甲苯萃取-微波消解-原子荧光光谱法测定富硒保健品中有机硒.docVIP

甲苯萃取-微波消解-原子荧光光谱法测定富硒保健品中有机硒和总硒 李四生1 董晓根2 李家涛1 周勤文1 李建伟1 (1.合肥市疾病预防控制中心,合肥　230022; 2.北京市丰台区疾病预防控制中心,北京　100071) 摘 要 目的:建立分离、消解、测定富硒保健品中有机硒和总硒的分析方法。方法:采用甲苯萃取分离样品中的有机硒后,利用HNO3-H2O2消解体系微波消解,原子荧光光谱法测定样品中的有机硒和总硒。结果:在优化工作条件下,硒的检出限为0.088μg/L,相对标准偏差为0.43% ~0.53%,线性范围为0~200μg/L,应用该方法检测不同富硒保健品中的总硒含量为0.87~13.04 mg/kg,有机硒含量为0.76~8.54 mg/kg,总硒加标回收率为95.1% ~106.2%。结论:该方法简便、灵敏、重现性好、干扰少,适合富硒保健品中的有机硒和总硒测定。 关键词 甲苯萃取;微波消解;原子荧光光谱法;富硒保健品;有机硒;总硒 Determination of organic and total selenium contents in selenium-enriched health food by methylbenzene extraction-microwave-assisted digestion-atomic fluorescence spectrometry LiSi-sheng1, DongXiao-gen2, LiJia-tao1, Zhou Qin-wen1, LiJian-wei1 (1·HefeiCentre for Disease Control and Prevention, Hefei230022,China; 2·FengtaiCentre for Disease Control and Prevention, Beijing 100071, China) Abstract Objective: To develop a method for the separation, digestion and determination of organic and total selenium in selenium-enriched health food· Methods: The organic selenium extracted and separated from selenium-enriched health food was digested by a mixture of concentrated nitric acid and hydrogen peroxide(HNO3-H2O2) in the sealed vessel· Then the organic selenium was subjected to the analysis by atomic fluorescence spectrometry(AFS)·Except the methylbenzene extraction, total selenium was digested and measured as same as organic selenium· Results: Under the optimal work condition, the detection limit of selenium by this method was 0.088μg/L, the linear range 0~200μg//L, the relative standard derivation 0.43% ~0.53%·Thetotal selenium content of 0.87~13.04 mg/kg and the organic selenium contentof0·76~8·54 mg/kg were detected respectively from the selenium enriched health food by this method with the recovery rate of 95.1% ~106.2% for total selenium· Conclusion: This method is proved to be simple, rapid, sensitive accurate and repeatable· So it is suitable to the determination of organic and total selenium in selenium-enriched health food· Key words Methylbenzen