氢化物发生-原子荧光光谱法测定食品样品中的锑(Ⅲ)和锑(Ⅴ)

Determination of stibium(Ⅲ) and stibium(Ⅴ) in food samples by hydride generation-atomic fluorescence spectrometry

目的建立氢化物发生-原子荧光光谱法测定食品样品（蔬菜、大米、龙虾、草鱼）中Sb（Ⅲ）和Sb（Ⅴ）的分析方法。方法选取3.5 mol/L HCl为提取剂,超声提取,以10 g/L氟化钠作为Sb（Ⅴ）的掩蔽剂,在1.0 mol/L HCl介质中选择性的测定Sb（Ⅲ）含量,用差减法求得Sb（Ⅴ）含量。结果 Sb（Ⅲ）和Sb（Ⅲ＋Ⅴ）的检出限分别为0.15μg/L和0.07μg/L,相对标准偏差（RSD）分别为3.5%和7.4%（n=11）。应用此法对食品样品中的Sb（Ⅲ）和Sb（Ⅴ）进行分析,并与微波消解法测定值相比较,该法总锑的提取率为80%以上,Sb（Ⅲ）和Sb（Ⅲ＋Ⅴ）的加标回收率分别为81.4%~91.4%和89.6%~101.8%。结论该法具有操作简单、检出限低、线性关系好、回收率高等特点,适用于食品中锑的价态分析。

Objective To establish a method for the analysis of Sb（ Ⅲ） and Sb（ Ⅴ） in food samples such as vegetable,rice,crayfish and grass carp by hydride generation-atomic fluorescence spectrometry（ HG-AFS）. Methods Using 3. 5 mol / L HCl as extractant,taking 10 g / L sodium-fluoride for a masking agent. After the Sb（ Ⅲ） was determined in the medium of1. 0 mol / L HCl,the concentration of Sb（ Ⅴ） was calculated by the difference. Results The determination limits of Sb（ Ⅲ）and Sb（ Ⅲ ＋ Ⅴ） were 0. 15 μg / L and 0. 07 μg / L,respectively; this method was applied for the analyzed of Sb（ Ⅲ） and Sb（ Ⅴ） in food samples,and compared with the microwave digestion method,and the relative standard deviations（ RSDs） were3. 5% and 7. 4%（ n = 11）; the extraction rate of total Stibium was more than 80%,and recoveries of the Sb（ Ⅲ） and Sb（ Ⅲ ＋Ⅴ） were 81. 4%-91. 4% and 89. 6%-101. 8%. Conclusion With easy operation,low detection limit,good analytic accuracy and high recovery rate,this method is suitable for valence state analysis of Sb in the food samples.