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.

Active Publication Date: 2015-09-23
ZHEJIANG UNIV
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The above extraction methods ar

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  • Method for determining content of total selenium, inorganic selenium and organic selenium of selenium yeast

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Experimental program
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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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Abstract

The invention discloses a method for determining content of total selenium, inorganic selenium and organic selenium of selenium yeast. The method comprises the steps: heating and digesting a sample in hydrochloric acid to uniformly reduce selenium in the sample to be quadrivalence selenium, generating a piaselenole complex by virtue of the quadrivalence selenium and 2,3-diaminonaphthalene (DAN) under the subacidity condition, and extracting by utilizing cyclohexane; determining fluorescent intensity by utilizing a fluorophotometer, and calculating the content of selenium in the sample. 3mL of mixed acid is used for determining the total selenium, so that the consumption of the mixed acid can be greatly reduced; the digestion and extraction are carried out in a water bath in a round-bottomed flask with a cover, so that the pollution of strong oxidation reductive acid on the environment of a laboratory can be avoided, the volatile loss of selenium can be prevented, and the recovery rate is relatively high; the consumption of a cresol red indicator agent is canceled, so that the interference of the sample on the judgment of the color variation of the indicator agent can be avoided, and the interference of the indicator agent on a to-be-detected solution can be reduced. The determination time of the total selenium and inorganic selenium is greatly shortened, and the digestion of total selenium and extraction of inorganic selenium can be completed in about one hour.

Description

technical field [0001] The invention relates to a method for determining the content of selenium in yeast selenium, especially the content of organic selenium. Background technique [0002] In 1974, the US Food and Drug Administration (FDA) began to allow selenium to be added to livestock, poultry and pig feed. So far, the research and application of inorganic selenium and organic selenium have entered a wider field (Ullrey, 1992). One of the most economical sources of organic Se is the enrichment of inorganic Se by yeast (Neve, 1998). Yeast can absorb carbon, nitrogen, phosphorus, sulfur and minerals as well as trace elements, because selenium and sulfur are congener elements with similar physical and chemical properties, making them replace sulfur in yeast cell biosynthesis reactions (Jian Zheng, 2003), selenium-enriched yeast is a microbial fermentation product produced by adding inorganic selenium such as sodium selenite during yeast culture to convert it into organic ...

Claims

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Application Information

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IPC IPC(8): G01N21/64
Inventor 王凤芹张煜席玲玲汪以真
Owner ZHEJIANG UNIV
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