Research Article | | Peer-Reviewed

Confirmation of the ICP-MS Method for the Determination of Blood Lead

Received: 25 April 2026     Accepted: 1 June 2026     Published: 9 June 2026
Views:       Downloads:
Abstract

Background Lead is a common occupational toxicant. Long-term exposure to lead can damage the nervous and hematopoietic systems. Blood lead concentration is an important biomarker for assessing recent lead exposure. Establishing an accurate and sensitive method for blood lead determination is of great significance for occupational health monitoring. Objective To establish and validate an inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of lead in blood. Methods Using an Agilent 7850 ICP-MS instrument, blood samples were directly diluted with a diluent containing 0.5% nitric acid and 0.01% Triton X-100. Holmium (Ho) was used as an online internal standard. Lead was measured at m/z 206, 207, and 208 in standard mode. The method was validated for linearity, detection limit, quantification limit, recovery, and precision according to the national standard GBZ/T 316.2-2018. Results Excellent linearity was observed in the range of 0–100 μg/L, with correlation coefficients (R²) of 1 for all three mass numbers. The detection limit was 0.013 μg/L, and the quantification limit was 0.044 μg/L. Recoveries at low (0.4 μg/L), medium (40.0 μg/L), and high (400.0 μg/L) concentration levels were 96.23%, 102.28%, and 100.64%, respectively, with relative standard deviations (RSD) of 1.10%, 0.45%, and 0.43%. Conclusion The method is simple, sensitive, and reproducible. All performance indicators are superior to the national standard requirements, making it suitable for rapid and accurate determination of lead in blood among occupationally exposed populations.

Published in Science Research (Volume 14, Issue 3)
DOI 10.11648/j.sr.20261403.15
Page(s) 99-104
Creative Commons

This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.

Copyright

Copyright © The Author(s), 2026. Published by Science Publishing Group

Keywords

Blood Lead, ICP-MS, Method Validation

1.引言
铅是一种广泛存在的重金属毒物,在蓄电池、冶炼、颜料、电子废弃物回收等行业中职业接触风险较高 。铅进入人体后可对多个系统造成损害,其中神经系统和造血系统最为敏感。儿童长期低水平铅暴露可导致智力发育障碍,成人慢性铅中毒则表现为周围神经病、贫血、肾功能损害等 。我国《职业病危害因素分类目录》将铅及其化合物列为重点监测的职业病危害因素。
血铅浓度是反映近期铅暴露(约1个月内)的可靠生物标志物,与中毒症状的严重程度高度相关 。美国CDC建议儿童血铅参考值为50μg/L,我国职业接触限值规定血铅不超过400μg/L 。因此,建立准确、灵敏的血铅测定方法对于职业健康监护、环境暴露评估和临床中毒诊断具有重要意义。
血铅的测定方法经历了从光谱法到质谱法的发展历程。石墨炉原子吸收光谱法(GFAAS)是传统的金标准方法,具有成本较低、操作相对简单的优点,但分析速度慢、线性范围窄,且易受基体干扰。阳极溶出伏安法虽然灵敏度高,但电极稳定性差,不适合大批量样品检测
近年来,电感耦合等离子体质谱法(ICP-MS)因其高灵敏度(检出限可达ng/L级)、宽线性范围(5~6个数量级)和多元素同时分析能力,逐渐成为生物样品金属测定的首选技术。我国于2018年发布了GBZ/T 316.2-2018《血中铅的测定 第2部分:电感耦合等离子体质谱法》,为ICP-MS测定血铅提供了标准化依据。然而,不同实验室在仪器型号、前处理细节、内标选择等方面存在差异,需要根据实际条件进行方法确证
本研究依据GBZ/T 316.2-2018,采用安捷伦7850 ICP-MS仪(配备碰撞反应池和自动进样器),建立并确证血中铅的测定方法。主要内容包括:优化样品前处理和仪器参数,评估方法的线性范围、检出限、定量限、回收率和精密度,为职业卫生检测实验室提供可靠的方法学数据。
2.材料与方法
2.1.仪器与试剂
电感耦合等离子体质谱仪:Agilent 7850 ICP-MS(美国安捷伦公司),配备自动进样器、碰撞反应池。超纯水机:Milli-Q Advantage A10(电阻率18.2 MΩ·cm)。硝酸:优级纯,ρ=1.42 g/mL(德国Merck公司)。Triton X-100:分析纯(美国Sigma-Aldrich公司)。稀释液:0.5%硝酸+0.01% Triton X-100。铅标准溶液(编号SJBZ2640),用稀释液稀释成0.50μg/mL。所有聚乙烯、玻璃器皿用20%硝酸浸泡过夜,冲洗晾干。
2.2.仪器条件
参考GBZ/T 316.2-2018及安捷伦7850推荐条件,优化后的参数见表1
表1 仪器操作条件。

