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目的建立用于工作场所及室内空气中甲醛采样的固相吸附采样管,并建立相应的高效液相色谱检测方法。方法基于2,4-二硝基苯肼与羰基官能团发生化学衍生反应生成甲醛-2,4-二硝基苯腙的原理,采用浸渍硅胶管吸附空气中甲醛,吸附的衍生化产物经乙腈解吸后,C18色谱柱分离,紫外检测器测定。结果本方法在0.07~11.43 mg/L呈良好线性关系,相关系数为0.999 98,甲醛检出限为0.02 mg/L,最低检出浓度为0.01 mg/m3。固相吸附管对甲醛的解吸效率为97.33%~101.00%,平均衍生效率为97.76%~99.10%,精密度为2.43%~3.59%,采样效率为96.49%~98.78%,甲醛的穿透容量大于44.39μg,采样管保存时间大于4个月,采样后室温避光条件下样品至少可以保存7 d。结论空气中甲醛的浸渍硅胶管衍生捕集-高效液相色谱检测方法满足室内空气及工作场所空气中甲醛的测定。
Objective To establish a solid phase adsorption sampling tube for formaldehyde sampling in the workplace and indoor air and establish a corresponding HPLC detection method. Methods Based on the principle of chemical derivatization of 2,4-dinitrophenylhydrazine with carbonyl functional groups to produce formaldehyde-2,4-dinitrophenylhydrazone, formaldehyde in air was adsorbed by impregnated silica gel and the adsorbed derivatized product was desorbed by acetonitrile After C18 column separation, UV detector determination. Results The method showed good linearity in the range of 0.07-11.43 mg / L with a correlation coefficient of 0.999 98. The detection limit of formaldehyde was 0.02 mg / L and the lowest detection limit was 0.01 mg / m3. The desorption efficiency of formaldehyde for the solid phase adsorption tube was 97.33% -101.00%, the average derivatization efficiency was 97.76% -99.10%, the precision was 2.43% -3.59%, the sampling efficiency was 96.49% -98.78%, the penetration capacity of formaldehyde was greater than 44.39μg, the sampling tube is stored for more than 4 months, and the sample can be stored for at least 7 days under dark conditions at room temperature after sampling. Conclusion Formaldehyde-impregnated silica gel tube derivatization-high performance liquid chromatography (HPLC) in the air meets the determination of formaldehyde in indoor air and workplace air.