, and vaccinia (Sambandan et al, 2019). Stability analysis constitutes a crucial aspect of drug discovery and development.…”

Section: Introductionmentioning

confidence: 99%

Identification and structural characterization of major stress degradation products of halcinonide by liquid chromatography–high‐resolution mass spectrometry

Giri,

Badgujar,

Paritala

et al. 2023

Biomedical Chromatography

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Halcinonide is a topical corticosteroid approved by the US Food and Drug Administration (FDA), known for its anti‐inflammatory and antipruritic properties. The therapeutic benefits of halcinonide have rendered it an effective treatment regimen for various dermatological conditions such as psoriasis, dermatitis, and eczema. However, stability of the drug substance is a prerequisite in determining the therapeutic efficacy and plays a crucial role during formulation development and long‐term storage. As corticosteroids are highly susceptible to degradation, the current study aims to expose halcinonide to different stress conditions and understand its stability behavior. An HPLC method was developed for the separation of halcinonide and its degradation products. Separation was accomplished in gradient mode using an Eclipse Plus C18 column (250 × 4.5 mm, 5 μm) with ammonium formate (10 mM, pH 6.5) and acetonitrile as the mobile phases. LC–Q‐TOF/MS/MS studies were conducted on halcinonide, which led to the identification of degraded products using optimized mass parameters. A potential mechanistic degradation pathway for halcinonide, along with the major identified degradation products has been established. The chromatographic method that was developed has been validated in compliance with the Q2(R1) guideline of the International Council for Harmonization. ProTox‐II was used to perform in silico toxicity studies in order to evaluate the toxicity potential of both halcinonide and the identified degradation products.

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Identification and characterization of unknown degradation impurities in beclomethasone dipropionate cream formulation using HPLC, ESI-MS and NMR

Cited by 8 publications

References 29 publications

Chemical and physical stability of selected drugs for aerosol therapy with Sirmione thermal water

Chemical and physical stability of selected drugs for aerosol therapy with Sirmione thermal water

Stability assessment and content determination test of oral liquid forms of beclomethasone dipropionate prepared in hospital pharmacy

Identification and structural characterization of major stress degradation products of halcinonide by liquid chromatography–high‐resolution mass spectrometry

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