参数

设计值

射频功率

1450 W

冷却气流量(Ar)

12.5 L/min

辅助气流量(Ar)

0.70 L/min

雾化气流量(Ar)

0.92 L/min

蠕动泵转速

30 r/min

雾化器温度

3 ℃

采样深度

8 mm

测定模式

标准模式(无碰撞气体)

测定质量数

206Pb, 207Pb,208Pb

内标元素

165Ho

内标引入方式

在线三通混合

内标浓度

10.0μg/L

采集次数

3次

积分时间

0.1 s/质量数

每个样品总时间

约2 min

2.3.方法确证指标
参照《临床检验方法学评价》 及GBZ/T 316.2-2018要求,对以下指标进行验证:
样品空白的选取与试剂空白的确认:选取3个10mL样品管,分别加入10ml从采血管抽出的去离子水配成样品空白;再用稀释液配成试剂空白,用7850电感耦合等离子质谱仪进行测试;确定试剂空白和样品空白中铅含量均小于0.17μg/L。
线性范围与标准曲线:用0.5%硝酸稀释铅标准溶液,配制0.0、0.5、1.0、5.0、10.0、50.0、100.0μg/L系列浓度。以铅响应值(206Pb、207Pb和208Pb)与内标响应值(165Ho)的比值为纵坐标,浓度为横坐标绘制标准曲线,计算回归方程和相关系数。
检出限与定量限:选取1个50 mL样品管,按GBZ/T 316.2-2018方法处理后配成空白样品;加入0.5μg/mL铅标准溶液40μL,用0.5% HNO₃-0.01% Triton X-100稀释至40.00 mL(铅加标浓度为0.40μg/L)。连续测定11次,计算检出限(LOD = 3×标准误差)和定量限(LOQ = 10×标准误差)。
回收率:选取3个50mL样品管,分别加入0.4μg/L,40.0μg/L和400.0μg/L铅标准溶液2.50mL,用正常血液和稀释液稀释到50.00mL,处理后用7850电感耦合等离子质谱仪测试。铅理论浓度为0.4μg/L,40.0μg/L,400.0μg/L。计算回收率 = 实测浓度 / 理论浓度 × 100%
精密度:用0.4μg/L、40.0μg/L和400.0μg/L平行测试的标样及回收率数据计算精密度。计算精密度 = 标准误差 / 理论浓度
3.结果
3.1.线性范围与标准曲线
依据GBZ/T 316.2-2018,用0.5% HNO₃-0.01% Triton X-100稀释剂配制铅标准系列溶液,浓度分别为0.0、0.5、1.0、5.0、10.0、50.0、100.0μg/L。采用安捷伦7850 ICP-MS在标准模式下测定,以铅响应值与内标钬响应值的比值为纵坐标,浓度为横坐标绘制标准曲线。结果显示,在206Pb、207Pb和208Pb三个质量数下,铅在0~100μg/L范围内线性关系极佳,回归方程分别为y = 2452.7x + 239.67、y = 2157x + 156.56和y = 9852.7x + 693.5,相关系数R²均为1(图1)。安捷伦7850的超高灵敏度离子透镜系统使208Pb的灵敏度达到>100000 cps/ppb,较标准要求的检测能力有显著提升。
Figure 1. 图1 206Pb、207Pb和208Pb标准曲线和线性回归方程。
3.2.检出限与定量限
连续测定低浓度(0.4μg/L)血铅样品7次,以208Pb计算血铅测定值的平均值和标准偏差(SD)。根据公式检出限 = 3 × 标准误差,计算得检出限为0.013μg/L,根据公式定量限 = 10 × 标准误差,计算出定量限为0.044μg/L(表2)。两项指标均显著优于GBZ/T 316.2-2018规定的0.17μg/L和0.7μg/L要求。
表2 检出限与定量限。

