title: Simple HPLC method for detection of trace ephedrine and pseudoephedrine in high-purity methamphetamine.
abstract: A simple and sensitive HPLC technique was developed for the qualitative determination of ephedrine and pseudoephedrine (ephedrines), used as precursors of clandestine d-methamphetamine hydrochloride of high purity. Good separation of ephedrines from bulk d-methamphetamine was achieved, without any extraction or derivatization procedure on a CAPCELLPACK C18 MGII (250 × 4.6 mm) column. The mobile phase consisted of 50 mM KH2 PO4-acetonitrile (94:6 v/v %) using an isocratic pump system within 20 min for detecting two analytes. One run took about 50 min as it was necessary to wash out overloaded methamphetamine for column conditioning. The analytes were detected by UV absorbance measurement at 210 nm. A sample (20 mg) was simply dissolved in 1 mL of water, and a 50 μL aliquot of the solution was injected into the HPLC. The detection limits for ephedrine and pseudoephedrine in bulk d-methamphetamine were as low as 3 ppm each. This analytical separation technique made it possible to detect ephedrine and/or pseudoephedrine in seven samples of high-purity d-methamphetamine hydrochloride seized in Japan. The presence of trace ephedrines in illicit methamphetamine may strongly indicate a synthetic route via ephedrine in methamphetamine profiling. This method is simple and sensitive, requiring only commonly available equipment, and should be useful for high-purity methamphetamine profiling.
authors.affiliation: Graduate School of Pharmaceutical Sciences, The University of Tokyo, 7-3-1, Hongo, Bunkyo-ku, Tokyo, 113-0033, Japan. ymakino@mol.f.u-tokyo.ac.jp
authors.forename: Yukiko
authors.initials: Y
authors.lastname: Makino
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004809:Ephedrine / Q000032:analysis*; D057230:Limit of Detection; D008694:Methamphetamine / Q000737:chemistry*; D054199:Pseudoephedrine / Q000032:analysis*; D012015:Reference Standards; D013056:Spectrophotometry, Ultraviolet
chemical_list: D008694:Methamphetamine; D054199:Pseudoephedrine; D004809:Ephedrine