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
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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1.0mL·min~(-1);(3)四氧化三锰纳米粒子的用量为50mg;(4)洗脱剂为3mol·L~(-1)盐酸溶液,用量为2mL;(5)样品溶液的体积为20mL。铅和铜的线性范围依次为0.01~5.0,0.02~1.0μg·L~(-1),检出限(3s/k)依次为4,8ng·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%。
ICP-MS was applied to the determination of lead and copper in vegetables with solid phase extraction of self made nanosized Mn_3O_4.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 1.0mL·min~(-1);(3)amount of nanosized Mn_3O_4was 50mg;(4)the eluant was 3mol·L~(-1 )HCl solution and its amount was 2mL;(5)volume of the sample solution was 20mL.Linearity ranges of lead and copper were found in the ranges of 0.01-5.0,0.02-1.0μg·L~(-1 )respectively,with detection limits(3s/k)of 4,8ng·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%.
ICP-MS was applied to the determination of lead and copper in vegetables with solid phase extraction of self made nanosized Mn_3O_4.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 1.0mL·min~(-1);(3)amount of nanosized Mn_3O_4was 50mg;(4)the eluant was 3mol·L~(-1 )HCl solution and its amount was 2mL;(5)volume of the sample solution was 20mL.Linearity ranges of lead and copper were found in the ranges of 0.01-5.0,0.02-1.0μg·L~(-1 )respectively,with detection limits(3s/k)of 4,8ng·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%.
引文
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[3]阮喜云,钟士江,刘庆勇,等.铜过量的表现[J].国外医学医学地理分册,1999(4):157-159.
[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,ABRUA 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.
[13]王许诺,王增焕,陈瑛娜.固相萃取-石墨炉原子吸收法测定海水中铅、镉和铜[J].分析试验室,2016,35(10):1157-1160.
[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.
[16]蒲秋梅,任凤莲,江放明,等.分子印迹功能介孔材料富集-火焰原子吸收光谱法测定溶液中痕量铅[J].分析试验室,2012,31(9):110-113.
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