检测项目

血铅值(μg/L)

测定平均值

0.3849

理论浓度

0.4000

标准偏差

0.0044

检出限

0.013

定量限

0.044

3.3.回收率与精密度
分别测定0.4μg/L, 40.0μg/L和400.0μg/L铅标准溶液7次,按标准方法处理后测定,计算回收率和精准度。结果见表3,低、中、高浓度的回收率分别为96.23%、102.28%和100.64,符合方法要求(85%~115%)。精密度分别为1.10%、0.45%和0.43%,同样满足方法要求(≤10%)
表3 回收率和精准度试验结果。

理论浓度(μg/L)

实测浓度(μg/L)

回收率(%)

精密度(%)

0.4

0.3849 ± 0.0044

96.23

1.10

40.0

40.91 ± 0.18

102.28

0.45

400.0

402.57 ±1.70

100.64

0.43

4.讨论
4.1.方法学性能分析
本研究建立的血铅ICP-MS测定方法在0~100μg/L范围内线性关系极佳(R²=1),覆盖了职业接触人群血铅的常见范围(一般<400μg/L)及急性中毒时的较高浓度(可达1000μg/L以上)。通过稀释可进一步扩展至1000μg/L。方法检出限为0.013μg/L,远低于我国儿童血铅干预水平(50μg/L)和职业接触限值(400μg/L),满足最严格的筛查要求
在回收率方面,低、中、高三个浓度水平的回收率均接近100%,表明该方法准确度高,无明显系统误差。精密度RSD均小于1.5%,重复性优良,适合大批量样品的日常检测。
4.2.干扰控制与内标选择
血样基体复杂,含有高浓度盐分和蛋白质,可能导致基体效应和信号漂移。本研究采用在线引入165Ho内标进行校正,有效补偿了基体效应和仪器波动。实验全程内标响应稳定在±10%以内,保证了测定结果的可靠性。
铅的三个同位素中,204Pb受204Hg干扰,206Pb、207Pb和208Pb基本无同质异位素干扰。正常血样中汞含量极低,因此选择206Pb、207Pb和208Pb同时测定取均值可进一步提高准确性。稀释液中加入0.01% Triton X-100有助于裂解血细胞、溶解膜蛋白,同时降低表面张力,提高雾化稳定性
4.3.与国家标准及其他方法的比较
与GBZ/T 316.2-2018相比,本方法的检出限(0.013μg/L)显著优于标准要求的0.17μg/L,定量限(0.044μg/L)也远低于0.7μg/L。这主要得益于安捷伦7850 ICP-MS的高灵敏度离子透镜系统和优化的前处理条件。在回收率和精密度方面,本方法同样达到或超过了标准要求。
与文献报道的其他ICP-MS方法 相比,本方法采用直接稀释法(稀释倍数约10倍),避免了微波消解等复杂前处理步骤,单个样品分析时间仅需2 min,大大提高了检测通量,适合大规模职业健康筛查
4.4.局限性与改进方向
本研究存在以下局限性:仅验证了铅单元素,未扩展至血中其他金属(如镉、锰、铬等)。实际工作中可利用ICP-MS的多元素同时检测能力,建立血中多种金属的联合测定方法。此外,未进行实验室间比对,未来应参与室间质评计划,进一步验证方法的准确性和可比性。
改进方向包括:建立血中多元素同时测定的标准操作程序;引入自动进样器实现高通量分析;开发在线稀释系统减少人工操作误差。
5.结论
本研究依据GBZ/T 316.2-2018,使用安捷伦7850 ICP-MS建立了血中铅的直接稀释测定方法,并完成了全面的方法学确证。结果表明,该方法在0~100μg/L范围内线性良好(R²=1),检出限低至0.013μg/L,定量限为0.044μg/L,低、中、高浓度回收率分别为96.23%、102.28%和100.64%,精密度RSD分别为1.10%、0.45%和0.43%。各项指标均显著优于国家标准要求,且操作简便、成本较低、适合大批量样品检测。本方法可作为职业接触人群血铅筛查的可靠手段,为职业卫生监测和临床中毒诊断提供技术支持。
References
[1] 中华人民共和国国家卫生健康委员会. 职业病危害因素分类目录 [S]. 北京: 中国标准出版社, 2015.
[2] 孟金萍, 孙淑华, 王艳蓉,等.铅的生物学毒性效应 [J]. 中国比较医学杂志, 2007(01): 58-61.
