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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 the determination of dimethylsulfoxide (DMF) and dimethylacetamide (DMA) in the air of the workplace by high performance liquid chromatography (HPLC). Methods DMF and DMA in the air were collected by silica gel in the air of the workplace and desorbed by pure water. The samples were separated by Eclipse Plus C18 liquid chromatography and detected by a dot matrix detector and quantified by external standard method. Results When the concentration of DMF and DMA was between 20.00 and 400.00 mg / L, the calibration curves showed a good linearity with the correlation coefficients of 0.999 7 and 0.999 9, respectively. The minimum detectable concentrations were 3.0 and 0.05 mg / m3; the intra-and inter-batch precision were <5.0%; the average recoveries were 99.0% -99.6% and 99.6% -100.2% respectively; the sampling efficiencies were 98.2% -100.0% and 97.4% -100.0% respectively; The permeation capacities were 10.2 and 9.9 mg, respectively. The desorption efficiencies were 93.0% -96.9% and 94.0% -98.5%, respectively. The samples were stored at room temperature for 7 days. Conclusion The method has high sensitivity, good precision and strong qualitative ability, which can better adapt to the detection of DMF and DMA in the air of the workplace.