色谱 ›› 2018, Vol. 36 ›› Issue (1): 51-58.DOI: 10.3724/SP.J.1123.2017.09044

• 研究论文 • 上一篇    下一篇

快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中16种多环芳烃

宋晓娟, 李海燕, 尹明明, 马玉琴   

  1. 连云港市环境监测中心站, 江苏 连云港 222001
  • 收稿日期:2017-09-26 出版日期:2018-01-08 发布日期:2018-01-22
  • 通讯作者: 李海燕,E-mail:lygjcz2017@163.com.

Determination of 16 polycyclic aromatic hydrocarbons in marine sediments by gas chromatography-tandem mass spectrometry with accelerated solvent extraction

SONG Xiaojuan, LI Haiyan, YIN Mingming, MA Yuqin   

  1. Lianyungang Municipal Environmental Monitoring Center Station, Lianyungang 222001, China
  • Received:2017-09-26 Online:2018-01-08 Published:2018-01-22

摘要:

建立了快速溶剂萃取(ASE)-气相色谱-串联质谱(GC-MS/MS)分析海洋沉积物中16种多环芳烃(PAHs)的分析方法。样品由正己烷-丙酮(1∶1,v/v)溶液萃取,经无水硫酸钠脱水、氮吹浓缩后,采用硅胶固相萃取小柱进行净化,然后经HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)分离,在电子轰击电离源下以多反应监测(MRM)模式进行检测,内标法定量。分析结果表明,16种PAHs在0.01~1.00 mg/L范围内线性关系良好,相关系数(R)大于0.997;目标物的加标回收率为75.8%~97.8%;日内与日间精密度(RSD)均小于10%。当取样量为20.0 g时,16种PAHs的方法检出限为0.048~0.234 μg/kg。该法快速、准确、稳定,能够满足海洋沉积物中痕量PAHs的测定。

关键词: 多环芳烃, 海洋沉积物, 快速溶剂萃取, 气相色谱-串联质谱

Abstract:

A method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) with accelerated solvent extraction (ASE) was developed for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in marine sediments. The sediment samples were extracted with hexane-acetone (1:1, v/v). The extracts were dehydrated with anhydrous sodium sulfate, and concentrated with a termovap sample concentrator. The concentrated solutions were further cleaned up with Si SPE columns. The purified solutions were then isolated by HP-5MS column (30 m×0.25 mm×0.25 μm). The analytes were detected using electron impact source under multiple reaction monitoring (MRM) mode. The results showed that the 16 PAHs had good linearities in the range of 0.01-1.00 mg/L with the correlation coefficients (R) greater than 0.997. The spiked recoveries of the 16 PAHs were in the range of 75.8%-97.8%, and the relative standard deviations (RSDs) were less than 10%. The method detection limits (MDLs) of the 16 PAHs ranged from 0.048-0.234 μg/kg with 20.0 g sampling weight. This method is suitable for the determination of trace PAHs in marine sediments.

Key words: accelerated solvent extraction (ASE), gas chromatography-tandem mass spectrometry (GC-MS/MS), marine sediments, polycyclic aromatic hydrocarbons (PAHs)

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