Issue 3, 2022

Microwave-assisted extraction for further Cl, Br, and I determination in medicinal plants by ICP-MS: a study of carbon interferences

Abstract

A microwave-assisted extraction (MAE) method for further Cl, Br, and I determination in medicinal plants was developed. Halogen determination was performed by inductively coupled plasma mass spectrometry (ICP-MS) and a study on carbon interferences was carried out using a sample extract. The sample mass used for the optimization of the MAE method was 0.5 g. The following parameters for MAE were evaluated: the extraction solution (6 or 10 mL of water, 100 mmol L−1 NH4OH, or 100 mmol L−1 TMAH), extraction time (5 or 20 min), and temperature (90 or 240 °C). The accuracy was evaluated by analyte recovery experiments, by using certified reference materials (CRMs), and by comparing the results with those obtained using a reference method (microwave-induced combustion). Using the optimized extraction conditions (6 mL of 100 mmol L−1 TMAH solution and 5 min of microwave heating at 240 °C), no statistical difference was observed in comparison to the certified values. Recoveries were close to 95% and the relative standard deviation was lower than 8%. The carbon concentration in the extracts using H2O, 100 mmol L−1 NH4OH or 100 mmol L−1 TMAH was in the range of 980 to 9800 mg L−1. In a systematic study of interferences with the sample extract, no interferences were observed for Cl and Br up to 1000 mg L−1 of carbon in solution. On the other hand, it was possible to observe signal enhancement for I with 500 mg L−1 of carbon. Thus, a dilution step was needed to obtain an accurate analytical response for this element. Blank values were always negligible resulting in relatively low limits of quantification: 125, 0.125, and 0.045 μg g−1 for Cl, Br, and I, respectively. In this way, the proposed MAE method was considered suitable, simple and fast for further Cl, Br, and I determination by ICP-MS. However, care regarding the carbon content to avoid erroneous signal enhancement is necessary.

Graphical abstract: Microwave-assisted extraction for further Cl, Br, and I determination in medicinal plants by ICP-MS: a study of carbon interferences

Article information

Article type
Paper
Submitted
12 N’w 2021
Accepted
09 Yan 2022
First published
09 Yan 2022

J. Anal. At. Spectrom., 2022,37, 535-543

Microwave-assisted extraction for further Cl, Br, and I determination in medicinal plants by ICP-MS: a study of carbon interferences

M. S. Nascimento, G. T. Druzian, L. S. F. Pereira, M. F. Mesko, R. S. Picoloto, P. A. Mello and E. M. M. Flores, J. Anal. At. Spectrom., 2022, 37, 535 DOI: 10.1039/D1JA00429H

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