The development and validation of a new method for the fast determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn in rice by inductively coupled plasma optical emission spectrometry

Abstract

An alternative method of rice sample preparation for measuring the total content of selected elements, i.e., Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn, by ICP OES was developed. The proposed approach is based on the ultrasound-assisted extraction (USAE) of rice samples in the presence of a small amount of concentrated HNO₃. The optimal operating parameters were found using the design of experiments (DOE) approach, and the studied experimental factors were the temperature of the ultrasonic bath (A), the sonication time (B), and the volume of concentrated HNO₃ added per 0.5 g of a rice sample (C). Under the optimal conditions of the USAE procedure, i.e., A = 60 °C, B = 16 min and C = 4.0 mL, the rice samples were readily solubilized, and the obtained sample solutions could be analyzed by ICP OES with the simple standard solution calibration (without matrix matching). The analysis of the certified reference material (rice flour, NIST SRM 1568b) confirmed the satisfactory trueness of the USAE-ICP OES method. Additionally, no statistically significant differences between the results obtained for the samples prepared by USAE and open-vessel wet digestion (WD, the reference method) were found. In comparison to the routinely used microwave-assisted digestion and open-vessel digestion, the USAE approach offers lower acid consumption, lower detection limits (LODs) of elements, ranging from 4.0 ng g⁻¹ for Mn to 2.7 µg g⁻¹ for K, and a much shorter time of sample preparation.