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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 determination of Sb (Ⅲ) and Sb (Ⅴ) in food samples (vegetables, rice, lobster and grass carp) by hydride generation- atomic fluorescence spectrometry. Methods Selective determination of Sb (Ⅲ) in 1.0 mol / L HCl medium was carried out using 3.5 mol / L HCl as extraction solvent and ultrasonic extraction with 10 g / L sodium fluoride as masking agent for Sb (V) Subtraction method was determined Sb (Ⅴ) content. Results The detection limits of Sb (Ⅲ) and Sb (Ⅲ + Ⅴ) were 0.15 μg / L and 0.07 μg / L, respectively. The relative standard deviations (RSDs) were 3.5% and 7.4%, respectively. The Sb (Ⅲ) and Sb (Ⅴ) in food samples were analyzed by this method and compared with the microwave digestion method, the total antimony extraction rate was over 80% + Ⅴ) recoveries were 81.4% ~ 91.4% and 89.6% ~ 101.8%, respectively. Conclusion The method has the advantages of simple operation, low detection limit, good linearity and high recovery rate. It is suitable for valence analysis of antimony in food.