两种尿锑检测方法的比较

Comparison of two methods for detection of antimony in urine

目的建立石墨炉原子吸收光谱法和原子荧光光谱法测定尿中锑,比较两种方法的可靠性和可比性。方法用0.1%曲拉通稀释尿样,以胶体钯为基体改进剂消除干扰,石墨炉原子吸收光谱法直接测定尿中的锑;尿样经混合酸消化后,用原子荧光光谱法测定尿中的锑。结果石墨炉原子吸收光谱法测定尿液中锑,线性范围为0.0~40.0μg/L,相关系数为0.998 3~0.999 2,方法检出限为0.01μg/L,相对标准偏差为1.0%~2.8%,加标回收率为99.1%~101.8%。原子荧光光谱法测定尿中锑,线性范围为0.0~10.0μg/L,线性关系较好,相关系数为0.999 4~0.999 9,最低检出限为0.06μg/L,相对标准偏差为1.9%~2.4%,加标回收率为97.8%~100.9%。现场应用两方法检测109人次尿样,测定均值无明显差异。结论两种方法均适用于职业健康检查和职业性中毒尿中锑的检测。

Objective To compare reliability between graphite furnace atomic absorption and comparability of determination of antimony in urine spectrometry and atomic fluorescence spectrometry. Methods The urine was diluted with 0.1g Triton. The interference was eliminated with colloidal palladium as matrix modifier. Then the antimony in urine was directly determination by the graphite furnace atomic absorption spectrometry. Another method was to digest the urine by mixed acid, then to determine the antimony in urine by atomic fluorescence spectrometry. Results The linearity range of antimony in urine determined by graphite furnace atomic absorption spectrometry was 0.0 ~ 40.0 /zg/L. Its correlation coefficient was 0. 998 3~0. 999 2, the detection limit was 0.01 gg/L, the relative standard deviation was 1.0%~2.8%, and the average recoveries rate was 99.1% ~ 101.8%. The linearity range of antimony in urine determined by atomic fluorescence spectrometry was 0.0 ~ 10.0 μg/L. Its correlation coefficient was 0. 999 4~0. 999 9, the detection limit was 0.06 /xg/L, the relative standard deviation was 1.9% ~2.4%, and the average recovery rate was 97.8%~100.9%. Through field application of these two methods to detect the antimony in urine among 109 person times, no significant difference of the determination means was found between these two methods. Conclusions Both two methods can be used for detection of urine antimony in occupation health examination and occupation poisoning examination.