高效液相色谱法同时测定工作场所空气中二甲基甲酰胺和二甲基乙酰胺

Simultaneous determination of DMF and DMA in workplace air by high-performance liquid chromatography

目的建立工作场所空气中二甲基甲酰胺（DMF）和二甲基乙酰胺（DMA）的硅胶管采集高效液相色谱测定方法。方法工作场所空气中DMF和DMA用硅胶管采集,纯水解吸,经Eclipse Plus C18液相色谱柱分离,二极管点阵检测器检测,外标法定量。结果 DMF和DMA质量浓度在20.00～400.00 mg/L时,标准曲线线性关系良好,相关系数分别为0.999 7和0.999 9;按采集空气样品3.0 L计算,最低检出浓度分别为0.03和0.05 mg/m3;批内及批间精密度均〈5.0%;平均加标回收率分别为99.0%～99.6%和99.6%～100.2%;采样效率分别为98.2%～100.0%和97.4%～100.0%;穿透容量分别为10.2和9.9 mg;解吸效率分别为93.0%～96.9%和94.0%～98.5%;样品在常温条件下可保存7 d。结论本方法灵敏度高、精密度好及定性能力强,能更好适应工作场所空气中DMF和DMA检测。

Objective To establish a method for measuring the amount of dimethylformamide（ DMF） and dimethylacetamide（ DMA） in the workplace air with silicone tube,by high-performance liquid chromatography. Methods The air samples of DMF and DMA were quantitatively detected by the method of external standard after a series of handle steps：collected with silicone tube first,and then desorbed with pure water,separated with a Eclipse Plus C18 column and tested with a diode matrix detector. Results For DMF and DMA,the standard curve showed a good linear relationship under the mass concentration of 20. 00-400. 00 mg / L（ correlation coefficient = 0. 999 7 or 0. 999 9）; the air samples were calculated according to 3. 0 L,the minimum detection concentration were 0. 03 and 0. 05 mg / m3 respectively. Both the within-run and between-run precisions were all less then 5. 0%,and the average value of adding standard recovery accounted for 99. 0%-99. 6% and 99. 6%-100. 2% respectively,and the sampling efficiency accounted for 98. 2%-100. 0% and 97. 4%-100. 0% respectively,penetrating capacity were 10. 2 and 9. 9 mg respectively,and the desorption efficiency accounted for93. 0%-96. 9% and 94. 0%-98. 5% respectively. The samples could be stored at room temperature for at least 7 days.Conclusion With higher sensitivity,good precision and strong determination,this method is more suitable for detecting DMF and DMA in the workplace air.