正交试验设计优化微波消解法测定血中铅  

Determination of lead in blood with orthogonal test design optimized microwave digestion method

作　　者：陈宇鸿[1] 

机构地区：[1]温岭市疾病预防控制中心,浙江温岭317500

出　　处：《中国卫生检验杂志》2018年第2期149-151,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的研究微波消解条件在血铅前处理中的应用,探索出适用于微波消解消化血中铅的条件。方法以微波消解剂比例(硝酸/过氧化氢)、温度、压力、以及保持时间为4个研究因素,回收率作为评价指标,微波消解消化血样,L9(34)的正交设计优化微波消解血中铅的最佳参数,并对该方法的精密度与回收率及标准物质进行测定验证。结果血铅微波消解效率的影响因素依次为温度、压力、保持时间、微波消化液比例(硝酸:过氧化氢)。最佳微波消解条件:微波消化液比例(硝酸:过氧化氢)为5∶1,温度为180℃,压力为2 533 k Pa,保持时间为5 min。此条件下,采用石墨炉原子吸收光谱法测得血铅的RSD值为1.64%~2.12%,回收率为96.7%~98.8%。结论此方法消化耗时短且彻底,不易污染及损失,适宜于处理批量血样,并且能有效提高分析的准确度。Objective To study the application of microwave digestion conditions in the pretreatment of blood lead,and to explore the optimal conditions for the digestion of lead in digestion. Methods Microwave digestion ratio（ nitrate/hydrochloric acid）,power,climbing time and holding time were selected as the four factors for study,the recovery rate was chosen as the evaluation index,microwave was used for sample digestion,L9（ 34） orthogonal design was adopted for the optimizing the best parameters of lead in blood by microwave digestion,and the precision and recovery of the method and standard material were measured and verified. Results The influence factors of the microwave digestion efficiency of blood lead were temperature,pressure,time and proportion of microwave digestion（ nitric acid： hydrogen peroxide）. The best condition of microwave digestion included that microwave digestion liquid ratio（ nitric acid,hydrogen peroxide） was 5 ∶1,the temperature was 180 ℃,presure was 2 533 kpa,holding time was 5 min. In this condition,the RSD value of blood lead with graphite furnace atomic absorption spectrometry was within 1. 64%-2. 12%,and the recovery rate was within 96. 7%-98. 8%. Conclusion This method is short and thorough,not easy to contaminate and loss,suitable for mass blood samples,and can effectively improve the accuracy of analysis.

关 键 词：正交试验 优化 微波消解 血样 铅 

分 类 号：O657.31[理学—分析化学]