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1,2-二氯乙烷接触生物监测指标及检测方法研究
作者:周丽屏 邓燕君 刘移民

摘要:

目的  研究1,2-二氯乙烷(1,2-DCE)染毒处理大鼠血样中1,2-DCE含量与静式染毒柜空气中1,2-DCE的剂量-反应关系,探讨人血样中1,2-DCE作为接触生物监测指标的可行性,建立人血样中1,2-DCE的检测方法。方法  使用静态顶空进样器及气相色谱质谱联用仪测定染毒处理大鼠血样中1,2-DCE含量,采用Pearson相关分析法分析染毒处理大鼠血样中1,2-DCE含量与静式染毒柜空气中1,2-DCE浓度的关系。取15份无接触1, 2-DCE的正常人血样各3.0 ml,分别加入2.0 ml 1,2-DCE标准应用液后马上密封顶空瓶盖,置于静态顶空装置中80 ℃加热平衡20 min,顶空瓶上方蒸汽经毛细管色谱柱分离,选择离子进行定量测定血样中1,2-DCE,并绘制标准工作曲线。分别在1 d及3 d内对人血中1, 2-DCE含量进行6次重复测定,计算相对标准偏差,得出方法批内及批间精密度范围。根据P=(C2-C0)/C1×100%,计算本方法的加标回收率。结果  静式吸入染毒柜内1, 2-DCE浓度为1 472、2 550、3 093、3 976和4 418 mg/m3的剂量组大鼠血样中,1,2-DCE含量均值分别为24.1、231.6、344.3、395.1、538.5 μg/L,与1,2-DCE剂量呈正相关,剂量-反应关系回归方程为y=0.162x-195.8,r值为0.982 2,P=0.003,染毒精密度实验的相对标准偏差范围在7.04%~13.15%。3.0 ml人血样中1,2-DCE在0.259~2 587 μg/L范围内线性关系良好,总体回归方程为y=47 901x-357 446,r值为0.999 8。以人血样中1, 2-DCE质量浓度为0.259 μg/L的样品检测的6次数据计算峰/峰信噪比值均值为56.55,检出限为0.014 μg/L,定量限为0.046 μg/L。批内精密度为1.23%~2.76%,批间精密度为2.21%~4.64%。3.0 ml人血样平均加标回收率为93.3%~98.6%。结论  血中1,2-DCE可作为接触生物监测指标,静态顶空进样器及气相色谱质谱联用仪测定血中1,2-DCE含量灵敏度高、线性范围宽、干扰少、精密度好、操作简单。

关键词:二氯乙烷类;环境监测;血液;静态顶空进样-气相色谱质谱联用法

Abstract:

Objective  To investigate the feasibility of using the concentration of 1,2-DCE in blood as a biological monitoring indicators and build the determination method of 1,2-DCE in blood.Methods  Dose-response relationship of the exposure of 1,2-DCE and the level of 1,2-DCE in rat blood were investigated using the Pearson's correlation analysis. The concentration of 1,2-DCE in blood was determined using Headspace Sampler-Gas Chromatography-Mass Spectrometer (HS-GC-MS). 3.0 ml blood sample diluting with 2.0 ml 1,2-DCE standard serial solution was placed in 15 headspace bottles respectively and heated at 80 ℃ for 20 min.The vapor upon the headspace bottle was separated by capillary column and the concentration of 1,2-DCE was determined by massspectrum in SIM mode to draw a standard work curve. The within-run precision and the between-run precision were calculated by the relative standard deviation (RSD) of the concentration of 1,2-DCE in blood which was determined 6 times in a day and 6 times within 3 days respectively. The recovery rate was calculated by P=(C2 -C0)/C1×100%.Results  When the treatment groups were exposed at dosage of 1 472, 2 550, 3 093, 3 976, and 4 418 mg/m3, the average concentration of 1,2-DCE in rat blood was 24.1,231.6,344.3,395.1,538.5 μg/L. There was a positive correlation between the concentration of 1,2-DCE in rat blood and the exposed level of 1,2-DCE.The equation of dose-response relationship was y=0.162x -195.8,r=0.982 2,P=0.003 and the precision of exposure experiments was 7.04% -13.15%. 1,2-DCE contents within 0.259 -2 587 μg/L showed a good linear relationship and the regression equation was y=47 901x -357 446, r= 0.999 8. When the blood containing 0.259 μg/L 1,2-DCE was determined for six times, the average peak/peak signal-to-noise ratio was 56.55. The limit of detection (LOD) was 0.014 μg/L and the limit of quantification (LOQ) was 0.046 μg/L. The within-run precision was 1.23% -2.76% and the between-run precision was 2.21% -4.64%. The average recovery rate was 93.3% - 98.6%.Conclusion  The concentration of 1,2-DCE in blood could be used as a biological monitoring indicator. The method of the concentration of 1,2-DCE in blood determining by HS-GC-MS was characterized by high sensitivity, wide linear range, small interference, high precision and easy operation.

Key words: Ethylene dichlorides;Environmental monitoring;Blood;HS-GC-MS

发表日期:2016/2

引用本文:

图/表:

  • 10.3760/cma.j.issn.0253-9624.2016.02.015.F001

    10.3760/cma.j.issn.0253-9624.2016.02.015.F001

  • 10.3760/cma.j.issn.0253-9624.2016.02.015.F002

    10.3760/cma.j.issn.0253-9624.2016.02.015.F002

  • 10.3760/cma.j.issn.0253-9624.2016.02.015.T001:表1 人血样中1, 2-DCE线性范围、回归方程、相关系数(n=3)

    10.3760/cma.j.issn.0253-9624.2016.02.015.T001:表1 人血样中1, 2-DCE线性范围、回归方程、相关系数(n=3)

  • 10.3760/cma.j.issn.0253-9624.2016.02.015.T002:表2 方法的精密度、加标回收率实验结果(n=6)

    10.3760/cma.j.issn.0253-9624.2016.02.015.T002:表2 方法的精密度、加标回收率实验结果(n=6)

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