title: High-performance liquid chromatography analysis of anti-inflammatory pharmaceuticals with ultraviolet and electrospray-mass spectrometry detection in suspected counterfeit homeopathic medicinal products.
abstract: A simple high-performance liquid chromatography (HPLC) method with both ultraviolet (UV) and electrospray ionisation mass spectrometry (ESI-MS) detection has been developed for the determination of seven pharmaceuticals in counterfeit homeopathic preparations. Naproxen, Ketoprofen, Ibuprofen, Diclofenac, Piroxicam, Nimesulide and Paracetamol were separated by reversed phase chromatography with acetonitrile-water (0.1% acetic acid) mobile phase, and detected by UV at 245 nm and by ESI-MS in negative ionisation mode with the exception of Paracetamol which was detected in positive ionisation mode. Benzoic acid was used as internal standard (IS). This method was successfully applied to the analysis of homeopathic preparations like mother tinctures, solutions, tablets, granules, creams, and suppositories. Linearity was studied with UV detection in the 50-400 microg mL(-1) range and with ESI-MS in the 0.1-50 microg mL(-1) range. Good correlation coefficients were found in both UV and ESI-MS. Detection limits ranged from 0.18 to 41.5 ng in UV and from 0.035 to 1.00 ng in ESI-MS.
authors.affiliation: Dipartimento del Farmaco, Istituto Superiore di Sanità, Viale Regina Elena 299, 00161 Rome, Italy. apanusa@iss.it
authors.forename: Alessia
authors.initials: A
authors.lastname: Panusa
authors.forename: Giuseppina
authors.initials: G
authors.lastname: Multari
authors.forename: Giampaolo
authors.initials: G
authors.lastname: Incarnato
authors.forename: Luigi
authors.initials: L
authors.lastname: Gagliardi
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005607:Fraud / Q000517:prevention & control*; D006705:Homeopathy; D004364:Pharmaceutical Preparations / Q000592:standards*; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; D004364:Pharmaceutical Preparations