摘要
采用加速溶剂萃取-柱层析-高分辨质谱法检测废线路板粉末样品中17种2,3,7,8-PCDD/Fs的含量。采用TRDIOXIN-5MS毛细管色谱柱（60 m×0.25 mm×0.25μm）进行分离和多离子检测（MID）模式进行检测,以保留时间和同位素特征离子丰度比进行定性,用13C标记同位素稀释内标法进行定量。结果表明,17种2,3,7,8-PCDD/Fs化合物的标准曲线的线性相关性良好,线性相关系数均大于0.999 9,该方法分析的提取内标的平均回收率范围为37.25%-82.75%,RSD〈8%,样品中各异构体的加标回收率为112.66%-124.26%,RSD〈7%。应用该方法检测废线路板粉末样品,回收率在58.67%-123.00%范围内,1,2,3,4,6,7,8-HpCDF、1,2,3,4,6,7,8-HpCDD、OCDF、OCDD的质量比分别为2.74、2.50、5.57、16.37 pg/g,TEQ分别为0.027 4、0.025 0、0.005 6、0.016 4 ng/kg。
The contents of 17 kinds of 2,3,7,8-PCDD / Fs in waste circuit board powder were detected by accelerated solvent extractor device-column chromatography-high resolution mass spectrometry. The extracts were separated by HRGC on a TRDIOXIN-5MS column（ 60 m × 0. 25 mm × 0. 25 μm） and determined by HRMS on multiple ion detection（ MID） mode. The identification of PCDD / Fs was based on the retention times of13C-labelled standard and the abundance ratios of the two exacted mass-to-charge ratios. The quantitative analysis was performed using the ratios of the integrated areas of the13C-labelled standards. The results showed that the calibration curve of 17 kinds of 2,3,7,8-PCDD / Fs had a good linear correlation,the linear correlation coefficient were above 0. 999 9. ASE extraction had the recoveries ranging from 37. 25% to 82. 75%,RSD 8%,the isomers of samples had the recoveries ranging from 112. 66% to 124. 26%,RSD 7%. The waste circuit boards powder samples were measured using this method,with the recoveries from 58. 67% to 123. 00%,the mass ratios of 1,2,3,4,6,7,8-HpCDF,1,2,3,4,6,7,8-HpCDD,OCDF,OCDD were 2. 74,2. 50 pg / g,5. 57 and 16. 37 pg / g,respectively. TEQ of them were 0. 027 4,0. 025 0 ng / kg,0. 005 6 and 0. 016 4 ng / kg.
出处
《中国环境监测》
CAS
CSCD
北大核心
2016年第6期130-134,共5页
Environmental Monitoring in China
基金
江苏省环境保护厅环保科研课题(2012029)
关键词
高分辨质谱法
二噁英
废线路板粉末
high resolution mass spectrometry
dioxin
waste circuit boards powder
