Determination of 5 Selenium Species by Gradient Elution LC-ICP/MS
A gradient elution liquid chromatography coupled with inductively coupled plasma-mass spectrometry(ICP/MS)method was established for determination of SeCys2,MeSeCys,Se(Ⅳ),SeMet and Se(Ⅵ).5 selenium species samples were separated using a Hamilton PRP-X100 anion exchange column,with mobile phase A 40 mmol·L-1(NH4)2HPO4+5 mmol·L-1 C6H8O7·H2O(pH=4.6)and mobile phase B 60 mmol·L-1(NH4)2HPO4+5 mmol·L-1 C6H8O7·H2O(pH=4.6)at flow rate of 1.0 mL·min-1,and the mobile phase switching times were 3.0 min and 6.4 min,respectively,they were determined by ICP/MS and quantified with external standard calibration method.5 selenium species were detected within 8.5 min.In the concentration range of 0.5~200.0 μg·L-1,the correlation coefficients(r)of the 5 selenium species were greater than 0.999.The limits of detection of the method were 0.10~0.39 μg·L-1.Compared with the method in GB/T 5750.6-2023,the analysis time of this method was shortened by 46.8%,and the resolutions and sensitivities of 5 selenium species were better.