title: Detection of undeclared erectile dysfunction drugs and analogues in dietary supplements by ion mobility spectrometry.
abstract: An ion mobility spectrometry (IMS) method was developed to screen for the presence of undeclared synthetic erectile dysfunction (ED) drugs or drug analogues in herbal dietary supplements claiming to enhance male sexual performance. Ion mobility spectra of authenticated reference materials including three FDA approved drugs (sildenafil citrate, tadalafil, vardenafil hydrochloride trihydrate) and five previously identified synthetic analogues (methisosildenafil, homosildenafil, piperidenafil, thiosildenafil, thiomethisosildenafil) were measured to determine their reduced ion mobilities (K(0)). All eight compounds exhibited reduced mobilities between 0.8257 and 1.2876 cm(2)/(Vs). Twenty-six herbal products were then screened for the presence of these compounds, and 15 of the 26 products tested positive for the presence of ED drug or drug analogue adulterants based on their reduced ion mobilities. IMS results were compared against the results obtained from an independent LC/MS reference method for the identical samples. Herbal dietary supplements containing adulterants were classified with 100% accuracy and most of the adulterants were correctly identified by a comparison of the K(0) of the adulterant to the K(0) of the authenticated reference material. The results demonstrate that IMS is a viable method for screening herbal dietary supplements for the presence of ED drug or drug analogue adulterants.
authors.affiliation: FDA, Division of Pharmaceutical Analysis, 1114 Market St., St. Louis, MO 63101, USA. Connie.Gryniewicz@fda.hhs.gov
authors.forename: Connie M
authors.initials: CM
authors.lastname: Gryniewicz
authors.forename: John C
authors.initials: JC
authors.lastname: Reepmeyer
authors.forename: John F
authors.initials: JF
authors.lastname: Kauffman
authors.forename: Lucinda F
authors.initials: LF
authors.lastname: Buhse
mesh_terms: D000328:Adult; D000588:Amines / Q000032:analysis; D002243:Carbolines / Q000032:analysis; D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination; D007172:Erectile Dysfunction / Q000188:drug therapy*; D006801:Humans; D007093:Imidazoles / Q000032:analysis; D007477:Ions / Q000737:chemistry; D008297:Male; D010879:Piperazines / Q000032:analysis; D028321:Plant Preparations / Q000032:analysis; D011687:Purines / Q000032:analysis; D012015:Reference Standards; D000068677:Sildenafil Citrate; D013057:Spectrum Analysis; D013450:Sulfones / Q000032:analysis; D000068581:Tadalafil; D014227:Triazines / Q000032:analysis; D000069058:Vardenafil Dihydrochloride
chemical_list: D000588:Amines; D002243:Carbolines; D007093:Imidazoles; D007477:Ions; D010879:Piperazines; D028321:Plant Preparations; D011687:Purines; D013450:Sulfones; D014227:Triazines; D000069058:Vardenafil Dihydrochloride; D000068581:Tadalafil; D000068677:Sildenafil Citrate