Gas chromatography/trace analysis of derivatized azelaic acid as a stability marker.

Azelaic acid, a naturally occurring saturated dicarboxylic acid, is found in many topical formulations for its various medical benefits or as a byproduct of the oxidative decomposition of unsaturated fatty acids. The poor volatility of azelaic acid hinders its applicability in GC analysis. Therefore, azelaic acid was derivatized by methylation and silylation procedures to enhance its volatility for GC analysis. Accordingly, dimethyl azelate (DMA) and di(trimethylsilyl) azelate were synthesized and characterized by GC-MS. Subsequently, a GC with flame ionization detection method was developed and validated to analyze trace amounts of azelaic acid in some marketed skin creams. Unlike DMA, di(trimethylsilyl) azelate was chemically unstable and degraded within few hours. Nonane was used as a stable internal standard. Variability due to derivatization and extraction was controlled by a standard addition procedure. DMA analysis was linear in a wide concentration range (100 ng/mL to 100 mg/mL). Moreover, the method was accurate (96.4-103.4%) and precise with inter- and intraday variability <2.0% and LOQ and LOD of 100 and 10 ng/mL, respectively.

Physicochemical studies on Ciclopirox olamine complexes with divalent metal ions.

Ciclopirox olamine (CPO) metal complexes have been prepared and characterized using elemental analysis, infra red (IR), melting point and differential scanning calorimetry (DSC). Spectroscopic titration using molar ratio method indicated the occurrence of 1:1 complexes for CPO with almost all the examined metals. Physicochemical properties were also studied including aqueous solubility and apparent partition coefficient. Results showed that generally complex formation dramatically decreased the solubility and increased apparent partition coefficient. However, some metal complexes exhibited opposite effect. It could be concluded that complex formation can modify the solubility and apparent partition coefficient, which may suggest the use of complexes to manipulate the physicochemical properties of the drug.