title: Combined HPLC-DAD-MS, HPLC-MS(n) and NMR spectroscopy for quality control of plant extracts: the case of a commercial blend sold as dietary supplement.
abstract: The efficiency of 1D and 2D NMR spectroscopy along with HPLC-DAD-MS analyses in characterising the content of a dietary supplement is demonstrated. Experiments directly performed on a lyophilised sample of a commercial product gave details on the quality control of the product. The lack of the marker constituents of some of the declared plant species (Crataegus oxyacantha, Olea europea, Capsella bursa-pastoris and Fumaria officinalis) and the presence of banned adulterants, responsible for the strong antihypertensive effect of the supplement were established. The analyses proved the presence of indole alkaloids belonging to the group of Rauwolfia sp., such as ajmaline, reserpine and yohimbine. Quantitative HPLC analysis showed that the content of reserpine in the product was in the therapeutic range and therefore responsible for the collapses of the patients.
authors.affiliation: Department of Chemistry, Building of Pharmaceutical Sciences, University of Florence, Via Ugo Schiff 6, 50019 Sesto Fiorentino, Firenze, Italy. Electronic address: anastasiakarioti@yahoo.it.
authors.forename: A
authors.initials: A
authors.lastname: Karioti
authors.forename: E
authors.initials: E
authors.lastname: Giocaliere
authors.forename: C
authors.initials: C
authors.lastname: Guccione
authors.forename: G
authors.initials: G
authors.lastname: Pieraccini
authors.forename: E
authors.initials: E
authors.lastname: Gallo
authors.forename: A
authors.initials: A
authors.lastname: Vannacci
authors.forename: A R
authors.initials: AR
authors.lastname: Bilia
mesh_terms: D000470:Alkaloids / Q000032:analysis; D000959:Antihypertensive Agents / Q000009:adverse effects* / Q000032:analysis; D002138:Calibration; D002626:Chemistry, Pharmaceutical; D002851:Chromatography, High Pressure Liquid; D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination; D006801:Humans; D009682:Magnetic Resonance Spectroscopy; D013058:Mass Spectrometry; D060735:Pharmacovigilance; D010936:Plant Extracts / Q000032:analysis*; D018515:Plant Leaves; D010946:Plants, Medicinal; D011786:Quality Control; D011926:Rauwolfia / Q000378:metabolism; D013678:Technology, Pharmaceutical
chemical_list: D000470:Alkaloids; D000959:Antihypertensive Agents; D010936:Plant Extracts
keywords: Dietary supplements; HPLC-UV–MS; HPLC–MS(n); NMR; Phytovigilance; Quality control