A stability-indicating HPLC assay method for budesonide

Hou, Shuguang; Hindle, Michael; Byron, Peter R.

doi:10.1016/s0731-7085(00)00424-6

Cited by 34 publications

(15 citation statements)

References 10 publications

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“…Assuming equal intensity for both isomers, and absence of stereoselective reactions for 22S epimer, the most abundant peak in post-administration samples, eluting at 9.7 min was proposed to be the 22S epimer. This is in agreement with previous studies where the epimers were separated in similar chromatographic conditions (column and mobile phase), and the 22R epimer eluted first than the 22S epimer [28].…”

Section: Detection Of Budesonide Metabolites By Lc-ms/mssupporting

confidence: 93%

Identification of budesonide metabolites in human urine after oral administration

Matabosch¹,

Pozo²,

Pérez‐Mañá

et al. 2012

Anal Bioanal Chem

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Budesonide (BUD) is a glucocorticoid widely used for the treatment of asthma, rhinitis, and inflammatory bowel disease. Its use in sport competitions is prohibited when administered by oral, intravenous, intramuscular, or rectal routes. However, topical preparations are not prohibited. Strategies to discriminate between legal and forbidden administrations have to be developed by doping control laboratories. For this reason, metabolism of BUD has been re-evaluated using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with different scan methods. Urine samples obtained after oral administration of 3 mg of BUD to two healthy volunteers have been analyzed for metabolite detection in free and glucuronide metabolic fractions. Structures of the metabolites have been studied by LC-MS/MS using collision induced dissociation and gas chromatography-mass spectrometry (GC/MS) in full scan mode with electron ionization. Combination of all structural information allowed the proposition of the most comprehensive picture for BUD metabolism in humans to this date. Overall, 16 metabolites including ten previously unreported compounds have been detected. The main metabolite is 16α-hydroxy-prednisolone resulting from the cleavage of the acetal group. Other metabolites without the acetal group have been identified such as those resulting from reduction of C20 carbonyl group, oxidation of the C11 hydroxyl group and reduction of the A ring. Metabolites maintaining the acetal group have also been identified, resulting from 6-hydroxylation (6α and 6β-hydroxy-budesonide), 23-hydroxylation, reduction of C6-C7, oxidation of the C11 hydroxyl group, and reduction of the C20 carbonyl group. Metabolites were mainly excreted in the free fraction. All of them were excreted in urine during the first 24 h after administration, and seven of them were still detected up to 48 h after administration for both volunteers.

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Section: Detection Of Budesonide Metabolites By Lc-ms/mssupporting

confidence: 93%

Identification of budesonide metabolites in human urine after oral administration

Matabosch¹,

Pozo²,

Pérez‐Mañá

et al. 2012

Anal Bioanal Chem

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“…This method was adapted from a method previously developed as a quantitative HPLC-UV assay for budesonide [23]. A flow splitter (Upchurch Scientific Inc., Oak Harbor, WA) was used after the HPLC column so that approximately 1.2 mL/min of the eluent was delivered to the PDA detector, and about 0.3 mL/min introduced to the electrospray probe of the mass spectrometer.…”

Section: Lc-ms Conditionsmentioning

confidence: 99%

Chromatographic and mass spectral characterization of budesonide and a series of structurally related corticosteroids using LC–MS

Hou

Hindle

Byron

2005

Journal of Pharmaceutical and Biomedical Analysis

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“…A review of literature revealed that all HPLC methods published so far for budesonide are based on separation of two epimers even though both epimers are similar in their potency with respect to their anti-inflammatory activity [39][40][41]. Since our work involved design and development of pulmonary drug delivery systems for budesonide, our objective was to develop a simple, rapid and stability indicating HPLC method of analysis.…”

Section: Development Of Hplc Methods For Estimation Of Budesonidementioning

confidence: 99%

Preparation and In Vitro Evaluation of Budesonide Spray Dried Microparticles for Pulmonary Delivery

Naikwade

2009

Sci. Pharm.

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The present study describes development and in vitro evaluation of budesonide microparticles prepared by spray drying for delivering drug directly to lungs via dry powder inhaler. This paper introduces new formulations for pharmaceutical applications which includes conventional formulations and novel spray dried microparticles viz., pulmosols, microspheres and porous particles. Optimized spray drying parameters for generation of microparticles were: inlet temperature, 130 °C; outlet temperature, 80 °C; aspirator rate, 240 mWc (60%); solution feed rate, 2 ml/min; spraying air flow pressure, 2 bar. Microparticles appeared to be spherical, low-density particles characterized by smooth surface. MMAD and GSD ranged from 2.5-4.6 µm and 1.5-2.7 respectively. Effective index of microspheres (54.48) and porous particle formulations (64.22) was higher than the conventional formulation (49.21) indicating more effective deposition of microparticles to the lungs. Carr's Index (20-30%) and Hausner ratio (1.2-1.7) for all formulations indicated good powder flow properties. Formulations emitted a fine particle fraction of 25-47%. Microparticles showed extended in vitro drug release upto 4 hours with high respirable fractions, thus use of microparticles potentially offers sustained release profile along with improved delivery of drug to the pulmonary tract.

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A stability-indicating HPLC assay method for budesonide

Cited by 34 publications

References 10 publications

Identification of budesonide metabolites in human urine after oral administration

Identification of budesonide metabolites in human urine after oral administration

Chromatographic and mass spectral characterization of budesonide and a series of structurally related corticosteroids using LC–MS

Preparation and In Vitro Evaluation of Budesonide Spray Dried Microparticles for Pulmonary Delivery

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