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雪冰中痕量高氯酸盐的在线富集方法

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姜苏, 李院生, 潘广文, 王越. 雪冰中痕量高氯酸盐的在线富集方法[J]. 环境化学, 2012, 31(2): 249-253.
引用本文: 姜苏, 李院生, 潘广文, 王越. 雪冰中痕量高氯酸盐的在线富集方法[J]. 环境化学, 2012, 31(2): 249-253.
shu
JIANG Su, LI Yuansheng, PAN Guangwen, WANG Yue. On-line preconcentration of trace level perchlorate in snow and ice[J]. Environmental Chemistry, 2012, 31(2): 249-253.
Citation: JIANG Su, LI Yuansheng, PAN Guangwen, WANG Yue. On-line preconcentration of trace level perchlorate in snow and ice[J]. Environmental Chemistry, 2012, 31(2): 249-253.
shu

雪冰中痕量高氯酸盐的在线富集方法

  • 1.

    中国极地研究中心, 国家海洋局极地科学重点实验室, 上海, 200136;

  • 2.

    戴安中国有限公司上海实验室, 上海, 201203

  • 基金项目:

    国家科技支撑计划项目(2006BAB18B01)

    国家自然科学基金(40906098)

    中国极地科学战略研究基金(20080208)

    国家海洋局青年海洋科学基金(2009512)资助.

On-line preconcentration of trace level perchlorate in snow and ice

  • 1.

    SOA Key Laboratory for Polar Science, Polar Research Institute of China, Shanghai, 200136, China;

  • 2.

    Shanghai Laboratory, Dionex China Limited, Shanghai, 201203, China

  • Fund Project:

