Multivariate optimization of simple procedure for determination of Fe and Mg in cassava starch employing slurry sampling and FAAS

- A slurry sampling procedure was developed for cassava starch analysis.
- Iron and magnesium were determined by fast sequential FAAS.
- The analytical variables were optimized using a Box-Behnken design multivariate.
- The procedure is simple, low-cost, precise, accurate and reliable.

A slurry sampling procedure has been developed for Fe and Mg determination in cassava starch using flame atomic absorption spectrometry. The optimization step was performed using a univariate methodology for 200 mg samples and a multivariate methodology, using the Box-Behnken design, for other variables, such as solvent (HNO3:HCl), final concentration (1.7 mol L−1) and time (26 min). This procedure allowed determination of iron and magnesium with detection limits of 1.01 and 3.36 mg kg−1, respectively. Precision, expressed as relative standard deviation (%RSD), was of 5.8 and 4.1% (n = 10) for Fe (17.8 mg kg−1) and Mg (64.5 mg kg−1), respectively. Accuracy was confirmed by analysis of a standard reference material for wheat flour (NIST 1567a), which had certified concentrations of 14.1 ± 0.5 mg kg−1 for Fe and 40 ± 2.0 mg kg−1 for Mg, and the concentrations found using proposed method were 13.7 ± 0.3 mg kg−1 for Fe and 40.8 ± 1.5 mg kg−1 for Mg. Comparison with concentrations obtained using closed vessel microwave digestion was also realized. The concentrations obtained varied between 7.85 and 17.8 mg kg−1 for Fe and 23.7-64.5 mg kg−1, for Mg. The simplicity, easily, speed and satisfactory analytical characteristics indicate that the proposed analytical procedure is a good alternative for the determination of Fe and Mg in cassava starch samples.