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工作场所空气中三价铬和六价铬的高效液相色谱-电感耦合等离子体质谱同时测定法

Simultaneous determination of trivalent chromium and hexavalent chromium in workplace air by high performance liquid chromatography-inductively coupled plasma mass spectrometry method

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【作者】 曹林波姜丽华张婧怡翁少梅张仕浩崔世勇

【Author】 CAO Linbo;JIANG Lihua;ZHANG Jingyi;WENG Shaomei;ZHANG Shihao;CUI Shiyong;Physical and Chemical Laboratory,Shanghai Baoshan District Center for Disease Control and Prevention;

【通讯作者】 崔世勇;

【机构】 上海市宝山区疾病预防控制中心理化检验科

【摘要】 目的 以高效液相色谱-电感耦合等离子体质谱(highperformanceliquid chromatography-inductively coupled plasma mass spectrometry,HPLC-ICP-MS)法为检测手段,建立同时测定工作场所空气中三价铬Cr(Ⅲ)和六价铬Cr(Ⅵ)含量的方法。方法 样品用碱性聚偏二氟乙烯(polyvinylidene difluoride,PVDF)滤膜采集,通过乙二胺四乙酸(ethylene diamine tetraacetic acid,EDTA)-硝酸铵溶液洗脱,以硝酸铵为流动相,液相色谱分离,电感耦合等离子体质谱检测,外标法定量。结果 三价铬和六价铬在1~500μg/L范围内相关系数>0.999,方法检出限分别为0.000 024 mg/m~3和0.000 034 mg/m~3(以采样45 L计算),定量限为0.000 44 mg/m~3;加标回收率在87.7%~105%之间,相对标准偏差均<5%。结论 该方法准确、灵敏、检测范围宽,适用于工作场所空气中Cr(Ⅲ)和Cr(Ⅵ)的同时测定,为职业安全检测领域的发展提供了参考。

【Abstract】 Objective To establish a method for the simultaneous determination of trivalent chromium[Cr (Ⅲ )] and hexavalent chromium[Cr(Ⅵ)] in workplace air using high-performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS). Methods Samples were collected using an alkaline polyvinylidene difluoride(PVDF) filter,eluted with an ethylene diamine tetraacetic acid(EDTA)-NH4NO3solution,separated by liquid chromatography using NH4NO3as the mobile phase,and detected by inductively coupled plasma mass spectrometry. Quantification was performed using an external standard calibration curve. Results The correlation coefficients for Cr(Ⅲ ) and Cr(Ⅵ) were greater than 0.999 within the concentration range of 1-500 μg/L. The limits of detection were 0.000 024 mg/m3and 0.000 034 mg/m3,respectively(based on a sampling volume of 45 L),and the quantification limit was 0.000 44 mg/m3. The recovery rate ranged from 87.7% to 105%,with relative standard deviations all below 5%. Conclusion This method is accurate,sensitive,and has a wide detection range,it is suitable for the simultaneous determination of Cr(Ⅲ ) and Cr(Ⅵ) in workplace air,providing a reference for the advancement of occupational safety testing.

【基金】 上海市宝山区科学技术委员会面上项目(21-E-08)
  • 【文献出处】 职业与健康 ,Occupation and Health , 编辑部邮箱 ,2025年16期
  • 【分类号】R134.4;O657.63
  • 【下载频次】24
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