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应用 TDA AAS 直接测定法医毒理学检验死后材料中的汞。

Application of TDA AAS to Direct Mercury Determination in Postmortem Material in Forensic Toxicology Examinations.

机构信息

Institute of Forensic Research, Department of Forensic Toxicology, Westerplatte 9, Krakow, Poland.

Department of Chemistry, Jagiellonian University, Gronostajowa 2, Krakow, Poland.

出版信息

J Anal Toxicol. 2019 Jun 1;43(5):385-391. doi: 10.1093/jat/bky107.

Abstract

Mercury is a heavy metal with high toxicity, the level of which depends on the form of the metal. One of the newer techniques for determining trace amounts of total mercury in various materials, including biological samples, is thermal decomposition, amalgamation and atomic absorption spectrometry (TDA AAS). The TDA AAS method was optimized and validated using a mercury analyzer (DMA-80). The limits of detection for mercury were 0.10 and 0.20 μg/L (nickel and quartz boats, respectively). The working range of the calibration curve was at least from 0.6 to 200 ng Hg/mL; the intra-day precision in samples (RSD)-in the range of: 1.66-6.86% (blood), 0.82-1.47% (urine) and 2.01-3.44% (hair); the inter-day precision (over 8 days): 2.51%, and 2.5% (blood spiked with 2.5 and 10 ng Hg, respectively), 5.10% and 3.16% (urine spiked with 2.0 and 6.0 ng Hg, respectively). The accuracy (as relative error, mean value) determined on the basis of the study of reference materials of blood (Seronorm Trace Elements Whole Blood L-1, L-2, L-3), urine (Seronorm Trace Elements Urine, Urine L-2), and hair (Human Hair NIES CRM No. 13) was: 2.00% (blood), 0.50% (urine) and 0.86% (hair); recovery of 2.5 ng Hg (blood): 93-97%. The method was used for the determination of mercury in 76 samples of various biological matrices, including samples of whole blood, urine, hair, bile and vitreous humor. Mercury concentrations in postmortem blood (n = 24) were in the range: 0.61-12.4 μg/L (median 3.02 μg/L); urine (n = 12): 0.16-2.19 μg/L (median 0.81 μg/L); hair (n = 14): 0.08-0.53 μg/g (median 0.22 μg/g); bile (n = 12): 1.15-7.11 μg/L (median 2.41 μg/L and vitreous humor (n = 13): 0.22-1.01 μg/L (median 0.47 μg/L). The method is suitable for the purposes of forensic toxicology analysis.

摘要

汞是一种具有高毒性的重金属,其毒性水平取决于金属的形态。一种用于测定各种材料(包括生物样本)中总汞痕量的新技术是热分解、汞齐化和原子吸收光谱法(TDA AAS)。使用汞分析仪(DMA-80)对 TDA AAS 方法进行了优化和验证。汞的检测限分别为 0.10 和 0.20μg/L(镍和石英舟)。校准曲线的工作范围至少为 0.6 至 200ngHg/mL;样品的日内精密度(RSD)范围为:1.66-6.86%(血液)、0.82-1.47%(尿液)和 2.01-3.44%(头发);8 天内的日间精密度为 2.51%,血液中分别添加 2.5 和 10ngHg 的加标回收率为 2.5%,尿液中分别添加 2.0 和 6.0ngHg 的加标回收率为 5.10%和 3.16%。基于对血液(Seronorm Trace Elements Whole Blood L-1、L-2、L-3)、尿液(Seronorm Trace Elements Urine、Urine L-2)和头发(Human Hair NIES CRM No.13)参考物质研究的结果,确定了准确度(以相对误差,平均值表示)为:2.00%(血液)、0.50%(尿液)和 0.86%(头发);血液中添加的 2.5ngHg 的回收率为 93-97%。该方法用于测定 76 种不同生物基质样本中的汞,包括全血、尿液、头发、胆汁和玻璃体样本。24 例死后血液样本中的汞浓度范围为:0.61-12.4μg/L(中位数为 3.02μg/L);12 例尿液样本中的浓度范围为:0.16-2.19μg/L(中位数为 0.81μg/L);14 例头发样本中的浓度范围为:0.08-0.53μg/g(中位数为 0.22μg/g);12 例胆汁样本中的浓度范围为:1.15-7.11μg/L(中位数为 2.41μg/L)和 13 例玻璃体样本中的浓度范围为:0.22-1.01μg/L(中位数为 0.47μg/L)。该方法适用于法医毒物分析。

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