高效液相色谱-原子荧光光谱法分析鱼肌中的总硒和形态硒

Analysis of total selenium and form selenium in fish muscle by high performance liquid chromatography-atomic fluorescence spectrometry

硒是人体必需的15种营养素之一,人体内不同形态硒的生物活性存在明显差异,鱼类是含硒量较高的动物,是人体摄入硒的重要来源,因此准确测试鱼肌中总硒和形态硒含量具有重要的意义。将鱼肌样品消解,采用原子荧光光谱法对消解液进行分析,总硒浓度在0~10μg/L内线性关系良好,标准曲线相关系数大于0.999,检出限为0.09μg/L,相对标准偏差(RSD)为0.77%,加标回收率为104.2%,表明方法准确度较好。优化高效液相色谱-原子荧光光谱法的测试参数分析形态硒,其测试结果为硒代胱氨酸、亚硒酸盐、硒代蛋氨酸、硒酸盐等4种形态硒的标准曲线在10~200μg/L浓度范围内线性关系良好,相关系数均大于0.999,检出限在2.87~4.47μg/L之间,相对标准偏差(RSD)在1.14%~2.13%之间,各形态消解前加标的加标回收率在91.6%~108.9%之间,消解后加标的加标回收率在90.1%~109.7%之间,结果表明该方法对鱼肌形态硒测定有很好的准确性和可靠性。

Selenium is one of the fifteen essential nutrients for human body.The biological activity of different forms of selenium in human body is obviously different.Fish has high selenium content and is an important source of selenium intake for human body.Therefore,it is of great significance to accurately measure the content of total and form selenium in fish muscle.Fish muscle samples are digested and analyzed by atomic fluorescence spectrometry.The linear relationship of total selenium concentration within 0-10μg/L is good,the correlation coefficient of the standard curve is greater than 0.999,and the detection limit is 0.09μg/L,the relative standard deviation(RSD)is 0.77%,and the recovery is 104.2%,indicating that the method is accurate.Optimizing the parameters of High-performance liquid chromatography Atomic fluorescence spectroscopy for speciation analysis,the four forms of Secys,Se(IV),SeMet and Se(VI)have a good linear relationship within 10-200μg/L.The linear correlation coefficient of the standard curve is greater than 0.999.The detection limit is 2.87-4.47μg/L,the relative standard deviation(RSD)is 1.14%-2.13%.The recovery rates of various of form selenium before digestion range from 91.6%to 108.9%,while the recovery rates after digestion range from 90.1%to 109.7%.The results show that the method is accurate and reliable for the determination of form selenium in fish muscle.