Extraction Induced by Emulsion Breaking for Ca, Fe, Mg, and Zn Determination in Edible Oils Using High-Resolution Continuous Source Flame Atomic Absorption Spectrometry

Author(s):  
Uillian Mozart Ferreira da Mata Cerqueira ◽  
Gisseli Souza Valasques ◽  
Cheilane Tavares de Souza ◽  
Sulene Alves Araújo ◽  
Marcos Almeida Bezerra ◽  
...  
Author(s):  
NE Fedorova ◽  
MV Egorova ◽  
AS Rodionov

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.


2014 ◽  
Vol 1010-1012 ◽  
pp. 417-421
Author(s):  
Chao Li ◽  
Shang Long Chen

The aim of this work was to evaluate the microemulsification after incomplete digestion as sample preparation procedure for determination of Ca in leisure foods by high resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Microemulsions were prepared with digestive liquor and n-butyl alcohol as an auxiliary emulsifier after incomplete digestion treatment. The appropriate fuel flow, 70 L/h, and the optimum burner height, 5 mm, were obtained by single factor experimental design. The results showed that the correlation coefficient was better than 0.999, the characteristic concentration was 0.086 mg/L, the precision (RSD) for 6 replicate measurements of Ca was 1.7% and the average of recoveries was 102.1%. F-test and t-test (95% confidence level) in between the proposed method and the comparative method, using microwave digestion-HR-CS FAAS, had no significant difference. Therefore, the proposed method was accurate and stable with a high practical value. It provided scientific basis for determination of metal elements in food.


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