ABSTRACT
A method was developed and validated for the determination of 16 prostaglandin analogs in cosmetic products. The QuEChERS (Quick, Easy, Cheap, Efficient, Rugged, Safe) liquid-liquid extraction method, typically used for pesticide residue analysis, was utilized as the sample preparation technique. The prostaglandin analogs were chromatographically separated and quantified using high performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS). Thirty-one cosmetic products were surveyed, and 13 products were determined to contain a prostaglandin analog with amounts ranging from 27.4 to 297µg/g. The calculated concentrations for the cosmetic products were in a similar range when compared to the concentrations of three different prostaglandin analog-containing prescription products.
Subject(s)
Chromatography, High Pressure Liquid/methods , Cosmetics/chemistry , Prostaglandins, Synthetic/chemistry , Tandem Mass Spectrometry/methods , Molecular Structure , Prostaglandins, Synthetic/isolation & purification , Solid Phase ExtractionABSTRACT
An isocratic high-performance liquid chromatographic (HPLC) method was developed to determine the enantiomeric purity of a benzindene prostaglandin (U-62,840) which is currently being evaluated for pharmaceutical applications. The enantiomers were converted to diastereomeric amide derivatives using optically pure S-(--)-1-phenylethylamine (greater than 99.9%). Separation of the diastereomers was demonstrated on achiral silica-based stationary phases using a hexane-dioxane-water mobile phase and UV detection at 214 nm. Due to the use of an optical derivatizing agent, method validation addressed the issues of optical purity of the reagent and comparative rates of reaction of each enantiomer. Analytical data is reported that demonstrates quantitative derivation, linearity, accuracy, precision, and ruggedness of the optimized assay conditions. Limit of quantitation for the enantiomeric impurity was determined to be 1.1% (signal-to-noise ratio 13). A brief description of the results of a parallel study of an enantiomeric separation using various chiral HPLC columns is included.
Subject(s)
Prostaglandins, Synthetic/isolation & purification , Prostaglandins/isolation & purification , Chromatography, High Pressure Liquid , Indicators and Reagents , Phenethylamines/analysis , StereoisomerismABSTRACT
PGBx, a new polymeric derivative of PGB1, previously was shown to (a) restore oxidative phosphorylation to degraded isolated rat liver mitochondria in vitro and (b) to reverse the effects of cardiogenic ischemia in monkeys and cerebral ischemia in rabbits. This report describes in detail the synthesis and purification of PGBx via PGB1, starting with azelaic acid. Details of the in vitro mitochondrial assay are also reported. Purified PGBx exhibiting maximal reactivation of mitochondrial phosphorylation has a mean molecular weight of 2350. Yield of PGBx based on azelaic acid is 4% and based on PGB1 is 25%.
