三重四极杆质谱技术测定固体废弃物中多氯联苯

Determination of PCBs in Solid Waste by Triple Quadrupole Mass Spectrometry

以二氯甲烷为萃取剂,采用快速溶剂萃取、凝胶渗透色谱净化、三重四极杆质谱技术测定固体废弃物中7种多氯联苯单体,选择十氯联苯为内标物,2,4,5,6-四氯间二甲苯为替代物。质谱采用MRM扫描,优化了目标物质保留时间、母离子和子离子质量数及碰撞能量等参数。方法在0.050 mg/L～2.00 mg/L范围内线性良好,7种多氯联苯单体的检出限为0.194 ng/g～0.355 ng/g(以称取30 g样品、定容至2.0 mL计),标准样品回收率多在60%～105%之间,空白加标样品测定值的相对标准偏差在8.6%～13.0%之间。

7 components of PCBs in solid waste were determined with triple quadrupole mass spectrometry by using accelerated solvent extraction and gel-permeation chromatograph purification. During the analysis process, methylene dichloride was used as extraetant, decachlorobiphenyl as internal standard and 2,4,5,6 - Tetrachloro-m-xylene as surrogate. MRM was used as a quantitative scan mode. Experimental parameters were optimized for retention times of target compounds, mass numbers of parent ions and daughter ions and collision energy. The calibration curves of the method showed a good linearity from 0. 050 mg/L to 2.00 mg/L, detection limits of 7 components of PCBs ranged form 0. 194 ng/g to 0. 355 ng/g （ 30 g sample, formulated into a volume 2.0 mL）. Standard sample recoveries were between 60% and 105%. Relative standard deviations of spiked blank sample were between 8.6% and 13.0%.