title: A validated Ultra High Pressure Liquid Chromatographic method for the characterisation of confiscated illegal slimming products containing anorexics.
abstract: A fully validated UHPLC-DAD method for the identification and quantification of pharmaceutical preparations, containing molecules frequently found in illegal slimming products (sibutramine, modafinil, ephedrine, nor-ephedrine, metformin, theophyllin, caffeine, diethylpropion and orlistat) was developed. The proposed method uses a Vision HT C18-B column (2 mm × 100 mm, 1.5 μm) with a gradient using an ammonium acetate buffer pH 5.0 as aqueous phase and acetonitrile as organic modifier. The obtained method was fully validated based on its measurement uncertainty (accuracy profile). Calibration lines for all components were linear within the studied ranges. The relative bias and the relative standard deviations for all components were respectively smaller than 3.0% and 1.5%, the β-expectation tolerance limits did not exceed the acceptance limits of 10% and the relative expanded uncertainties were smaller than 3% for all of the considered components. A UHPLC-DAD method was obtained for the identification and quantification of these kind of pharmaceutical preparations, which will significantly reduce analysis times and workload for the laboratories charged with the quality control of these preparations and which can, if necessary, be coupled to a MS-detector for a more thorough characterisation.
authors.affiliation: Division of food, Medicines and Consumer Safety, Section Medicinal Products, Scientific Institute of Public Health-IPH, J. Wytmansstraat 14, B-1050 Brussels, Belgium.
authors.forename: E
authors.initials: E
authors.lastname: Deconinck
authors.forename: K
authors.initials: K
authors.lastname: Verlinde
authors.forename: P
authors.initials: P
authors.lastname: Courselle
authors.forename: J O De
authors.initials: JO
authors.lastname: Beer
mesh_terms: D001067:Appetite Depressants / Q000032:analysis*; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods / Q000592:standards; D019587:Dietary Supplements / Q000032:analysis* / Q000592:standards*; D004338:Drug Combinations; D004340:Drug Contamination / Q000331:legislation & jurisprudence*; D057230:Limit of Detection; D016014:Linear Models; D012015:Reference Standards; D015203:Reproducibility of Results
chemical_list: D001067:Appetite Depressants; D004338:Drug Combinations