摘要
目的建立工作场所空气中氢醌(对苯二酚)、间苯二酚、邻苯二酚、对硝基苯酚和2,4-二硝基苯酚同时测定的高效液相色谱检测方法。方法空气样品采用复合管(前端玻璃纤维滤膜,后段硅胶)采集,10%甲醇溶液解吸,经C18色谱柱分离,二极管阵列检测器(PDA)检测,在230 nm波长下,外标法进行定量测定。结果5种酚类化合物线性关系良好,r>0.999。方法检出限:玻纤滤膜为0.13~0.41μg/ml,硅胶吸附剂为0.16~1.04μg/ml。方法定量下限:玻纤滤膜为0.44~1.36μg/ml,硅胶吸附剂为0.52~3.46μg/ml。平均解吸效率:玻纤滤膜为97.5%~100.1%,硅胶吸附剂为86.9%~100.3%。批内和批间精密度:玻纤滤膜为0.71%~4.88%、0.91%~4.82%,硅胶吸附剂为0.47%~4.62%、0.76%~5.52%。在-20℃条件下,样品可保存30 d以上。结论本法灵敏度,精密度,准确性及线性范围均满足规范要求,样品的采集及保存也可满足限值的要求,适用于工作场所空气中氢醌、间苯二酚、邻苯二酚、对硝基苯酚和2,4-二硝基苯酚的同时测定。
Objective To develop a method for simultaneous determination of Dydroquinone,Resorcinol,Pyrocatechol,4-Nitrophenol and 2,4-Dinitrophenol in workplace air by high performance liquid chromatography.Methods Air samples were collected by composite tube(front end glass fiber filter membrane,back section silica gel),10%methanol was desorbed,separated by C18 chromatographic column,detected by photo-diode array(PDA)detector,and quantitatively determined by external standard method at the wave-length of 230 nm.Results The linear relationship of 5 phenolic compounds was good(r>0.999).The detection limit of glass fiber filtration membrane and silica gel adsorbent were 0.13-0.41 g/ml and 0.16-1.04 g/ml respectively.The quantitative limit of glass fiber filtration membrane was 0.44-1.36 g/ml,and the silica gel adsorbent was 0.52-3.46 g/ml.The average desorption efficiency of glass fiber membrane and silica gel adsorbent were 97.5%-100.1%and 86.9%-100.3%,respectively.In and between batches,the precision glass fiber filtration membrane was 0.71%-4.88%,0.91%-4.82%,silica gel adsorbent was 0.47%-4.62%,0.76%-5.52%.Samples can be stored for at least 30 days at-20℃.The possible co-existing interferences of aniline,phenol,p-nitrochlorobenzene,o-nitrophenol and trinitrophenyl did not interfere with the determination.Conclusion The sensitivity,precision,accuracy and linear range of this method all meet the requirements of the specification.The collection and preservation of samples can also meet the requirements of the limits.It is suitable for the simultaneous determination of hydroquinone,resorcinol,hydroquinone,hydroquinone,hydroquinone,p-nitrophenol and 2,4-dinitrophenol in the air of the workplace.
作者
宋为丽
张铮
江金凤
杨莉
刘亚攀
Song Weili;Zhang Zheng;Jiang Jinfeng;Yang Li;Liu Yapan(Wuhan Occupation Disease Prevention and Treatment Hospital,Wuhan 430015,China)
出处
《中华劳动卫生职业病杂志》
CAS
CSCD
北大核心
2021年第8期605-609,共5页
Chinese Journal of Industrial Hygiene and Occupational Diseases
基金
中国卫生监督协会2019年团体标准立项计划((2019)28号)。
关键词
色谱法
高效液相
工作场所
空气
复合采样管
酚类化合物
Chromatography,high pressure liquid
Workplace
Air
Composite sampling tube
Phenolic compounds
