Speaker
Summary
Introduction
Elemental profiling has been increasingly applied in beef traceability studies. Reliable multielement data are essential to support authenticity and quality assessments. However, beef is a complex organic matrix, rich in proteins and lipids, which directly affects the efficiency of microwave-assisted acid digestion. Proteins enhance heat generation, whereas lipids may adhere to vessel walls, reducing digestion efficiency and homogeneity¹. Therefore, choosing appropriate procedure is essential to ensure complete decomposition for accurate and reproducible multielement determination.
Description of the Work
In this study, five acid digestion procedures were evaluated to optimize parameters such as sample mass, acid concentration, digestion time, and temperature, aiming to maximize the extraction efficiency of chemical elements in beef samples. Nine analytical portions of a beef rump cap sample were subjected to acid digestion using each of the procedures. The resulting solutions were analyzed by triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS/MS) and microwave plasma optical emission spectrometry (MP-AES). Reproducibility was assessed based on the coefficient of variation of the values determined in the analytical portions of the rump cap sample. To verify the accuracy of the results and perform analytical quality control, the certified reference materials SRM 1566b Oyster Tissue, RM 8414 Bovine Muscle Powder, and BCR 668 Mussel Tissue were used. The procedure employing 500 mg of sample and 5 mL of HNO₃ (65% v/v) provided the highest overall accuracy, with satisfactory recoveries for 31 elements. However, the procedure using 250 mg of sample, 4 mL HNO₃ (65% v/v) and 1 mL H₂O₂ (30% v/v) showed similar accuracy (29 elements) while achieving a higher number of elements above the detection limits and improved reproducibility of measured mass fractions in the beef samples. This procedure also produced clear digests, ensuring efficient element extraction and was therefore considered the most suitable for multielement determination in beef samples.
Conclusions
The acid digestion procedure was optimized using the lowest mass and reagent consumption, which generated accurate and reliable results allowing the determination of the elements As, B, Ba, Ca, Ce, Cd, Co, Fe, Gd, K, La, Mg, Mo, Na, Nd, Pb, Pr, Rb, Sb, Sr, Th, U, V, Y, and Zn.
References
¹ SHEEHAN, A.; FUREY A. (2024). Advanced review of the contributing factors for the Microwave Digestion of food matrices for trace elemental analysis. Talanta Open, 9, 100309. DOI: 10.1016/j.talo.2024.100309.
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