Evaluation of Medicinal Plant Decomposition Efficiency Using Microwave Ovens and Mini-Vials for Cd Determination by TS-FF-AAS

Sample preparation is an important step in the analytical process because it can introduce different error sources. Its efficiency is checked based on the quality and reliability of the data obtained, and the time spent on this task. This work evaluates medicinal plant decomposition parameters using polypropylene mini-vials heated by microwave radiation, applying the single vessel concept. As an example, sample mass amount (5 mg), mixture of oxidant agents (200 µL conc. HNO₃+150 µL 30% v/v H₂O₂), microwave time and power were evaluated by heating 24 mini-vials in both closed-vessel (CV) and focused (F) microwave ovens. In order to achieve the best-optimised condition for sample preparation, cadmium and residual carbon determinations were carried out for all experiments. The residual carbon (between 0.30 and 0.45%) was determined by CHN elemental analysis and the cadmium concentration (up to 0.80 µg g⁻¹) by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) in three different medicinal plants. The accuracy of the proposed methods was assessed using certified reference materials (rye grass, BCR 281 and bovine liver, NIST 1577b) as well as conventional microwave assisted decomposition. The new method used a minimum sample amount (5 mg) and reagent volume (ca. 400 µL) and only 4 and 10 min of microwave sample decomposition for CV and F ovens, respectively. In addition, the capacity of both microwave ovens was increased up to 4 times while contamination risks were inherently reduced with the single vessel concept.