自制四氧化三锰纳米粒子固相萃取-电感耦合等离子体质谱法测定蔬菜中铅和铜

ICP-MS Determination of Lead and Copper in Vegetables with Solid Phase Extraction of Self Made Nanosized Mn₃O₄

摘要: 采用自制四氧化三锰纳米粒子固相萃取-电感耦合等离子体质谱法测定蔬菜中铅和铜的含量。优化的固相萃取条件如下：①样品溶液的pH为4.0；②样品溶液的流量为1.0 mL·min^-1；③四氧化三锰纳米粒子的用量为50 mg；④洗脱剂为3 mol·L^-1盐酸溶液，用量为2 mL；⑤样品溶液的体积为20 mL。铅和铜的线性范围依次为0.01~5.0，0.02~1.0 μg·L^-1，检出限（3s/k）依次为4，8 ng·L^-1。加标回收率为80.0%~108%，测定值的相对标准偏差（n=7）为0.94%~3.2%。

Abstract: ICP-MS was applied to the determination of lead and copper in vegetables with solid phase extraction of self made nanosized Mn₃O₄. The optimized conditions of solid phase extraction were as follows:① pH of the sample solution was 4.0; ② flow rate of the sample solution was 1.0 mL·min^-1; ③ amount of nanosized Mn₃O₄ was 50 mg; ④ the eluant was 3 mol·L^-1 HCl solution and its amount was 2 mL; ⑤ volume of the sample solution was 20 mL. Linearity ranges of lead and copper were found in the ranges of 0.01-5.0, 0.02-1.0 μg·L^-1 respectively, with detection limits (3s/k) of 4, 8 ng·L^-1 respectively. Values of recovery found by standard addition method were in the range of 80.0%-108%, and values of RSDs (n=7) were in the range of 0.94%-3.2%.