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目的:通过对微波消解—塞曼石墨炉原子吸收光谱法测定皮蛋中铅实施分析质量控制和进行分析误差预测,提高实验室铅检测能力和质量控制能力,确保检测数据的准确性和可靠性。方法:按微量元素分析中精密度和准确度的AQC工作程序进行,用塞曼石墨炉原子吸收光谱法GB5009.12-2010对空白溶液(3%硝酸溶液)、2种铅标准溶液(0.1C、0.9C,C为分析方法测定范围的上限,本实验C为100.0μg/kg)、皮蛋、加标质量控制样品(0.5μg/g)进行测定。结果:5种试样的批内、批间变异分析,差异无统计学意义(F0.05),每种试样的总标准差(St)小于其测定浓度的5%,总平均回收率可信限R/d=1.02,质控考核结果为满意。结论:采用精密度—偏性和准确度的工作程序对微波消解—塞曼石墨炉原子吸收光谱法测定皮蛋中铅进行分析质量控制,保证实验结果误差在可控制的范围内,获得高度可信的分析结果。
OBJECTIVE: To improve the quality of lead detection and quality control in laboratory, and to ensure the accuracy and reliability of detection data by analyzing the quality control of Pb in the preserved eggs by microwave digestion - Zeeman graphite furnace atomic absorption spectrometry and analyzing the error prediction. Methods: According to the AQC working program of precision and accuracy of trace element analysis, the effects of the blank solution (3% nitric acid solution), two kinds of lead standard solution (0.1C , 0.9C, C is the upper limit of the analytical method for the determination of the range, the experiment C is 100.0μg / kg), preserved eggs, spiked quality control samples (0.5μg / g) were measured. Results: There were no significant differences among the five samples (P <0.05, P <0.05). The total standard deviation (St) of each sample was less than 5% , The total average recovery rate credible R / d = 1.02, the quality control examination results are satisfactory. Conclusion: The quality control of lead in the preserved eggs by microwave digestion-Zeeman graphite furnace atomic absorption spectrometry was analyzed by using the working procedure of precision-bias and accuracy to ensure that the experimental results were within the controllable range and gained a high level of confidence Analysis of the results.