建立了固相萃取(SPE)/气相色谱质谱(GC/MS)联用检测灰尘中氯代多环芳烃(ClPAHs)的方法.以正己烷和二氯甲烷混合液为提取溶剂,索氏提取灰尘样品中的20种ClPAHs,活性硅胶层析柱与活性炭混合硅胶SPE柱协同净化.净化后的提取液采用GC/MS测定,SIM模式扫描,并用质谱特征离子定量分析.结果表明,填充量为0.2 g(W(活性炭)∶W(硅胶)=1∶40)的活性炭混合硅胶SPE小柱能有效地将ClPAHs分离出来,载样后采用反向溶剂洗脱,既提高了回收率又减少了洗脱剂甲苯的用量,净化效果好.处理灰尘样品后检测分析,20种ClPAHs的平均回收率稳定在60.4%—120.1%,相关系数〉0.99,检出限为0.04—0.17 ng.g-1,相对标准偏差为1.6%—10.2%.本方法前处理简单,定性、定量准确可靠,可广泛应用于环境介质中氯代多环芳烃的检测.
A method was developed for the detection of 20 chlorinated polycyclic hydrocarbons(ClPAHs) in dust samples by solid-phase extract(SPE) and gas chromatography-mass spectrometry(GC/MS).The samples were Soxhlet extracted with dichloromethane-hexane mixture for more than 16 h.The extracts were purified through activated silica gel glass column,and then the SPE column self-packed with activated carbon-blended silica gel mixture.After cleanup,the extracts were analyzed by GC/MS in SIM mode,using characteristic ions for quantification.The SPE packed with a 0.2 g mixture of activated carbon-blended silica gel(1 ∶ 40,W/W) was found to have a good selectivity in separating ClPAHs from interference.And it reduced the toxic eluate when the SPE column was back-flushed after the sample extracts were loaded.The linear range,recovery and MDLs of 20 ClPAHs were examined.The recoveries of ClPAHs ranged from 60.4% to 120.1%,and the correlation coefficient was more than 0.99.The pretreatment procedure of this method is easy,and the quantification is sensitive and accurate.The method can be used to detect ClPAHs in many ambient media.