Elemental Analysis of Phytotherapeutic Products by Inductively Coupled Plasma–Tandem Mass Spectrometry

A procedure for the determination of As, Cd, Cr, Ni, Pb, and V in phytotherapy medicines by inductively coupled plasma–tandem mass spectrometry is reported. The use of tandem mass spectrometry with oxygen into an octopole reaction system at various gas flow rates and the combination of on-mass and mass-shift modes was evaluated. Cadmium, Cr, Ni, and Pb were determined as free atomic ions while As and V were determined as the oxides AsO+ and VO+ in the same run. Samples were prepared by microwave-assisted digestion with dilute nitric acid and hydrogen peroxide. Two plant-certified reference materials (apple leaves and tomato leaves) were used to check the accuracy. For tandem mass spectrometry with 0.5 mL min−1 O2, recoveries in the 85–113% were typically obtained and no statistical differences were observed at the 95% confidence level (t-test) in comparison with the certified values. Using these conditions, the limits of detection for the method were 0.01, 0.0002, 0.008, 0.008, 0.003, and 0.002 µg g−1 for As, Cd, Cr, Ni, Pb, and V, respectively. The procedure was used for the analysis of four phytotherapic drugs and the determined concentrations were up to 0.168 µg g−1 As, 0.03 µg g−1 Cd, 0.82 µg g−1 Cr, 1.18 µg g−1 Ni, 0.52 µg g−1 Pb, and 2.4 µg g−1 V with average precision values of 8% as the relative standard deviation. The found concentrations were compared with limits proposed in official guidelines and, in most cases, the values were below the maximum limits allowed.

Palavras-chave

Contaminants, elemental impurity determination, ICP-MS/MS, inductively coupled plasma–tandem mass spectrometry, phytotherapy medicines, spectral interferences, trace analysis