摘要
目的:建立快速准确的湿法消解-原子荧光光谱法用于人血清和人尿中硒的测定。方法:采用硝酸、高氯酸对尿样及血清进行湿法消解,利用原子荧光光谱法测定其中的硒含量。结果:对尿样及血清分别进行最佳消解条件的摸索,同时优化检测条件。得出最佳条件如下:尿样/硝酸体积比为1∶1;血清/硝酸高氯酸混酸体积比为1∶5;还原剂硼氢化钾(KBH4)浓度为2%;灯电流,70 mA;载气流量,400 ml/min;酸性介质,10%盐酸,硒在浓度范围1.0μg/L~40.0μg/L内线性关系良好,线性相关系数为1.0000,检出限为0.095μg/L,尿液加标回收率在100.0%~117.7%之间,血清加标回收率在97.4%~102.5%,四次平行测定相对标准偏差小于4.0%。结论:该方法简便快速、准确灵敏,适用于血清及尿中硒的测定。
Objective:To establish a rapid and precise method for the determination of selenium in human serum and urine by wet digestion coupling with atomic fluorescence spectrometer approach. Methods : After a pretreatment with nitric acid or perchlotic acid wet digestion, we used atomic fluorescence spectrometer methodology to detect selenium in human serum and urine. Re- sults: Under the optimized digestion and detection conditions : urine/HNOa ratio 1 : 1 and serum/HNO3 - HClO4 ratio 1 : 5, respectively; KBH4 concentraton, 2% (w/w) ; lamp current, 70 mA; flow rate of carrying gas, 400 ml/min; reaction medium, 10% HCl, wide linear relationship was achieved in the range of 1.0 μg/L - 40.0 μg/L with relative coefficient of 1. 0000 and the detection limit was estimated to be 0. 095 μg/L. We got satisfied recovery rates of spiked urine samples of 100.0% to 117.7% and spiked serum samples of 97.4% - 102.5% , respectively with RSDs of four replicate experiments less than 4.0%. Conclusion : The present method is precise, rapid and sensitive enough for the determination of selenium in human serum and urine.
出处
《中国卫生检验杂志》
CAS
2010年第11期2750-2752,共3页
Chinese Journal of Health Laboratory Technology
关键词
湿法消解
原子荧光
硒
血清
人尿
Wet digestion
Atomic fluorescence spectrometer
Selenium
Human serum
Urine