全自动顶空固相微萃取GC-MS测定土壤中多氯联苯

单美娜; 李亮

doi:10.13421/j.cnki.hjwsxzz.2021.05.011

全自动顶空固相微萃取GC-MS测定土壤中多氯联苯

单美娜,
李亮

Determination of PCBs in Soil by Automated Headspace Solid Phase Microextraction-GC-MS

摘要

摘要:
目的建立全自动顶空固相微萃取(SPME)气相色谱—质谱法(GC-MS)同时测定土壤中18种PCBs的分析方法。
方法研究了土壤取样量、加水量、萃取温度、萃取时间对SPME富集效果的影响，并确定了最佳优化条件为4 g土壤样品加入6 mL纯净水中，70 ℃下萃取30 min。
结果在(250~2 500)pg/g范围内线性关系良好，方法的检出限为(20~50)pg/g。加标回收率在90.2%~125.5%之间，相对标准偏差在1.58%~9.91%之间。
结论方法综合了SPME简便快捷和GC-MS较高的精密度和准确度的优点，尤其适合于土壤中痕量多氯联苯的快速筛查分析。

Abstract:
Objective To establish a method based on automated headspace solid phase microextraction (SPME)-gas chromatography-mass spectrometry (GC-MS) for the determination of 18 polychlorinated biphenyls (PCBs) in soil.
Methods Through analyzing the effects of soil amount to be sampled, water volume to be added, extraction temperature, and extraction duration on the enrichment of SPME, we identified the optimal conditions as following: adding 6 mL of purified water into 4 g of soil sample, followed by extraction at 70 ℃ for 30 min.
Results A good linear relationship was observed in the range of 250-2 500 pg/g. The detection limit was 20-50 pg/g. The recovery rate ranged from 90.2% to 125.5%, and relative standard deviation was from 1.58% to 9.91%.
Conclusion Combining the advantages of fast, convenient of SPME and precise, and accurate of GC-MS, this method is particularly suitable for rapid screening analysis of trace PCBs in soil.

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