Modern Methodological Approaches to Sample Preparation for the Determination of Trace Elements in Food Products and Plant Raw Materials

Introduction. Various copper compounds are most widely used as plant protection agents in agriculture. From a hygienic point of view, information on excessive accumulation of copper in plants related to the use of a specific formulation of copper- containing pesticides is of interest.

Our objective was to assess feasibility of increasing statistical significance of results of determining low residue levels of a copper-containing pesticide in apple samples by flame atomic absorption spectrometry using a high-resolution spectrometer in combination with developed approaches to sample preparation of plant-based foods, including homogenization with dry ice and microwave mineralization.

Materials and methods: We analyzed 30 samples of apples collected in three different agro-climatic zones by flame atomic absorption spectrometry and electrothermal atomization atomic absorption spectrometry. Both methods were validated on 10 samples with added copper at levels 1-5 of the lower limit of quantitation. A statistical calculation was performed based on a simple Student’s test to assess the significance of differences between the results of measurements by flame and electrothermal techniques. Homogeneity of variances was estimated using the Fisher test to clarify the possibility of comparing two data sets.

Results: The use of a technique of cryo-grinding and microwave decomposition in a microwave reactor in combination with a high-resolution continuum source atomic absorption spectrometry demonstrated a decrease in scattering and the limit of detection and better repeatability in the analysis of parallel samples. Results of statistical calculations confirmed the homogeneity of variances in data samples obtained for electrothermal and flame techniques, and the further Student’s t-test showed insignificant differences between the results of measurements obtained by FAAS and ET-AAS.

Conclusion: Our findings prove that modern methods of sample preparation in combination with highly sensitive equipment allow a significant reduction in the limit of detection and scattering of test results.

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