Development and validation of a high-performance liquid chromatographic method for the analysis of budesonide.
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.
Gupta
Mukur
M
Adherex Technologies Inc., Durham, NC 27713, USA.
Bhargava
Hridaya N
HN
D000097:Acetonitriles; D000893:Anti-Inflammatory Agents / Q000032:analysis*; D019819:Budesonide / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D006863:Hydrogen-Ion Concentration; D008863:Microspheres; D010368:Pectins / Q000737:chemistry; D015203:Reproducibility of Results; D013696:Temperature; D013997:Time Factors
D000097:Acetonitriles; D000893:Anti-Inflammatory Agents; D019819:Budesonide; D010368:Pectins; C032159:acetonitrile