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

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。

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

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.