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Upcoming ASMS Abstract - Tuesday Poster 352
Rapid Screening and Confirmation of PDE5 Inhibitors in Dietary Ingredients by DART-MS Ambient Ionization Robert Goguen, Julie Carbonello, Elizabeth Crawford, and Brian Musselman IonSense, Inc., Saugus, MA 01906, USA Phosphodiesterase type 5 inhibitors (PDE5 Inhibitors) are used to treat erectile dysfunction (ED). Numerous different PDE5's have been detected in herbal supplements, vitamin tablets and adulterated pharmaceuticals. In response to this adulteration problem the AOAC has issued a call for methods focused on development of technologies for rapid determine the presence of various PDE5s in dietary ingredients. This work describes the method we have developed to address this adulteration problem. Analysis of PDE-5 inhibitor standards at multiple concentrations was completed using a Direct Analysis in Real Time (DART-SVP) ambient ionization source coupled to both a HRMS and a QQQ LC/MS system. Samples and standards were prepared for analysis by dissolving a quantity with solvents. For preparation of adulterated materials, an aliquot of each standard solution was applied directly to the supplement material and allowed to dry before extraction. 33 replicates of each supplement were analyzed. The [M+H]+ with accurate mass assignment was used to confirm PDE5s presence in the screening method. Statistical analysis of the accuracy of the method was assessed for each of the analytes in each type of sample. An MS/MS method was used for the confirmation method.
DART-MS for rapid, preliminary screening of urine for DMAA
Ashton D. Lesiak, Kendra J. Adams, Marek A. Domin, Colin Henck and Jason R. E. Shepard Boston College and University of Albany Dimethylamylamine (DMAA) is a sympathomimetic amine found in weight-loss/workout supplements or used as an appetite suppressant. DMAA is a stimulant that is banned by the World Anti-Doping Agency (WADA). Adverse health effects as well as fatalities have been implicated with its use. Direct analysis in real time mass spectrometry (DART-MS) is an ambient ionization method that was employed to rapidly identify the presence of DMAA in various samples without any extraction or preparations whatsoever. DMAA was first identified in supplements, sampled directly in their solid forms. Furthermore, DMAA was detected directly in urine over 48 h as a means of indicating recent abuse of the substance. DART-MS analysis is instantaneous, and coupled with the high mass accuracy associated with the time-of-flight mass analyzer, results in unequivocal identification of the presence of DMAA. These features demonstrate DART-MS as an attractive potential alternative screening method for the presence of drugs and medications or for toxicological investigations. Copyright ? 2013 John Wiley & Sons, Ltd. Just dip it: online coupling of "Dip-it" polymer monolith microextraction with plasma assisted laser desorption ionization mass spectrometry
Xin Wang, Xianjiang Li, Yu Bai and Huwei Liu
Beijing University
A polymer monolith microextraction (PMME) procedure coupled to plasma assisted laser desorption ionization mass spectrometry (PMME-PALDI-MS) was developed for rapid and organic solvent-free trace analysis. The extraction device used a "Dip-it" sampler coated with a MWNT incorporated monolith, and the analytes adsorbed on monoliths were effectively desorbed by laser, improving detection sensitivity.
Rapid screening for synthetic antidiabetic drug adulteration in herbal dietary supplements using direct analysis in real time mass spectrometry
Zhigui Zhou, Jialing Zhang, Wei Zhang, Yu Bai and Huwei Liua
Adulteration of herbal supplements with synthetic drugs is illegal. A rapid and reliable method which utilizes direct analysis in real time mass spectrometry (DART-MS) was developed for the identification of seven synthetic antidiabetic drugs used as adulterants in herbal dietary supplements. The supplement sample was simply extracted with methanol/water by manually shaking several times and directly analyzed using DART-MS. The presence of synthetic drug adulterants was confirmed through the accurate m/z values and MS/MS data obtained via quadruple time of flight mass spectrometry (QTOF MS). Parameters for the DART source were systematically optimized, and the limits of detection (LODs) in herbal supplement matrices were measured. This method was successfully applied to examine five commercial herbal dietary supplements, and two of them proved to be adulterated with metformin without labeling.
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