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A flow injection hydride atomic absorption spectrometry (FI-HAAS) method was developed for determining selenium in human milk and whole blood after microwave digestion of the sample. The sample (2 mL human milk or 0.25 mL blood) was introduced into the microwave vessel with 1.5 mL HN03 and 0.25 mL H202 and 300 W (4 min) and 600 W (4 min) were applied. The digestion was completed by heating to 140 C (2-3 h). Se (VI) was reduced to Se (IV) with hydrochloric acid. The instrumental conditions for FI-HAAS (concentrations of reducing agent and carrier acid, flow rate of argon carrier gas, and sample volume injected) were optimized. The detection limit of the proposed method was 0.23 ng/mL (assay) or 115 pg Se (absolute) in biological samples (1.15 ng/mL milk, 10.4 ng/mL blood). The precision values were 5.0% for milk and 4.0% for blood. The accuracy was evaluated with 2 reference materials, National Institute of Standards and Technology Non-Fat Milk Powder (found: 104.3 ± 7.2 ng/g, certified: 110 ± 10 ng/g) and Whole Blood Seronorm (found: 81 ± 7.3 ng/mL, reference: 83 ± 4 ng/mL). The results show the suitability of the method for selenium determination in human milk and whole blood. The method was applied to whole blood samples obtained from pregnant women and to human milk.

Optimization of Selenium Determination in Human Milk and Whole Blood by Flow Injection Hydride Atomic Absorption Spectrometry