尿砷测定试管快速消解氢化物原子荧光法的建立及评价

Establishment and evaluation of a method for determination of total arsenic in urine by test-tube rapid digestion hydride generation atomic fluorescence spectrometry

目的建立尿砷测定的试管快速消解氢化物原子荧光法，并分析该方法的质量控制措施。方法尿样经刻度试管和石墨消解仪快速消解后，用原子荧光仪测定砷含量，采用精密度与准确度实验，实验室之间比对和复核实验等质量控制措施对其检测结果进行评价。结果尿砷含量在0～0．300mg／L线性范围内时．相关系数（r）〉0．9993，方法检出限为0．00021mg／L，相对标准偏差（RSD）≤4．62％，加标回收率为93．9％～104-3％，标准物质测定值均在不确定度范围内，国家尿砷盲样考核合格。结论本方法为微量取样，且快速检测、基体干扰少、实用性强，实验结果误差在可控制的范围内。

Objective To establish and evaluate a method for determination of total arsenic in urine by test-tube rapid digestion hydride generation atomic fluorescence spectrometry. Methods After digestion of urine samples using graduated test-tube and graphite digestion apparatus, arsenic content in urine was determined with atomic fluorescence spectrometer. Then the test results were evaluated by using quality control measures, such as precision and accuracy experiments, and the results between different laboratories were reviewed and compared. Results The urinary arsenic was in a linear range of 0 - 0.300 mg/L, correlation coefficient （r） 〉 0.999 3, detection limit was 0.000 21 rag/L, relative standard deviation （RSD） ≤4.62% and the recoveries of standard addition were 93.9% - 104.3%. The value of standard reference material measured was within the allowable range. The blind sample of the national urinary arsenic was qualified. Conclusions This method is suitable for large scale determination of urinary arsenic for its micro sample amount needed, less interference and strong practicability. The error results are in a controlled range.