GFAAS Determination of Lead and Cadmium in Yeast Extract with Separation by Ion Exchange
摘 要
酵母抽提物样品(1.000 g)经硝酸(20 mL)消解并蒸干后加水(10 mL),调整其酸度至pH 4.0。溶液通过D401离子交换树脂分离,用0.002 5 mol·L-1硝酸溶液(pH 2.6)淋洗交换柱后,用0.2 mol·L-1硝酸溶液洗脱吸附于树脂上的铅(Ⅱ)和镉(Ⅱ)。将洗脱液蒸至近干,用水定容至10 mL。用石墨炉原子吸收光谱法测定其中铅、镉的含量,两者的线性范围依次为50~350,3~15 pg,检出限(3s)依次为5.0,0.3 pg。对3个实样按所提出方法进行分析,并用标准加入法计算方法的回收率为84.0%~115%,测定值的相对标准偏差(n=8)为1.8%~12%。
Abstract
The sample (1.000 g) of yeast extract was digested with HNO3 (20 mL). The solution was evaporated to dryness, and the residue was taken up with water (10 mL), and the acidity was adjusted to pH 4.0. D401 ion-exchange resin was used for separation of lead and cadmium from the solution. After rinsing the column with 0.002 5 mol·L-1 HNO3 solution (pH 2.6), lead(Ⅱ) and cadmium(Ⅱ) were desorbed from the column with 0.2 mol·L-1 HNO3 solution, and the eluate was evaporated to near dryness. Water was added attaining to 10 mL, and contents of lead and cadmium in the solution were determined by GFAAS. Linearity ranges were found between 50 to 350 pg (lead) and 3 to 15 pg (cadmium), with detection limits (3s) of 5.0, 0.3 pg respectively. Three samples were analyzed by this method, and values of recovery found by standard addition method were in the range of 84.0% to 115%, giving values of RSD's (n=8) ranged from 1.8% to 12%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx201802013
所属栏目 工作简报
基金项目
收稿日期 2017/2/25
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联系人作者吴文启(ciqw@163.com)
备注胡雨欣(1990-),女,湖南长沙人,助理工程师,主要从事物质的化学成分检测工作
引用该论文: HU Yuxin,XIE Xiaoyan,WEI Yiling,TAN Wei,LI Fen,WU Wenqi. GFAAS Determination of Lead and Cadmium in Yeast Extract with Separation by Ion Exchange[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(2): 187~191
胡雨欣,谢晓雁,韦懿玲,谭微,李奋,吴文启. 离子交换分离-石墨炉原子吸收光谱法测定酵母抽提物中铅和镉[J]. 理化检验-化学分册, 2018, 54(2): 187~191
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参考文献
【1】GB 5009.12-2010食品安全国家标准食品中铅的测定[S].
【2】GB/T 23530-2009酵母抽提物[S].
【3】吴文启.分析化学的成果与挑战[C].重庆:西南师范大学出版社, 2000.
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【5】刘辉,江军.纳米TiO2富集分离石墨炉原子吸收法测定食品中的镉[J].食品研究与开发, 2012,31(1):108-110.
【6】GB 17378.4-2007海洋监测规范[S].
【7】苏熘东,郝冰冰,李静,等.应用内标的PAN-Ni体系快速共沉淀分离富集和火焰原子吸收光谱测定食盐中铅[J].理化检验-化学分册, 2006,42(2):97-99.
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【9】STRELOW F W E. An ion exchange selectivity scale of cations based on equilibrium distribution coefficients[J]. Analytical Chemistry, 1960,32(9):1185-1188.
【10】李奋,吴文启,谢晓雁,等.离子交换分离-石墨炉原子吸收光谱法测定饮用水中痕量铊[J].理化检验-化学分册, 2015,51(12):1675-1679.
【2】GB/T 23530-2009酵母抽提物[S].
【3】吴文启.分析化学的成果与挑战[C].重庆:西南师范大学出版社, 2000.
【4】刘辉,吴秋杰.纳米TiO2富集分离石墨炉原子吸收法测定食品中的铅[J].徐州工程学院学报(自然科学版), 2009,24(1):38-41.
【5】刘辉,江军.纳米TiO2富集分离石墨炉原子吸收法测定食品中的镉[J].食品研究与开发, 2012,31(1):108-110.
【6】GB 17378.4-2007海洋监测规范[S].
【7】苏熘东,郝冰冰,李静,等.应用内标的PAN-Ni体系快速共沉淀分离富集和火焰原子吸收光谱测定食盐中铅[J].理化检验-化学分册, 2006,42(2):97-99.
【8】周锦帆.Chelex-100螯合树脂在分离和测定中的应用[J].现代商检科技, 1992,2(5):46-52.
【9】STRELOW F W E. An ion exchange selectivity scale of cations based on equilibrium distribution coefficients[J]. Analytical Chemistry, 1960,32(9):1185-1188.
【10】李奋,吴文启,谢晓雁,等.离子交换分离-石墨炉原子吸收光谱法测定饮用水中痕量铊[J].理化检验-化学分册, 2015,51(12):1675-1679.
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