生活用纸杯中二噁英及其类似物多氯联苯迁移量的测定

Determination of the Migration of Dioxins and Their Analogues in Paper Cups for Daily Use

建立生活用纸杯中二噁英(PCDD/Fs)及其类似物多氯联苯(DL-PCBs)迁移量的高分辨气相色谱-高分辨质谱的检测方法。食品模拟物中二噁英及其类似物多氯联苯用正己烷-二氯甲烷溶液提取,浓缩液依次经浓硫酸、多段硅胶柱、氧化铝柱净化和分离后富集,保留时间及高分辨质谱定性,稳定性同位素稀释法定量。PCDD/Fs和DL-PCBs检测限在0.01~0.1ng/L之间,样品加标平行3次的检测结果PCDD/Fs平均回收率在64.8%~90.2%,RSD为1.05%~8.04%,DL-PCBs平均回收率在69.4%~92.4%,RSD为1.05%~5.96%,具有检测限低,回收率好和精密度高的优点。实际样品检测PCDD/Fs13C12标记同位素定量内标回收率为75.4%~93.1%,DL-PCBs13C12标记同位素定量内标回收率为72.9%~91.6%,满足日常检测要求。该方法准确、快速、可靠,可应用于生活用纸杯中二噁英(PCDD/Fs)及其类似物多氯联苯(DL-PCBs)迁移量的检测分析。

To establish a method for the determination of the migration of dioxin(PCDD/Fs)and its analogues polychlorinated biphenyls(DL PCBs)in paper cups for daily use was established by HRGC-HRMS.Dioxins and their analogues are polychlorinated biphenyls in food simulants.The concentrated solution extracted from n-hexane-dichloromethane solution is purified and separated with concentrated sulfuric acid,multi-stage silica gel column and alumina column,and then concentrated.They are determined by the retention time,high-resolution mass spectrometry and stable isotope dilution.The detection limit of PCDD/Fs and DL PCBs is 0.01~0.1 ng/L.The average recovery of PCDD/Fs is 64.8%~90.2%,RSD is 1.05%~8.04%,DL-PCBs is 69.4%~92.4%,RSD is 1.05%~5.96%,which have the advantages of low detection limit,good recovery and high precision.The recoveries 13C12 of PCDD/Fs and DL PCBs were 75.4%~93.1%and 72.9%~91.6%,which met the requirements of daily detection respectively.The method is accurate,fast and reliable,and can be used to detect the migration of PCDD/Fs and its analogues DL PCBs in paper cups for daily use.