Kowalska Joanna, Jeżewska Anna
Centralny Instytut Ochrony Pracy - Państwowy Instytut Badawczy / Central Institute for Labour Protection - National Research Institute, Warszawa, Poland (Zakład Zagrożeń Chemicznych, Pyłowych i Biologicznych / Department of Chemical, Aerosol and Biological Hazards).
Med Pr. 2016;67(1):43-50. doi: 10.13075/mp.5893.00194.
3,3'-Dimethylbenzidene (DMB) is a substance classified into the group of carcinogens. The value of maximum admissible concentration for this substance in the workplace air is not specified in Poland. Bearing in mind that DMB is used in domestic companies there is a need to develop a sensitive method for determining 3,3'-dimethylbenzidine in the work environment.
The method consists in passing DMB-containing air through sulfuric acid-treated glass fiber filters, washing out the substance settled on the filter, using water and solution of sodium hydroxide, liquid-liquid extraction with toluene, replacing dissolvent with acetonitrile and analyzing the obtained solution. Studies were performed using high-performance liquid chromatography (HPLC) technique. An Agilent Technologies chromatograph, series 1200, with a diode-array detector (DAD) and a fluorescence detector (FLD) was used in the experiment. In the test, an Ultra C18 column of dimensions: 250×4.6 mm, particle diameter (dp) = 5 μm (Restek) was applied.
The method is linear (r = 0.999) within the investigated working range of concentration 1.08-21.6 μg/ml, which is equivalent to air concentrations 2-40 μg/m3 for a 540 l air sample. The limit of detection (LOD) of quantification determination is 5.4 ng/ml and the limit of quantification (LOQ) - 16.19 ng/ml.
The analytical method described in this paper allows for selective determination of 3,3'-dimethylbenzidine in the workplace air in the presence of 1,4-phenylenediamine, benzidine, aniline, 3,3'-dimethoxybenzidine, 2-nitrotoluene, 3,3'-dichlorobenzidine and azobenzene. The method is characterized by good precision and good accuracy, it also meets the criteria for procedures involving the measurement of chemical agents, listed in EN 482:2012.
3,3'-二甲基联苯胺(DMB)是一种被归类为致癌物的物质。波兰未规定该物质在工作场所空气中的最大允许浓度值。鉴于国内企业使用DMB,有必要开发一种灵敏的方法来测定工作环境中的3,3'-二甲基联苯胺。
该方法包括使含DMB的空气通过经硫酸处理的玻璃纤维滤器,用水和氢氧化钠溶液冲洗滤器上沉积的物质,用甲苯进行液-液萃取,用乙腈替换溶剂并分析所得溶液。研究采用高效液相色谱(HPLC)技术进行。实验中使用了安捷伦科技1200系列色谱仪,配有二极管阵列检测器(DAD)和荧光检测器(FLD)。测试中应用了尺寸为250×4.6 mm、粒径(dp)= 5 μm的Ultra C18柱(Restek)。
该方法在所研究的1.08 - 21.6 μg/ml浓度工作范围内呈线性(r = 0.999),对于540 l空气样品,这相当于空气浓度为2 - 40 μg/m³。定量测定的检测限(LOD)为5.4 ng/ml,定量限(LOQ)为16.19 ng/ml。
本文所述的分析方法能够在存在1,4 - 苯二胺、联苯胺、苯胺、3,3'-二甲氧基联苯胺、2 - 硝基甲苯、3,3'-二氯联苯胺和偶氮苯的情况下,选择性地测定工作场所空气中的3,3'-二甲基联苯胺。该方法具有良好的精密度和准确度,也符合EN 482:2012中列出的涉及化学物质测量程序的标准。