碱性硅胶管吸附-衍生化解吸-HPLC法测定工作场所空气中二乙烯三胺

    Determination of diethylenetriamine in workplace air by HPLC based on adsorption on alkaline silica gel tubes and derivatization-desorption

    • 摘要:
      目的 建立一种测定工作场所空气中二乙烯三胺的碱性硅胶管吸附-衍生化解吸-高效液相色谱法, 并评价其应用效果。
      方法 在参考现有高效液相色谱检测技术的基础上, 采用碱性硅胶管分别进行长时间采样、短时间采样后进行测定, 对方法的测量范围、精密度、准确度、解吸效率、稳定性以及干扰试验进行研究。
      结果 方法质量浓度范围为0.19~30 μg/mL, 线性关系良好, 相关系数(r)>0.999。当采集样品体积为7.5 L、解吸液体积为2 mL时, 最低检出浓度为0.015 mg/m3, 最低定量浓度为0.051 mg/m3。平均解吸效率为92.1%~98.5%, RSD为2.81%~5.03%, 加标回收率为91.66%~102.67%, 室温下至少可保存15 d。配制0.5倍和2倍PC-TWA浓度的实验气, 采样效率为91.9%~100.0%。
      结论 本研究建立的碱性硅胶管吸附-衍生化解吸-液相色谱法测定工作场所空气中二乙烯三胺, 方法响应值高, 精密度好, 分析时间短, 可实现采样至分析流程的规范化操作, 准确可靠, 适用于工作场所空气中二乙烯三胺的测定及大规模职业卫生监测。

       

      Abstract:
      Objective To establish a method for the determination of diethylenetriamine (DETA) in workplace air by alkaline silica gel tube adsorption-derivatization desorption-high performance liquid chromatography (HPLC), and to evaluate its application efficacy.
      Methods Drawing on existing HPLC detection technologies, alkaline silica gel tubes were utilized for both long-term and short-term sampling, followed by subsequent analysis. The method was systematically characterized in terms of its linear range, precision, accuracy, desorption efficiency, stability, and anti-interference performance.
      Results The method exhibited a linear concentration range of 0.19-30 μg/mL with a linear correlation coefficient (r)>0.999, indicating excellent linearity. Under the conditions of a sampling volume of 7.5 L and a desorption solution volume of 2 mL, the limit of detection (LOD) was 0.015 mg/m3, and the limit of quantification (LOQ) was 0.051 mg/m3. The average desorption efficiency ranged from 92.1% to 98.5%, with a relative standard deviation (RSD) of 2.81%-5.03%. Spike recovery rates were 91.66%-102.67%, and the samples showed stability for at least 15 days at room temperature. For experimental atmospheres prepared at 0.5× and 2× the permissible concentration-time weighted average (PC-TWA), the sampling efficiency was 91.9%-100.0%.
      Conclusion The developed method of alkaline silica gel tube adsorption-derivatization desorption-HPLC for DETA in workplace air demonstrates high responsiveness, good precision, and short analysis time. It enables standardized operation from sampling to analysis, yielding accurate and reliable results, and is thus suitable for the determination of DETA in workplace air and large-scale occupational health monitoring.

       

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