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目的建立尿镉的高分辨率连续光源石墨炉原子吸收光谱测定方法。方法尿样采集后立即按照1%的比例加入优级纯浓硝酸,混匀后的尿样用1%硝酸-0.1%曲拉通X-100稀释液稀释,以0.1%硝酸钯溶液为基体改进剂,通过优化石墨炉灰化和原子化温度程序后,用石墨炉原子吸收分光光度法测定。结果该方法标准曲线在0.2 ng/ml~2.0 ng/ml时有良好的线性关系(r>0.998);检出限为1.3×10-12g(k=3),相对标准偏差<5%,回收率为94%~108%。测定高盐含量尿样时干扰少。结论本方法具有快速、简单、准确的特点,尿样须稀释10倍后测定是取得准确结果的关键;该方法可以用于实验室开展常规职业健康体检中尿镉的测定。
Objective To establish a method for the determination of urinary cadmium by high-resolution continuous light source graphite furnace atomic absorption spectrometry. Methods After the urine sample was collected, 1% pure nitric acid was added immediately. The mixed urine samples were diluted with 1% nitric acid-0.1% Triton X-100, and 0.1% palladium nitrate solution was used as the matrix After optimization of graphite furnace ashing and atomization temperature program, it was determined by graphite furnace atomic absorption spectrophotometry. Results The calibration curve showed good linearity (r> 0.998) at 0.2 ng / ml to 2.0 ng / ml. The detection limit was 1.3 × 10-12 g (k = 3) with relative standard deviation <5% The rate is 94% ~ 108%. Determination of high salt content of urine samples less interference. Conclusion The method is rapid, simple and accurate. The determination of urine samples after 10-fold dilution is the key to obtain accurate results. This method can be used for the determination of urinary cadmium in routine occupational health examination in the laboratory.