pulmicort and acetonitrile

A simple, rapid, and stability indicating reversed-phase high-performance liquid chromatography (HPLC) method of analysis for budesonide, a novel glucocorticoid prescribed for inflammatory bowel disease, was successfully developed. Budesonide is an epimeric mixture and both the epimers have similar anti-inflammatory activity. All the analytical methods reported in the literature are long and are based on separation of the epimers, thus our objective was to obtain a single sharp peak of the drug and to separate the drug peak from all the other degradation products. The method, was used to quantify budesonide in the developed formulation, employed a Kromasil C8, (150 mm x 4.6 mm) column with an isocratic mobile phase of acetonitrile-phosphate buffer (pH 3.2-0.025 M) (55:45 v/v), at a flow rate of 1.1 mL/min. Budesonide was detected by an ultraviolet detector at 244 nm. The method was validated for linearity, precision, repeatability, sensitivity, and selectivity. Selectivity was validated by subjecting stock solution of budesonide to acidic, basic, oxidative, and thermal degradation. The retention time of budesonide was about 4 min with symmetrical peaks. The method was linear over a concentration range 1-50 microg/mL (R2=0.9995). The limit of detection of budesonide was 0.1 microg/mL and the limit of quantitation was 0.25 microg/mL. The peaks of the degradation products did not interfere with the peak of budesonide. The developed method was used to quantify budesonide in budesonide-loaded micro-particles. Excipients present in the micro-particles did not interfere with the analysis and the recovery of budesonide from micro-particles was quantitative.

Topics: Acetonitriles; Anti-Inflammatory Agents; Budesonide; Chromatography, High Pressure Liquid; Drug Stability; Hydrogen-Ion Concentration; Microspheres; Pectins; Reproducibility of Results; Temperature; Time Factors

A sensitive and rapid high performance liquid chromatography method has been developed and used for the simultaneous determination of formoterol and budesonide in Symbicort Turbuhaler when assessing the aerodynamic characteristics of the emitted dose using Pharmacopoeial methods. This capability results in both time and cost saving. The mobile phase composition was acetonitrile-5 mM sodium dihydrogen orthophosphate, pH 3 (60: 40% v/v), and was passed at 1.5 ml min(-1) through a C18 column with a UV detection (wavelength 214 nm). The method was shown to give good analytical performance in terms of linearity, precision (using phenylpropanolamine as an internal standard), sensitivity and solution stability. The intra-day precision for both formoterol and budesonide were 0.75% and 1.11%, respectively (n = 10). The limit of quantitation for formoterol was 10 microgL(-1) and for budesonide was 120 microgL(-1), and the limit of detection were 3 and 30 microgL(-1), for both formoterol and budesonide, respectively. The method has been applied to determine the content of the emitted dose and the fine particle dose of Symbicort Turbuhaler.

Topics: Acetonitriles; Bronchodilator Agents; Budesonide; Chemistry Techniques, Analytical; Chemistry, Pharmaceutical; Chromatography, High Pressure Liquid; Ethanolamines; Formoterol Fumarate; Hydrogen-Ion Concentration; Nebulizers and Vaporizers; Phenylpropanolamine; Phosphoric Acids; Reproducibility of Results; Sensitivity and Specificity; Spectrophotometry, Ultraviolet