[3] 杜林, 黄鸿志, 王雅茜. 铅中毒及其防治研究进展 [J]. 广东微量元素科学, 2001, 8(5): 10.
[4] 杨晓琳, 王苗苗, 张金龙等. 铅暴露水平与主要生物监测指标的剂量-反应关系[J]. 职业与健康, 2013(19): 2.
[5] CDC. Adult Blood Lead Epidemiology and Surveillance (ABLES) Annual Report[R]. Atlanta: Centers for Disease Control and Prevention, 2024.
[6] 陶雪, 潘亚娟, 闫慧芳. 石墨炉原子吸收光谱法测定血铅若干问题探讨[J]. 中华劳动卫生职业病杂志, 2013, 31(8): 2.
[7] 游慧圆, 沈丽菲, 张琼等. 原子吸收光谱仪测定全血中铅, 镉的方法研究[J]. 大众科技, 2018(004): 020.
[8] 李筱薇, 高俊全. 阳极溶出伏安法与石墨炉原子吸收光谱法在血铅检测中的应用比较 [J]. 卫生研究, 2007, 36(1): 3.
[9] 张爱华, 董明, 李娟等. 电感耦合等离子体-质谱在职业卫生检测中应用 [J]. 中国职业医学, 2014, 041(001): 56-60.
[10] GBZ/T 316.2-2018, 血中铅的测定 第2部分: 电感耦合等离子体质谱法 [S]. 北京: 中国标准出版社, 2018.
[11] 王治国. 临床检验方法学评价 [M]. 第2版. 北京: 人民卫生出版社, 2020: 156-170.
[12] 张淼, 郑磊, 孙琦等. 电感耦合等离子体质谱法测定血铅实验影响因素 [J]. 卫生研究, 2023, 6: 136-141.
[13] Liu Y, Liu F, Dong KF, et al. Regional characteristics of children's blood lead levels in China: A systematic synthesis of national and subnational population data [J]. Science of The Total Environment, 2021, 769(9): 144649.
[14] 彭荣飞, 甘平胜, 黄聪. ICP-MS直接测定儿童全血中Pb, Cd, Cu, Zn, Mn, Fe和Ca [J]. 中国卫生检验杂志, 2006, 16(011): 1303-1304.
[15] Gajek R, Barley F, She J. Determination of essential and toxic metals in blood by ICP-MS with calibration in synthetic matrix [J]. Analytical Methods, 2013, 5, 2193-2202.
Cite This Article
  • APA Style

    Zhou, X. (2026). Confirmation of the ICP-MS Method for the Determination of Blood Lead. Science Research, 14(3), 99-104. https://doi.org/10.11648/j.sr.20261403.15

    Copy | Download

    ACS Style

    Zhou, X. Confirmation of the ICP-MS Method for the Determination of Blood Lead. Sci. Res. 2026, 14(3), 99-104. doi: 10.11648/j.sr.20261403.15

    Copy | Download

    AMA Style

    Zhou X. Confirmation of the ICP-MS Method for the Determination of Blood Lead. Sci Res. 2026;14(3):99-104. doi: 10.11648/j.sr.20261403.15

