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目的优化尿碘检测实验条件,建立过硫酸铵消化——砷铈催化分光光度法测定人体尿样中碘含量的方法。方法取人体尿样0.25μl经1.0 mol/L过硫酸铵溶液在100℃条件下消化,利用碘对砷铈氧化还原反应的催化作用,控制反应温度和时间,测定求出碘含量,并与其他常规检测方法进行测定结果的灵敏度、精密度及准确度比较。结果在所选择的实验条件下,本方法测定最低检出浓度为3μg/L,与其他常规检测法无显著性差异,尿碘浓度在0μg/L~300μg/L范围内线性关系良好,相关系数r可达0.9998,相对标准偏差1.07%~1.86%,加标回收率91%~103%,且本方法在22.3℃~35℃之间稳定性极好。结论所建立的方法测定人体尿样中碘元素含量,方法灵敏、准确度高、精密度好,实验参数经过优化后,大大减少有毒有害试剂使用量,降低环境污染,适用于大批量实际样品的检测需求。
Objective To optimize the experimental conditions of urinary iodine detection and to establish a method of ammonium persulfate digestion - arsenic and cerium catalytic spectrophotometry for the determination of iodine in human urine samples. Methods Human urine samples were digested with 1.0 mol / L ammonium persulfate solution at 100 ℃, catalytic effect of iodine on redox reaction of arsenic and cerium, control of reaction temperature and time, determination of iodine content, and other Routine detection methods for the determination of the sensitivity, precision and accuracy of the comparison. Results Under the selected experimental conditions, the method of determination of the lowest detection concentration of 3μg / L, and other routine testing no significant difference in urinary iodine concentration in the range of 0μg / L ~ 300μg / L within a good linear relationship, the correlation coefficient r up to 0.9998, the relative standard deviation of 1.07% ~ 1.86%, the recovery of 91% ~ 103%, and the method is excellent in stability between 22.3 ℃ ~ 35 ℃. Conclusion The established method for the determination of iodine in human urine samples is sensitive, accurate and precise, and the experimental parameters are optimized to greatly reduce the amount of toxic and harmful reagents and reduce environmental pollution, suitable for large quantities of actual samples Testing needs.