title: Detection of Synthetic Drugs as Adulterants in Natural and Herbal Slimming Products by LC-ESI-MS/MS with Polarity Switching.
abstract: The purpose of this study was to develop an LC-tandem MS method for the simultaneous detection of common synthetic drugs as adulterants in natural and herbal slimming products. Sixteen drugs belonging to a wide range of pharmaceutical classes were studied. Included in the list of drugs were anorexics, anxiolytics, antidepressants, diuretics, laxatives, and stimulants. The method used a C18 column (4.6 × 50 mm and 1.8 μm particle size). Separation of the drugs was achieved by gradient elution using 4 mM ammonium formate in water + 0.1% formic acid as the aqueous component and 4 mM ammonium formate in methanol + 0.1% formic as the organic component of the mobile phase. As not all of the analytes ionized in the positive mode, the mass spectrometer was operated in the electrospray ionization mode with polarity switching. The samples were extracted with methanol and the use of 50% acetonitrile in water and 50% methanol in water were investigated as diluents for injection into the LC-MS system. Utilizing both diluents, the validation parameters including accuracy, precision, LOD, and LOQ were assessed. The validation results and utilization of the method to analyze a variety of weight-loss supplements indicate that the two diluents give similar results and can be used interchangeably. This knowledge provides the user with the option of selecting either diluent for sample preparation depending on the sample matrix without having to revalidate the method. The method was applied to the analysis of weight-loss supplements available in local pharmacies, herbal pharmacies, and over the Internet.
authors.affiliation: U.S. Department of Health and Human Services, U.S. Food and Drug Administration, Northeast Regional Laboratory, Jamaica, NY 11433.
authors.forename: Phyllis
authors.initials: P
authors.lastname: Wilson
authors.affiliation: U.S. Department of Health and Human Services, U.S. Food and Drug Administration, Northeast Regional Laboratory, Jamaica, NY 11433.
authors.forename: Claude
authors.initials: C
authors.lastname: Masse
mesh_terms: D019440:Anti-Obesity Agents / Q000032:analysis*; D002110:Caffeine / Q000032:analysis; D002853:Chromatography, Liquid; D003503:Cyclobutanes / Q000032:analysis; D004340:Drug Contamination; D020113:Phenolphthalein / Q000032:analysis; D028321:Plant Preparations / Q000032:analysis*; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry
chemical_list: D019440:Anti-Obesity Agents; D003503:Cyclobutanes; D028321:Plant Preparations; D002110:Caffeine; D020113:Phenolphthalein; C058254:sibutramine