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    微波消解-电感耦合等离子体原子发射光谱法测定木耳中铝的含量

    Determination of Aluminum in Fungus by Inductively Coupled Plasma Atomic Emission Spectrometry with Microwave Digestion

    • 摘要: 摄入过多铝元素可能带来一定健康风险,而相关标准及文献中均缺乏木耳中铝含量的测定方法,故提出了题示方法,并对消解体系中氢氟酸的影响进行了讨论。取0.250 0 g烘干后的木耳样品于消解管中,加入5 mL硝酸、1 mL 30%(质量分数)过氧化氢溶液和0.5 mL氢氟酸,加盖后放置过夜,并于次日按照微波消解程序进行消解。赶酸、洗涤、用2%(体积分数)硝酸溶液定容,用电感耦合等离子体原子发射光谱法在396.152 nm检测波长下测定样品溶液中铝含量。结果显示,不加氢氟酸时铝的测定值显著低于认定值,而添加氢氟酸后的测定值均在认定值的不确定度范围内,铝的质量浓度在10.0 mg·L-1内与其对应的发射强度呈线性关系,检出限为5.9 μg·L-1;对生物成分分析标准物质进行精密度和加标回收试验,所得测定值的相对标准偏差(n=6)为4.0%~8.5%,回收率为89.0%~97.3%。方法用于10个木耳样品的分析,所得测定值为203~305 mg·kg-1

       

      Abstract: Excessive intake of aluminum may bring certain health risks, and the relevant standards and references lack the determination method of aluminum in fungus, so the title method was proposed, and the effect of hydrofluoric acid in the digestion system was discussed. 0.250 0 g of dried fungus sample was taken into digestion tube, 5 mL of nitric acid, 1 mL of 30% (mass fraction) hydrogen peroxide solution and 0.5 mL of hydrofluoric acid were added. The mixture was placed overnight after closing the lid, and digested according to the microwave digestion procedure on the next day. After removing the acid, washing, and making up the volume with 2% (volume fraction) nitric acid solution, the aluminum in the sample solution was determined by inductively coupled plasma atomic emission spectrometry at the detection wavelength of 396.152 nm. It was shown that the determined values without adding of hydrofluoric acid were significantly lower than the certified values, while the determined values after adding hydrofluoric acid were within the uncertainty range of the certified values. Linear relationship between values of the mass concentration of aluminum and its corresponding emission intensity was kept within 10.0 mg·L-1, and the detection limit was 5.9 μg·L-1. Tests for precision and spiked recovery were carried out on standard materials for biological component analysis, giving RSDs (n=6) of the determined values in the range of 4.0%-8.5%, and the recoveries were 89.0%-97.3%. The proposed method was applied to the analysis of 10 fungus samples, and the determined values were 203-305 mg·kg-1.

       

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