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  • Title: Microwave-assisted digestion using dilute nitric acid solution and investigation of calibration strategies for determination of As, Cd, Hg and Pb in dietary supplements using ICP-MS.
    Author: Pinheiro FC, Babos DV, Barros AI, Pereira-Filho ER, Nóbrega JA.
    Journal: J Pharm Biomed Anal; 2019 Sep 10; 174():471-478. PubMed ID: 31228850.
    Abstract:
    This study proposes an analytical procedure for microwave-assisted sample preparation of dietary supplements for athletes using dilute nitric acid solution followed by determination of elemental impurities (As, Cd, Hg and Pb) by inductively coupled plasma mass spectrometry (ICP-MS) according to the United States Pharmacopeia Chapters 2232 and 233. Calibration strategies as internal standardization (IS), multi-isotope calibration (MICal), and one-point standard addition (OP SA) were applied for correction of matrix effects. The optimization of the sample preparation procedure was performed using Doehlert experimental design based on overall desirability results (residual acidity, dissolved organic carbon and recoveries reached for certified reference material of Typical Diet) for each calibration method evaluated. Accuracy was also evaluated by recovery experiments according to the permissible daily exposure specific for each element and samples were spiked with element concentrations of 0.5J and 1.5J in order to check accuracies for As, Cd, Hg and Pb. Recoveries ranged from 82 to 120% using IS, 90 to 125% using MICal, 88 to 120% using OP SA and the repeatability was demonstrated by a precision lower than 10% RSD. Ten samples of dietary sport supplements were analyzed using the three calibration methods evaluated and the concentrations of As, Cd and Pb determined in eight samples were lower than the limits established by the Chapter 2232.
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