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%。
四氧化三锰
铅
铜
固相萃取
ICP-MS
Mn3O4
lead
copper
soild phase extraction
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%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201808005
所属栏目 工作简报
基金项目 江苏省卫生厅预防医学科研基金（Y2015035）；淮安市科技局科技支撑（社会发展）项目基金（HAS2015030）
收稿日期 2017/10/24
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联系人作者王芹(wlnear@163.com)
备注王露,硕士研究生,检验师,主要从事理化检验工作
引用该论文: WANG Lu,XU Rui,WANG Qin,SONG Xin,FENG Xiaoqing,WANG Yi,HANG Xueyu. ICP-MS Determination of Lead and Copper in Vegetables with Solid Phase Extraction of Self Made Nanosized Mn3O4[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(8): 892～895
王露,徐瑞,王芹,宋鑫,冯晓青,汪怡,杭学宇. 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[J]. 理化检验－化学分册, 2018, 54(8): 892～895
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【4】SERIFE T, FATMA G. Selective determination of copper and iron in various food samples by the solid phase extraction[J]. Food Chemistry, 2010,123(1):183-187.
【5】STONGE L M, DOLAR E, ANGLIM M A, et al. Improved determination of phenobarbital, primidone, and phenytoin by use of a preparative instrument for extraction, followed by gas chromatography[J]. Clinical Chemistry, 1979,25(8):1373-1376.
【6】ABDOLMOHAMMAD-ZADEH H, KOHANSAL S, SADEGHI G H. Nickel-aluminum layered double hydroxide as a nanosorbent for selective solid-phase extraction and spectrofluorometric determination of salicylic acid in pharmaceutical and biological samples[J]. Talanta, 2011,84(2):368-373.
【7】SOLEIMANI M, AFSHAR M G. Highly selective solid phase extraction of mercury ion based on novel ion imprinted polymer and its application to water and fish samples[J]. Journal of Analytical Chemistry, 2015,70(1):5-12.
【8】SUN J, LIANG Q, HAN Q, et al. One-step synthesis of magnetic graphene oxide nanocomposite and its application in magnetic solid phase extraction of heavy metal ions from biological samples[J]. Talanta, 2015,132(4):557-563.
【9】杨潇,张朝晖,张华斌,等.基于壳聚糖修饰碳纳米管表面铅离子印迹材料的制备及其性能研究[J].分析化学, 2011,39(1):34-38.
【10】ZHANG D, NIU H, ZHANG X, et al. Strong adsorption of chlorotetracycline on magnetite nanoparticles[J]. Journal of Hazardous Materials, 2011,192(3):1088-1093.
【11】GAO J, LOWE M A, ABRUÑA H D. Spongelike nanosized Mn3O4 as a high-capacity anode material for rechargeable lithium batteries[J]. Chemistry of Materials, 2011,23(13):3223-3227.
【12】苑鹤,王卫娜,吴秋华,等.磁性石墨烯固相萃取/原子吸收法测定环境水样中的痕量铜[J].分析测试学报, 2013,32(1):69-73.
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【14】王娜妮,王绪平,张扬,等.环境水体中痕量铅的碳纳米管固相萃取-原子吸收分光光度测定法[J].环境与健康杂志, 2014,31(9):801-803.
【15】YIN J, JIANG Z, CHANG G, et al. Simultaneous on-line preconcentration and determination of trace metals in environmental samples by flow injection combined with inductively coupled plasma mass spectrometry using a nanometer-sized alumina packed micro-column[J]. Analytica Chimica Acta, 2005,540(2):333-339.
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