Determination of Five Selenium Speciations in Eggs by HPLC-ICP/MS
In order to accurately determine the content of selenocysteine(SeCys2),methylselenocysteine(MeSeCys),selenomethionine(SeMet),selenate(Ⅵ)and selenite(Ⅳ)in eggs,a rapid method using high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP/MS)was developed.Selenium was extracted from the egg samples by enzymolysis of protease XIV and iodoacetamide solution.It was shaken in a Tris-HCl solution at 50℃water bathing for 4 h,centrifuged at 4℃with 10 000 r/min for 10 min,and the supernatant was filtered by 0.22 μm filter membrane and quantified by matrix matching external standard method.The results showed that the five selenium speciations in eggs raned from 0.1 to 1 000.0 μg/L,the linear correlation of the established method has good correlation,and the correlation coefficient(R2)was≥0.999;The detection limit of selenium in eggs was from 0.23 to 0.95 μg/kg,and the limits of quantification was from 0.80 to 3.00 μg/kg.The recoveries of 4 of 5 selenium speciations were in the range of 76.7%to 103.1%at low,medium and high addition levels,and the coefficient of variation within and between batches was less than 10%.The results indicated that the established HPLC-ICP/MS method had high sensitivity and good precision,and could provide a method for the determination of 5 kinds of selenium speciations in eggs.
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