固相萃取-电感耦合等离子体质谱法(ICP-MS)测定高盐食品中重金属元素的方法研究

Research on methods of heavy metals in high salt food by solid phase extraction inductively coupled plasma mass spectrometry(ICP-MS)

建立固相萃取-电感耦合等离子体质谱法(ICP-MS)测定高盐食品中铅、镉、铜、镍的分析方法。结果表明:当过柱溶液pH=5.5、过柱流速5 mL/min、采用3 mol/L的硝酸5 mL作为洗脱剂时,4种元素的分离富集效果最好。铅、镉、镍在0~50.0μg/L范围内线性关系良好,线性相关系数r>0.9999,铜在0~500.0μg/L范围内线性关系良好,线性相关系数r>0.9999;高盐实物标准样品紫菜粉(GBW10245)铅、镉、镍、铜测定值分别为(1.73±0.09)、(2.01±0.025)、(6.36±0.078)、(25.8±0.32)mg/kg,与真值中位值偏差分别为4.2%、0.5%、6.0%、-4.4%,相对标准偏差分别为5.2%、1.2%、1.2%、1.2%。

A solid phase extraction inductively coupled plasma mass spectrometry(ICP-MS)method was established for the determination of lead,cadmium,copper and nickel in high salt food.The results showed that when the pH of the column passing solution was 5.5,the flow rate was 5 mL/min,and 5 mL of 3 mol/L nitric acid was used as the eluent,the separation and enrichment effects of the four elements were the best.Lead,cadmium and nickel had good linear relationships in the range of 0-50.0μg/L with linear correlation coefficient r>0.9999,copper had good linear relationships in the range of 0-500.0μg/L with linear correlation coefficient r>0.9999.The measured values of lead,cadmium,nickel and copper in the high salt standard sample of seaweed powder(GBW10245)were(1.73±0.09),(2.01±0.025),(6.36±0.078),and(25.8±0.32)mg/kg,respectively.The deviations from the true median values were 4.2%,0.5%,6.0%and-4.4%,respectively,and the relative standard deviations were 5.2%,1.2%,1.2%and 1.2%,respectively.