Food Nuriion Fortifier Selenium Proein HPLC-ICP/MS Detecion Mehod To Establish The Research

With the development of speciation analysis, people gradually realized that the effect of an element is not only related to its content but also depends on its speciation and its migration transformation rule. Selenium is one of essential trace elements for the body, which exists in various forms, such as inorganic selenium(Se(IV)/Se(VI)) and organic selenium. Inorganic selenium is toxic. Organic selenium is good for the body with high bioavailability, found mainly in protein in forms of selenomethionine and etc., involved in the synthesis of the enzyme. Therefore it is necessary to establish a system for methods of selenium determination to set up standards for selenium-rich product markets. The research on the element speciation is of great importance to environmental protection and human health.Samples in this study was a nutrition fortifier--selenium protein, using high performance liquid chromatography with inductively coupled plasma mass spectrometry, to establish a fast, accurate method for determination of selenium selenium speciation analysis. The main characteristics and outcomes of the study are as follows:1. It established HPLC–ICP/MS as the method for determination of selenium in speciation of protein. It showed that Hamiltion X-100 chromatographic column had the best selenium separation effect. The coefficient of selenium calibration curve correlation was R2 > 0.999; detection limits of Se Cys2, Se Cys, Se(IV), Se Met and Se(VI) were 7.18 μg /kg, 5.80 μg /kg, 3.52 μg /kg 11.22, μg /kg, and 6.63 μg /kg.2. It established a suitable extraction method for speciation analysis of selenium protein. Among the acid, water, three enzymatic hydrolysis methods, the enzymatic hydrolysis extraction is of the highest efficiency3. It established the best conditions for instrument analysis. Best instrument parameters for the test: HPLC part(mobile phase tendency for 5 L ammonium citrate, p H 5.5), ICP/MS(mass-to-charge ratio for 78 m/z, ICP RF power is 1400 W, plasma gas flow rate is 18.0 L/min, and atomizer for speed is 0.98 L/min, auxiliary gas flow rate is 1.8 L/min, collision gas flow rate is 60 ml/min)4. Methodological verification. Verification tests were conducted in detection limits, precision and repeatability. Detection limits of five speciations of selenium were 7.18 μg /kg, 5.80 μg /kg, 3.52 μg /kg 11.22, μg /kg, and 6.63 μg /kg, respectively. Sample standard addition repeated six times with parallel sampling, the relative standard deviations were between 0.41%- 0.67% and 1.4%- 3.91% respectively in retention time and peak area of five speciations of selenium; and the peak area of five kinds of speciation of selenium and its concentration showed good linear relationship with the correlation coefficient of correction curves greater than 0.999.