长江南京段水体中7种苯胺类化合物的检测方法及生态风险评价

应用固相萃取结合高效液相色谱-串联质谱法,建立了同时测定环境水样中7种苯胺类化合物的检测方法.实验表明,以ZORBAX Eclipse Plus C18 (3.5μm,2.1×150mm)色谱柱为分离柱,乙腈-水(2mmol/L甲酸铵)为梯度洗脱的流动相,在电喷雾质谱正离子模式下,7min内可以分离目标化合物;在1~200μg/L浓度范围内,7种苯胺类化合物的峰面积与质量浓度的线性关系良好;添加水平分别为0.8、4.0、20.0mg/L时,目标化合物的平均回收率分别为68.5%~102.2%、71.4%~89.4%、62.0%~78.3%,相对标准偏差均小于6.9%;利用本方法对长江南京段平水期(2014.4)、丰水期(2014.8)和枯水期(2014.12)的14个采样点的环境水样进行检测,检出4-硝基苯胺、2,6-二乙基苯胺、3,4-二氯苯胺和4-异丙基苯胺4种苯胺类化合物,且4-硝基苯胺在3个时期14个采样点均能检出;风险商值法评估长江南京段水体中4-硝基苯胺的生态风险为低生态风险.

Analysis method and environmental risk assessment of 7aniline compounds of environmental water samples in Yangtze River of Nanjing section

An analysis method based on solid phase extraction (SPE) coupled with liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) with positive ionization mode has been developed for measuring of seven aniline compounds in environmental water samples. The target compounds were separated on ZORBAX Eclipse Plus C18 (3.5μm,2.1×150mm) column with mobile phases containing acetonitrile and 2mmol/L aqueous ammonium formate. Analytes confirmations were performed using multiple reactions monitoring (MRM) and seven compounds were separated within 7min. The calibration curve was linear in the range 1~1000μg/L. Recovery experiments were performed using MCX extraction cartridge and concentrations varied from 0.8~20μg/L. The recovery rates for target compounds were in the range of 68.5%~102.2%, 71.4%~89.4%, 62.0%~78.3% (RSD < 6.9%, n=3), respectively. Base on the analysis method, the water samples in Yangtze River of Nanjing section at 14sampling site during the flow period (April, 2014), the wet period (August, 2014) and the dry period (December, 2014) were analysed. Four target compounds, including 4-Nitroaniline, 2,6-diethyl-Benzenamine, 3,4-Dichloroaniline and 4-Isopropylaniline, were determined in the water, while 4-Nitroaniline was all determined at 14sampling site during the flow period, the wet period and the dry period. Risk quotient method was utilized to evaluate the environmental risks for 4-Nitroaniline, and the results was low risk levels.