高分辨气相色谱-高分辨质谱法同时测定生活用纸制品中的二噁英及其类似物的含量

Determination of Dioxin and Its Analogues in Paper Products by HRGC-HRMS

建立了生活用纸制品中17种二噁英(PCDD/Fs)及12种二噁英类似物多氯联苯(DL-PCBs)的高分辨气相色谱-高分辨质谱法(HRGC-HRMS)的检测方法。样品剪碎后匀浆,采用水浴振荡提取,提取液浓缩后依次经硫酸、多段硅胶柱、氧化铝柱净化和分离后浓缩,保留时间及高分辨质谱定性,稳定性同位素稀释法定量。本方法PCDD/Fs和DL-PCBs检测限在0.01~0.10ng/kg之间,样品加标平行6次的检测结果PCDD/Fs平均回收率在70.3%~92.1%,RSD为2.34%~7.48%,DL-PCBs平均回收率在72.4%~88.3%,RSD为2.19%~6.95%,具有检测限低,回收率良好和精密度高,满足日常检测要求。在实际样品检测中PCCD/Fs13C12标记同位素定量内标回收率为70.7%~92.9%,DL-PCBs13C12标记同位素定量内标回收率为70.1%~88.6%。该方法准确、快速、可靠,可应用于生活用纸制品中17种二噁英(PCDD/Fs)及12种二噁英类似物多氯联苯(DL-PCBs)的含量分析。

A high resolution gas chromatography-high resolution mass spectrometry(HRGC-HRMS)method for the determination of 17 kinds of dioxins(PCDD/Fs)and 12 kinds of dioxin analogues polychlorinated biphenyls(DL-PCBs)in paper products was established.The homogenate was extracted by shaking in water bath after being chopped.The extract was purified and separated by sulfuric acid,multi-stage silica gel column and alumina column,and then concentrated.The retention time and high-resolution mass spectrometry were used for qualitative analysis,and the stable isotope dilution method was used for quantitative analysis.The detection limits of PCDD/Fs and DL-PCBs were 0.01~0.10 ng/kg,the average recovery of PCDD/FS was 70.3%~92.1%,RSD was 2.34%-7.48%,the average recovery of DL-PCBs was 72.4%~88.3%,RSD was 2.19%~6.95%,with low detection limits,good recovery and high precision,meeting the requirements of daily detection.The recoveries of PCDD/Fs 13C12 and DL-PCBs 13C12 were 70.7%~92.9%and 70.1%~88.6%.The method is accurate,rapid and reliable,it can be applied to the content analysis of 17 kinds of PCDD/Fs and 12 kinds of DL-PCBs.