摘要
目的:采用气相色谱-质谱法建立土壤样品中指示性多氯联苯的检测方法。方法:土壤样品经干燥后,加入同位素内标,采用正己烷/二氯甲烷(v/v 1∶1)进行索氏提取后经磺化,过酸碱硅胶柱和中性氧化铝柱净化,选择离子监测模式,气相色谱-质谱测定。结果:7种指示性多氯联苯的检出限为1.1μg/L~4.5μg/L,在20μg/L~2000μg/L的浓度范围内线性良好(R≥0.999)。样品加标回收率为82.5%~101.5%,相对标准偏差(RSD)为3.45%~9.98%(n=6)。结论:该方法适用于土壤中指示性多氯联苯的测定。
Objective:To establish a method for the determination of indicator PCBs in soil by GC-MS.Methods: Soil sample was added with 13C12L labeled internal standard after drying,then soxhlet extracted by N-hexane/dichloromethane(v/v 1∶1).Further cleanup procedure was followed by sulfonation,acid-base silica gel column and alumina column,respectively.The sample was determined by GC-MS in selected ion monitoring mode.Results: The detection limit ranged of seven indicator PCBs was 1.1 μg/L~4.5 μg/L,and linear range was 20 μg/L~2000 μg/L(R≥0.999).The recoveries for the soil samples ranged from 82.5%~101.5%,and the relative standard deviation ranged from 3.45%~9.98%(n=6).Conclusion: Results indicated that,this study provided a accurate and sensitive method for determining the indicator PCBs in soil.
出处
《中国卫生检验杂志》
CAS
2010年第11期2722-2723,共2页
Chinese Journal of Health Laboratory Technology
基金
杭州市科技局项目(20091233Q27)
作者简介
[作者简介]王姝婷(1980-),女,博士,主管技师,主要从事理化检验工作。