气相色谱-三重四级杆质谱测定环境样品中17种二英

摘要

A method for determining 17dioxins and furans in environmental samples using gas chromatography coupled to triple quadrupole mass spectrometry (MS/MS) had been studied. Good linearity was obtained for the concentration ranged from 0.5to 2000ng/mL. The relative response factors were ranged from 0.96to 1.21, with the relative standard deviation below 14% for the 17congeners. The levels of quantitative of this method were at the range of 0.080~2.83pg/µL, which was suitable for ultra-trace dioxin analysis in environmental samples. Three sediments from the 15th round of intercalibration study were used as certified reference materials to confirm this analytical method. The obtained results are satisfactory. More than 40 environmental samples, including flue gas, fly ash, soil, and sediment were analysed using MS/MS. The obtained results were also compared with results by high resolution mass spectrometry (HRMS). Good linear correlation (R2=0.997) was observed when the concentration values ranged from 0to 60ng I-TEQ. For specific congeners, values of 2,3,7,8-TCDF and 1,2,3,7,8,9-HxCDF obtained by MS/MS were higher than by HRMS. However, value results of 1,2,3,7,8,9-HxCDD were lower. Because of the low cost of MS/MS on purchase, maintenance, and energy consumption, this method can be a simple and economic method for ultra-trace dioxin analysis in environmental samples.%研究了基于Agilent气相色谱-三重四级杆质谱测定环境样品中17种二英的分析方法.结果表明,在浓度范围0.5~2000ng/mL之间具有良好的线性,17种二英的相对响应因子在0.96~1.21之间,相对标准偏差<14%,定量限范围在0.080~2.83pg/μL之间,适合环境样品中超痕量二英的分析.利用该方法对第15轮二英国际实验室比对的沉积物样品进行了测试,总I-TEQ值落在Intercal给定的中位值±标准偏差范围内.研究选取污染源烟道气、飞灰、土壤和沉积物等40多个环境样品进行测试,并与高分辨质谱测定结果比较表明,当环境样品中二英浓度在0~60ng I-TEQ范围,两者数据具有较好的线性相关性,R2=0.997.就17种单体而言,利用三重四级杆质谱测定的2,3,7,8-TCDF和1,2,3,7,8,9-HxCDF结果会高于高分辨质谱,而1,2,3,7,8,9-HxCDD的结果低于高分辨质谱的测定值.鉴于三重四级杆质谱在购置、维护和能耗等方面的低成本优势,本方法可作为简易经济的环境中超痕量二英的分析方法.