    Copy | Download

  • @article{10.11648/j.sr.20261403.15,
      author = {Xiaomin Zhou},
      title = {Confirmation of the ICP-MS Method for the Determination of Blood Lead},
      journal = {Science Research},
      volume = {14},
      number = {3},
      pages = {99-104},
      doi = {10.11648/j.sr.20261403.15},
      url = {https://doi.org/10.11648/j.sr.20261403.15},
      eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.sr.20261403.15},
      abstract = {Background Lead is a common occupational toxicant. Long-term exposure to lead can damage the nervous and hematopoietic systems. Blood lead concentration is an important biomarker for assessing recent lead exposure. Establishing an accurate and sensitive method for blood lead determination is of great significance for occupational health monitoring. Objective To establish and validate an inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of lead in blood. Methods Using an Agilent 7850 ICP-MS instrument, blood samples were directly diluted with a diluent containing 0.5% nitric acid and 0.01% Triton X-100. Holmium (Ho) was used as an online internal standard. Lead was measured at m/z 206, 207, and 208 in standard mode. The method was validated for linearity, detection limit, quantification limit, recovery, and precision according to the national standard GBZ/T 316.2-2018. Results Excellent linearity was observed in the range of 0–100 μg/L, with correlation coefficients (R²) of 1 for all three mass numbers. The detection limit was 0.013 μg/L, and the quantification limit was 0.044 μg/L. Recoveries at low (0.4 μg/L), medium (40.0 μg/L), and high (400.0 μg/L) concentration levels were 96.23%, 102.28%, and 100.64%, respectively, with relative standard deviations (RSD) of 1.10%, 0.45%, and 0.43%. Conclusion The method is simple, sensitive, and reproducible. All performance indicators are superior to the national standard requirements, making it suitable for rapid and accurate determination of lead in blood among occupationally exposed populations.},
     year = {2026}
    }
    

    Copy | Download

  • TY  - JOUR
    T1  - Confirmation of the ICP-MS Method for the Determination of Blood Lead
    AU  - Xiaomin Zhou
    Y1  - 2026/06/09
    PY  - 2026
    N1  - https://doi.org/10.11648/j.sr.20261403.15
    DO  - 10.11648/j.sr.20261403.15
    T2  - Science Research
    JF  - Science Research
    JO  - Science Research
    SP  - 99
    EP  - 104
    PB  - Science Publishing Group
    SN  - 2329-0927
    UR  - https://doi.org/10.11648/j.sr.20261403.15
    AB  - Background Lead is a common occupational toxicant. Long-term exposure to lead can damage the nervous and hematopoietic systems. Blood lead concentration is an important biomarker for assessing recent lead exposure. Establishing an accurate and sensitive method for blood lead determination is of great significance for occupational health monitoring. Objective To establish and validate an inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of lead in blood. Methods Using an Agilent 7850 ICP-MS instrument, blood samples were directly diluted with a diluent containing 0.5% nitric acid and 0.01% Triton X-100. Holmium (Ho) was used as an online internal standard. Lead was measured at m/z 206, 207, and 208 in standard mode. The method was validated for linearity, detection limit, quantification limit, recovery, and precision according to the national standard GBZ/T 316.2-2018. Results Excellent linearity was observed in the range of 0–100 μg/L, with correlation coefficients (R²) of 1 for all three mass numbers. The detection limit was 0.013 μg/L, and the quantification limit was 0.044 μg/L. Recoveries at low (0.4 μg/L), medium (40.0 μg/L), and high (400.0 μg/L) concentration levels were 96.23%, 102.28%, and 100.64%, respectively, with relative standard deviations (RSD) of 1.10%, 0.45%, and 0.43%. Conclusion The method is simple, sensitive, and reproducible. All performance indicators are superior to the national standard requirements, making it suitable for rapid and accurate determination of lead in blood among occupationally exposed populations.
    VL  - 14
    IS  - 3
    ER  - 

    Copy | Download

Author Information
  • Abstract
  • Keywords
  • Document Sections

    Show Full Outline
  • 1.引言
  • 2.材料与方法
  • 3.结果
  • 4.讨论
  • 5.结论
  • References
  • Cite This Article
  • Author Information