Campillo N, Viñas P, López-García I, Hernández-Córdoba M
Department of Analytical Chemistry, University of Murcia, Murcia, E-30071, Spain.
Anal Biochem. 2000 May 1;280(2):195-200. doi: 10.1006/abio.2000.4516.
Procedures for the direct determination of total selenium in urine, serum, and blood using electrothermal atomic absorption spectrometry are presented. In the selected experimental conditions, Zeeman correction is mandatory to compensate for the high background signals. The sample diluted and containing 0.1% (w/v) Triton X-100 is introduced directly into the electrothermal atomizer. A solution containing 15% (w/v) hydrogen peroxide, 0.65% (w/v) nitric acid, and 0.5% (w/v) nickel is injected separately into the atomizer. Calibration is carried out using the standard additions method. The detection limit is 30 pg selenium. If palladium, instead of nickel, is used as the chemical modifier, calibration can be carried out against aqueous standards, and the detection limit is 45 pg. In this case, three separate injections are required to prevent precipitation problems in the automatic injector. The reliability of the procedures is checked by analyzing three certified reference materials and by recovery studies. Mean recoveries are 99.7% for serum, 99.4% for urine, and 100.8% for blood samples. Relative standard deviation values are +/-4.0% for serum, +/-3.9% for urine, and +/-4.5% for blood.
介绍了用电热原子吸收光谱法直接测定尿液、血清和血液中总硒的方法。在选定的实验条件下,必须采用塞曼校正来补偿高背景信号。将稀释且含有0.1%(w/v) Triton X - 100的样品直接引入电热原子化器。分别将含有15%(w/v)过氧化氢、0.65%(w/v)硝酸和0.5%(w/v)镍的溶液注入原子化器。采用标准加入法进行校准。检测限为30 pg硒。如果使用钯代替镍作为化学改进剂,则可根据水溶液标准进行校准,检测限为45 pg。在这种情况下,需要进行三次单独进样以防止自动进样器出现沉淀问题。通过分析三种有证标准物质和进行回收率研究来检验该方法的可靠性。血清的平均回收率为99.7%,尿液为99.4%,血液样品为100.8%。血清的相对标准偏差值为±4.0%,尿液为±3.9%,血液为±4.5%。