  • 摘要: 利用一维离子色谱建立了高氯酸盐的在线富集方法,以期为建立定量检测南极雪冰中痕量高氯酸盐的离子色谱-串联质谱法奠定基础.选用高容量、强亲水性的IonPac AS20阴离子交换柱进行分离,以淋洗液自动发生器在线产生的KOH作为淋洗液,等梯度淋洗.考虑到南极雪冰样品量十分有限,选定5 mL为富集体积,对应的富集时间为10 min.高氯酸盐质量浓度在0.5—50 μg·L-1范围内,方法具有良好的线性(相关系数为0.9995),检出限(以S/N=3计)为0.05 μg·L-1.将浓度为0.5 μg·L-1的标准溶液连续11次富集进样,所得峰面积的相对标准偏差(RSD)为4.7%.以人工配制的仅含有高氯酸盐的溶液实施了加标回收实验,回收率在85%—108%之间.
    Abstract: A simple on-line preconcentration method of perchlorate with ion chromatography is presented, which provides the necessary basis for the determination of trace level perchlorate in Antarctic snow and ice samples by the ion chromatography-electrospray tandem mass spectrometry (IC-ESI-MS-MS). Perchlorate is separated using an IonPac AS20 anion exchange column with high capacity and hydroxide selective, and isogradient potassium hydroxide eluent generated by the automated eluent generator. Due to the limited amount of Antarctic snow and ice samples, injection volume is set to be 5 mL with accumulative time of 10 minutes. The method is linear over the range of 0.5—50 μg·L-1 perchlorate, with linear correlation coefficient of 0.9995. The detection limit for perchlorate is 0.05 μg·L-1. And the relative standard deviation (RSD) of peak area for the eleven successive injections of 0.5 μg·L-1 perchlorate is 4.7%. The simulative water samples containing only perchlorate are used to carry out the recovery test, and results show that the spiked recoveries are in the range of 85%—108%.
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  • [1] Clewell R A, Merrill E A, Yu K O, et al. Predicting fetal perchlorate dose and inhibition of iodide kinetics during gestation: A physiologically-based pharmacokinetic analysis of perchlorate and iodide kinetics in the rat [J]. Toxicol Sci, 2003, 73: 235-255
    [2] Greer M A, Goodman G, Pleus R C, et al. Health effects assessment for environmental perchlorate contamination: The dose response for inhibition of thyroidal radioiodine uptake in humans [J]. Environ Health Perspect, 2002, 110 (9): 927-937
    [3] Snyder S A, Pleus R C, Vanderford B J, et al. Perchlorate and chlorate in dietary supplements and flavor enhancing ingredients [J]. Anal Chim Acta, 2006, 567: 26-32
    [4] Shi Y, Zhang P, Wang Y, et al. Perchlorate in sewage sludge, rice, bottled water and milk collected from different areas in China [J]. Environ Int, 2007, 33: 955-962
    [5] Plummer L N, Bohlke J K, Doughten M W. Perchlorate in Pleistocene and Holocene groundwater in north-central New Mexico [J]. Environ Sci Technol, 2006, 40(6): 1757-1763
    [6] Rajagopalan S, Anderson T A, Fahlquist L, et al. Widespread presence of naturally occurring perchlorate in high plains of Texas and New Mexico [J]. Environ Sci Technol, 2006, 40(10): 3156-3162
    [7] Rao B, Anderson T A, Orris G J, et al. Widespread natural perchlorate in unsaturated zones of the southwest United States [J]. Environ Sci Technol, 2007, 41(13): 4522-4528
    [8] Parker D R, Seyfferth A L, Reese B K. Perchlorate in groundwater: A synoptic survey of "Pristine" sites in the coterminous United States [J]. Environ Sci Technol, 2008, 42(5):1465-1471
    [9] Rajagopalan S, Anderson T, Cox S, et al. Perchlorate in wet deposition across North America [J]. Environ Sci Technol, 2009, 43(3):616-622
    [10] Dasgupta P K, Martinelango P K, Jackson W A, et al. The origin of naturally occurring perchlorate: The role of atmospheric processes [J]. Environ Sci Technol, 2005, 39(6): 1569- 1575
    [11] Renner R. Atmospheric processes may create perchlorate [J]. Environ Sci Technol, 2005, 39: 120A
    [12] Aribi H E, Le Blanc Y J C, Antonsen S, et al. Analysis of perchlorate in foods and beverages by ion chromatography coupled with tandem mass spectrometry (IC-ESI-MS/MS) [J]. Anal Chim Acta, 2006, 567: 39-47
    [13] 史亚利. 离子色谱与API2000(IC/MS/MS)联用分析食品和饮料中的高氯酸盐[J].环境化学, 2006, 25(1): 117-120
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  • 收稿日期:  2011-08-10
姜苏, 李院生, 潘广文, 王越. 雪冰中痕量高氯酸盐的在线富集方法[J]. 环境化学, 2012, 31(2): 249-253.
引用本文: 姜苏, 李院生, 潘广文, 王越. 雪冰中痕量高氯酸盐的在线富集方法[J]. 环境化学, 2012, 31(2): 249-253.
shu
JIANG Su, LI Yuansheng, PAN Guangwen, WANG Yue. On-line preconcentration of trace level perchlorate in snow and ice[J]. Environmental Chemistry, 2012, 31(2): 249-253.
Citation: JIANG Su, LI Yuansheng, PAN Guangwen, WANG Yue. On-line preconcentration of trace level perchlorate in snow and ice[J]. Environmental Chemistry, 2012, 31(2): 249-253.
shu

雪冰中痕量高氯酸盐的在线富集方法

  • 1.  中国极地研究中心, 国家海洋局极地科学重点实验室, 上海, 200136;
  • 2.  戴安中国有限公司上海实验室, 上海, 201203
  • 收稿日期:  2011-08-10
基金项目:

国家科技支撑计划项目(2006BAB18B01)

国家自然科学基金(40906098)

中国极地科学战略研究基金(20080208)

国家海洋局青年海洋科学基金(2009512)资助.

摘要: 利用一维离子色谱建立了高氯酸盐的在线富集方法,以期为建立定量检测南极雪冰中痕量高氯酸盐的离子色谱-串联质谱法奠定基础.选用高容量、强亲水性的IonPac AS20阴离子交换柱进行分离,以淋洗液自动发生器在线产生的KOH作为淋洗液,等梯度淋洗.考虑到南极雪冰样品量十分有限,选定5 mL为富集体积,对应的富集时间为10 min.高氯酸盐质量浓度在0.5—50 μg·L-1范围内,方法具有良好的线性(相关系数为0.9995),检出限(以S/N=3计)为0.05 μg·L-1.将浓度为0.5 μg·L-1的标准溶液连续11次富集进样,所得峰面积的相对标准偏差(RSD)为4.7%.以人工配制的仅含有高氯酸盐的溶液实施了加标回收实验,回收率在85%—108%之间.

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