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建立了一种利用阴离子交换高效液相色谱与氢化物发生原子荧光光谱联用同时测定四、六价硒及硒代半胱氨酸(SeCys)形态的方法。优化了六价硒的还原条件及仪器检测参数,以不同浓度的柠檬酸铵作为流动相,在10 min内同时分离了四、六价硒及硒代半胱氨酸(SeCys)。采用加标法定量,加标回收率在90%～119%之间,相对标准偏差为1.6%～3.1%(100μg/L),四、六价硒及硒代半胱氨酸(SeCys)的检出限分别为0.32μg/L、0.47μg/L和0.44μg/L(进样量为100μL)。应用该法对长期汞暴露人群补硒后尿中的小分子硒的形态进行了分析,仅检测到硒代半胱氨酸(SeCys)。
A method for the simultaneous determination of tetravalent and selenium-substituted cysteine (SeCys) by anion-exchange high-performance liquid chromatography with hydride generation atomic fluorescence spectrometry was established. The conditions for the reduction of hexavalent selenium and the parameters of the instrument were optimized. SeCys was separated from the selenium and selenocysteine in 10 min with different concentrations of ammonium citrate as the mobile phase. The recoveries were in the range of 90% -119% with the relative standard deviations (RSDs) of 1.6% -3.1% (100μg / L), the contents of selenium, selenium and selenocysteine The detection limits were 0.32μg / L, 0.47μg / L and 0.44μg / L respectively (injection volume was 100μL). This method was used to analyze the form of small molecule selenium in urine after long-term mercury exposure, and only selenocysteine (SeCys) was detected.