双道原子荧光光谱法同时测定螺旋藻粉中硒和碲
Simultaneous Determination of Selenium and Tellurium in Spirulina Powder by Double Channel Atomic Fluorescence Spectrometry
-
摘要:
目的 建立湿法消化-氢化物双道原子荧光光谱法同时测定螺旋藻粉中硒(Se)和碲(Te)的新方法。 方法 用硝酸、高氯酸分解样品,消化完全后在室温条件下加入浓盐酸将Se6+/Te6+还原成Se4+/Te4+,与硼氢化钾反应,采用标准曲线法测定硒和碲。 结果 测定结果表明,硒的线性范围为2.70~20.00 μg/L,相关系数(r)=0.999 7,最低检出限(DL)=0.77μg/L,回收率为93.5%~102.9%,精密度(相对标准偏差)为1.22~4.44;碲的线性范围为0.16~2.00μg/L,r=0.999 8,DL=0.042 μg/L,回收率为100.0%~101.2%,精密度为1.45~5.70。双元素同时测定法与单元素测定法差异无统计学意义。 结论 用湿法消化和氢化物发生-双道原子荧光光谱法可以同时测定螺旋藻粉中的硒和碲,方法简单快捷,结果准确,能满足测定要求。 Abstract:Objective To establish a new method for simultaneous determination of selenium (Se) and tellurium (Te) in wet-digestion prepared spirulina powder by hydride generation-double channel atomic fluorescence spectrometry. Methods After digestion with HNO3-HClO4, HCl solution was added for the reduction of Se6+/Te6+ into Se4+/Te4+, which acted with KBH4 solution. The concentrations of Se and Te were estimated by standard curve method. Results The calibration curve of Se was linear within the range of 2.70~20.00 μg/L with a correlation coefficient (r) of 0.999 7, and that of Te was within the range of 0.16-2.00 μg/L with r=0.999 8. The detection limits were 0.77 μg/L for Se and 0.042 μg/L for Te. The recovery rates of spiking standards for Se and Te were in the ranges of 93.5%-102.9% and 100.0%-101.2%, respectively. The relative standard deviations (RSDs) were 1.22%-4.44% for Se and 1.45%-5.70% for Te. No significant difference was found between the results of simultaneous determination and single (Se or Te) determinations. Conclusion The method for simultaneous determination of Se and Te in wet-digestion prepared spirulina powder by hydride generation-double channel atomic fluorescence spectrometry is simple, rapid, and the results are accurate.
下载:
