论文部分内容阅读
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 of solid phase extraction (SPE) / gas chromatography-mass spectrometry (GC / MS) for the detection of ClPAHs in dust was established. Soxhlet extraction was carried out using n-hexane and dichloromethane as solvent 20 kinds of ClPAHs, active silica gel column and activated carbon mixed silica SPE column were used to purify.The purified extract was analyzed by GC / MS and SIM mode and quantified by mass spectrometry characteristic ions.The results showed that the filling amount was 0.2 Cl (W (activated carbon): W (silica gel) = 1:40) was used to separate ClPAHs efficiently. After the samples were loaded with reverse solvent, the recovery was improved and the washing time was reduced The removal rate of toluene, the purification effect is good.Detection of dust samples after the test analysis, 20 kinds of ClPAHs average recovery was stable at 60.4% -120.1%, the correlation coefficient> 0.99, the detection limit of 0.04-0.17 ng.g-1, The relative standard deviations were 1.6% -10.2%. The pretreatment of this method is simple, qualitative, accurate and reliable. It can be widely used in the detection of chlorinated PAHs in environmental media.