Method for determining content of total selenium, inorganic selenium and organic selenium of selenium yeast
A determination method and yeast selenium technology, applied in material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of cumbersome and time-consuming, and achieve the effects of avoiding pollution, reducing interference and high recovery rate.
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Embodiment 1
[0025] Embodiment 1 The drawing of standard curve
[0026] Pretreatment of selenium powder: Accurately weigh 100.0 mg of elemental selenium, dissolve in 1 mL of concentrated nitric acid (69%), add 2 mL of perchloric acid (70%~72%), heat in a boiling water bath for 4 h; after cooling Add 8.4 mL of HCL (the concentration of hydrochloric acid is 0.1 mol / L), and then put it in a boiling water bath for 10 min. Accurately dilute to 1000 mL, this is the stock solution (Se content: 100 μg / mL). When in use, dilute the stock solution to 50 mL with 10 mL of 0.1 mol / L hydrochloric acid to obtain a standard working solution containing 0.2 μg selenium per mL.
[0027] Drawing of standard curve: Accurately measure 0.00, 0.20, 0.60, 1.00, 3.00, 12.00, 14.00 and 20.00mL selenium standard working solution respectively. Equivalent to 0.00 μg, 0.04 μg, 0.12 μg, 0.20 μg, 0.60 μg, 2.40 μg, 2.80 μg and 4.0 μg of selenium, dilute to 40 mL with water, adjust the pH to 1.5~2.0 with ammonia sol...
Embodiment 2
[0028] Example 2 Determination of Yeast Selenium Total Selenium Content
[0029] Accurately weigh about 50 mg of yeast selenium into a 100 mL stoppered round bottom flask, add 1 mL of concentrated nitric acid, then add 2 mL of perchloric acid (70%~72%), and then place it in a boiling water bath for magnetic stirring 1h; after cooling, add 8.4 mL HCL (hydrochloric acid concentration: 6 mol / L), and then put it in a boiling water bath for 10 min. Transfer the above solution to a volumetric flask without damage, and dilute to 100 mL with pure water, take out 2.0 mL and add it to the Erlenmeyer flask, then add 30-40 mL of water, adjust the pH to 1.5 with ammonia solution and 3 mol / L hydrochloric acid ~2.0, then add 3 mL EDTA mixture and shake well, then add 3 mL DAN solution, shake well, and keep in boiling water for 5 min. Take it out and cool it to room temperature, transfer it all to a 125 mL separatory funnel, add 10 mL cyclohexane to shake for 2.0 min, let it stand for stra...
Embodiment 3
[0030] Embodiment 3 Determination of Yeast Selenium Inorganic Selenium Content
[0031] Accurately weigh about 25 mg of yeast selenium into a 100 mL round-bottomed flask, add 10 mL of 6 mol / L hydrochloric acid solution, place in a boiling water bath, stir magnetically for 10 min, and adjust with ammonia solution and 3 mol / L hydrochloric acid after cooling. pH to 1.5~2.0, then add 3 mL EDTA mixture and shake well, then add 3 mL DAN solution, shake well, keep in boiling water for 5 min. Take it out and cool it to room temperature, transfer it all to a 125 mL separatory funnel, add 10 mL cyclohexane to shake for 2.0 min, and after standing to separate layers, measure the concentration of the cyclohexane layer with an excitation light wavelength of 376 nm and an emission light wavelength of 520 nm. The fluorescence intensity.
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