张敬, 潘亚娟, 宋爽, 闫慧芳. 不同基体改进剂在铅尿测定中的比对[J]. 环境卫生学杂志, 2018, 8(6): 493-498. DOI: 10.13421/j.cnki.hjwsxzz.2018.06.010
    引用本文: 张敬, 潘亚娟, 宋爽, 闫慧芳. 不同基体改进剂在铅尿测定中的比对[J]. 环境卫生学杂志, 2018, 8(6): 493-498. DOI: 10.13421/j.cnki.hjwsxzz.2018.06.010
    ZHANG Jing, PAN Yajuan, SONG Shuang, YAN Huifang. Comparing Different Matrix Modifiers on Lead Detection in Urine[J]. Journal of Environmental Hygiene, 2018, 8(6): 493-498. DOI: 10.13421/j.cnki.hjwsxzz.2018.06.010
    Citation: ZHANG Jing, PAN Yajuan, SONG Shuang, YAN Huifang. Comparing Different Matrix Modifiers on Lead Detection in Urine[J]. Journal of Environmental Hygiene, 2018, 8(6): 493-498. DOI: 10.13421/j.cnki.hjwsxzz.2018.06.010

    不同基体改进剂在铅尿测定中的比对

    Comparing Different Matrix Modifiers on Lead Detection in Urine

    • 摘要:
      目的 通过不同基体改进剂在尿铅测定方法中的比对,达到优化检测方法,以降低基体改进剂对尿铅测定结果的影响。
      方法 将酸化的尿样与基体改进剂混匀,采用原子吸收分光光度计进行测定。
      结果 方法线性范围为(0~200)μg/L,磷酸二氢铵作为基体改进剂峰面积定量r=0.998 5,峰高定量r=0.999 2,氯化钯作为基体改进剂峰面积定量r=0.999 3,峰高定量r=0.999 3。方法的最小检出浓度为1.00 μg/L,定量下限为3.00 μg/L,方法的加标回收率:磷酸二氢铵基体改进剂峰高定量加标回收率范围为:73.0%~86.0%,峰面积定量加标回收率范围为:73.0%~78.0%。氯化钯基体改进剂峰面积定量加标回收率范围为:97.0%~98.0%。峰高定量加标回收率范围为:97.0%~103%;方法精密度:磷酸二氢铵基体改进剂峰高定量精密度的范围为3.20%~14.0%,峰面积定量精密度的范围为4.60%~18.0%。氯化钯基体改进剂峰面积定量精密度的范围为1.00%~3.90%。
      结论 磷酸二氢铵基体改进剂处理的样品受到定量方式的影响使得峰面积定量结果低于峰高定量结果,石墨管使用寿命受改进剂的影响较大。氯化钯基体改进剂处理的样品不受定量方式限制,石墨管使用寿命较长,加标回收率及精密度结果均优于磷酸二氢铵基体改进剂且各项技术指标均满足《职业卫生标准制定指南第5部分:生物材料中化学物质测定方法》(GBZ/T 210.5-2008)的要求。因此,使用氯化钯作为基体改进剂测定样品时效果优于磷酸二氢铵基体改进剂。当样品浓度超过线性范围时,在处理样品时标准系列及样品的处理方法应一致,避免出现基体效应造成结果偏离。

       

      Abstract:
      Objectives To optimize the detection of lead in urine by comparing different matrix modifiers to reduce the effect of matrix modifier on measurement results.
      Methods Acidified urine samples and matrix modifier were mixed and using atomic absorption spectrophotometry (AAS) for the detection.
      Results The linearity was good in the range of (0~200) μg/L. The r was more than 0.99 when measured by peak area or by peak height. The limit of detection (LOD) was 1.00 μg/L and the limit of quantitation (LOQ) was 3.00 μg/L. The recovery was in the range of 73.0%~86.0% and 73.0%~78.0% for peak height and peak area when ammonium dihydrogen phosphate was used as a matrix modifier; and the recovery was in the range of 97.0%~98.0% and 97.0%~103% for peak area and peak height when palladium chloride was used as matrix modifier. The RSD was in the range of 3.20%~14.0% and 4.60%~18.0% for peak height and peak area when ammonium dihydrogen phosphate was used as a matrix modifier; and the RSD was in the range of 1.00%~3.90% for peak area when palladium chloride was used as a matrix modifier.
      Conclusions The quantitative result calculated by peak area was lower than that by peak height when ammonium dihydrogen phosphate was used as matrix modifier, but no limitation was observed on the quantitative result of palladium chloride matrix modifier treated samples. The service life of graphite tube was longer for palladium chloride matrix modifier and the recovery and precision of sample results treated by palladium chloride matrix modifier were better than those treated by ammonium dihydrogen phosphate matrix modifier. All technical indicators met the requirement of the Guidelines for the Establishment of Occupational Health Standards Part 5:Determination of Chemical Substances in Biological Materials (GBZ/T 210.5-2008). Therefore, palladium chloride was better than ammonium dihydrogen phosphate used as matrix modifier in the detection of lead in urine samples. When the concentration of lead in urine sample was out of the linear range, standard series and the sample treatment method should be the same, so as to avoid the deviation of results caused by matrix effect.

       

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