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目的建立电感耦合等离子体-质谱(ICP-MS)法直接测定镉中毒患者尿中镉以及钙、镁、锌、铁、铜和硒的分析方法。方法采用体积分数为0.1%的硝酸溶液对尿液稀释20倍后直接用ICP-MS法进行分析。采用整群抽样的方法,以200例职业性慢性镉中毒患者为观察组,以无接触职业病危害因素且职业健康检查未见异常的200名人员作为对照组,采集尿样对本方法进行验证。结果本方法测定尿中镉、钙、镁、锌、铁、铜和硒的方法检出限分别为0.28、250.00、110.00、4.22、9.17、2.24和2.36μg/L;平均加标回收率为96.3%~101.8%;批内精密度为0.4%~2.0%,批间精密度为1.1%~3.2%。观察组人群尿中镉、钙、锌、铁、铜和硒水平均高于对照组(P<0.01)。结论本方法简单快速、精密度好、准确性高、操作方便,检出限可以满足测定要求,可用于尿中镉、钙、镁、锌、铁、铜和硒的测定。
Objective To establish a method for the direct determination of urinary cadmium, calcium, magnesium, zinc, iron, copper and selenium in patients with cadmium poisoning by inductively coupled plasma mass spectrometry (ICP-MS). Methods The urine samples were diluted 20 times with 0.1% nitric acid solution and directly analyzed by ICP-MS. Using the method of cluster sampling, 200 patients with occupational chronic cadmium poisoning were taken as the observation group. 200 non-contact occupational hazards and no abnormal occupational health examination were taken as the control group. Urine samples were collected to verify the method. Results The detection limits of this method for the determination of cadmium, calcium, magnesium, zinc, iron, copper and selenium in urine were 0.28, 250.00, 110.00, 4.22, 9.17, 2.24 and 2.36 μg / L, respectively. The average recoveries were 96.3 % ~ 101.8%; Intra-assay precision was 0.4% ~ 2.0%, inter-batch precision was 1.1% ~ 3.2%. Urinary cadmium, calcium, zinc, iron, copper and selenium levels in observation group were higher than those in control group (P <0.01). Conclusion The method is simple and rapid, accurate, accurate, easy to operate, the detection limit can meet the determination requirements, can be used for determination of urinary cadmium, calcium, magnesium, zinc, iron, copper and selenium.