工作场所空气中二苯基甲烷二异氰酸酯浸渍滤纸采集-高效液相色谱法

摘要

目的 建立工作场所空气中二苯基甲烷二异氰酸酯(MDI)的浸渍滤纸采集-高效液相色谱测定方法.方法 空气中二苯基甲烷二异氰酸酯与浸渍滤纸上的1-(2-吡啶基)哌嗪反应生成MDI-脲衍生物而被吸附于滤纸上,经洗脱、过滤后,高效液相色谱仪测定.结果 二苯基甲烷二异氰酸酯的检出限为0.003 8 μg/ml,定量限为0.013 μg/ml,在0.013~2.000 μg/ml范围内线性良好(r=0.999 7),方法精密度为3.10%~8.03%(n=6),回收率为96.3%~101.9%,滤纸吸附容量为40.8 μg MDI,样品在2℃~8℃避光环境中可保存14 d.结论 本方法优化MDI标准曲线的配制方法,建立了测定工作场所空气中MDI的浸渍滤纸采集-高效液相色谱法.%Objective To develop a method for determining diphenylmethane diisocyanate in workplace air by HPLC with impregnated filter membrane. Methods MDI in workplace air reacted with 1-(2-pyridyl) piperazine on impregnated filter membrane to form MDI-urea derivatives, after elution and filtration, it was detected by HPLC-UV.Results Limit of detection was 0.003 8 μg/ml and limit of quantification was 0.013 μg/ml.Good linearity was obtained in the range of 0.013~2.000 μg/ml(r=0.999 7).The precision was 3.10%~8.03%(n=6), while the recovery was 96.3%~101.9%.Asorption capacity of the membrane was 40.8 μg MDI, and could be stored for 14 days in the light-proof environment of 2~8℃. Conclusion The method optimized testing steps for MDIˊs standard curve, and provided good guidance for determination of MDI in workplace air with impregnated fiter membrane.