HOMEPRODUCTSCOMPANYCONTACTFAQResearchDictionaryPharmaSign Up FREE or Login

A general analytical platform and strategy in search for illegal drugs.

Abstract
An effective screening procedure to identify and quantify active pharmaceutical substances in suspected illegal medicinal products is described. The analytical platform, consisting of accurate mass determination with liquid chromatography time-of-flight mass spectrometry (LC-QTOF-MS) in combination with nuclear magnetic resonance (NMR) spectroscopy provides an excellent analytical tool to screen for unknowns in medicinal products, food supplements and herbal formulations. This analytical approach has been successfully applied to analyze thousands of samples. The general screening method usually starts with a methanol extraction of tablets/capsules followed by liquid chromatographic separation on a Halo Phenyl-Hexyl column (2.7μm; 100mm×2.1mm) using an acetonitrile/0.1% formic acid gradient as eluent. The accurate mass of peaks of interest was recorded and a search made against an in-house database containing approximately 4200 substances, mostly pharmaceutical compounds. The search could be general or tailored against different classes of compounds. Hits were confirmed by analyzing a reference substance and/or by NMR. Quantification was normally performed with quantitative NMR (qNMR) spectroscopy. Applications for weight-loss substances like sibutramine and orlistat, sexual potency enhancement (PDE-5 inhibitors), and analgesic drugs are presented in this study. We have also identified prostaglandin analogues in eyelash growth serum, exemplified by isopropyl cloprostenate and bimatoprost. For creams and ointments, matrix solid-phase dispersion (MSPD) was found to give a clean extracts with high recovery prior to LC-MS analyses. The structural elucidation of cetilistat, a new weight-loss substance recently found in illegal medicines purchased over the Internet, is also presented.
AuthorsMonika Johansson, Dick Fransson, Torgny Rundlöf, Ngoc-Hang Huynh, Torbjörn Arvidsson
JournalJournal of pharmaceutical and biomedical analysis (J Pharm Biomed Anal) Vol. 100 Pg. 215-229 (Nov 2014) ISSN: 1873-264X [Electronic] England
PMID25171485 (Publication Type: Journal Article)
CopyrightCopyright © 2014 Elsevier B.V. All rights reserved.
Chemical References
  • Counterfeit Drugs
  • Dosage Forms
  • Solvents
  • Methanol
Topics
  • Chromatography, High Pressure Liquid (methods)
  • Counterfeit Drugs (analysis)
  • Databases, Pharmaceutical
  • Dosage Forms
  • Magnetic Resonance Spectroscopy (methods, standards)
  • Methanol (chemistry)
  • Molecular Structure
  • Molecular Weight
  • Quality Control
  • Reproducibility of Results
  • Solvents (chemistry)
  • Spectrometry, Mass, Electrospray Ionization (methods, standards)
  • Tandem Mass Spectrometry (methods, standards)

Join CureHunter, for free Research Interface BASIC access!

Take advantage of free CureHunter research engine access to explore the best drug and treatment options for any disease. Find out why thousands of doctors, pharma researchers and patient activists around the world use CureHunter every day.
Realize the full power of the drug-disease research graph!


Choose Username:
Email:
Password:
Verify Password:
Enter Code Shown: